Preparation and crystal structure of the oxalato-bridged CrIII–AgItwo-dimensional compound {Ag3(H2O)[Cr(dpa)(ox)2]3}n·2nH2O (dpa = 2,2′-dipyridylamine)

The reaction of the mononuclear complex [Cr(dpa)(ox)2]− (dpa = 2,2-dipyridylamine) with Ag+ in aqueous solution affords the two-dimensional compound {Ag3(H2O)[Cr(dpa)(ox)2]3}n·2nH2O (1) whose structure has been determined by single-crystal X-ray diffraction. Six crystallographically independent metal atoms (three chromium and three silver atoms) occur in 1. The three [Cr(dpa)(ox)2]− units in 1 act as ligands towards the silver atoms through the two oxalate groups. Each oxalate group acts as bridging ligand adopting five coordination modes: bis-bidentate, bis-bidentate/monodentate (outer), bis-bidentate/monodentate (inner), bidentate/bis-monodentate (outer) and bidentate/monodentate (outer).…

Unexpected magnetic topology in the heterobimetallic [ReIVBr4(μ-ox)CuII(bpy)2] compound

Abstract A novel oxalato-bridged rhenium(IV)-copper(II) compound, namely [ReIVBr4(μ-ox)CuII(bpy)2] (1), has been obtained by reacting (PPh4)2[ReBr4(ox)] with Cu(CF3SO3)2 and 2,2′-bpy in CH3CN, and its crystal structure determined by single-crystal X-ray diffraction. Intermolecular Br⋯Br interactions and nonbonding Cu⋯Br type contacts between the heterobimetallic dinuclear units lead to a two-dimensional supramolecular structure. Compound 1 behaves magnetically as a [ReIVCuII]2 tetranuclear species with weak antiferromagnetic interactions through the oxalato bridge and intermolecular Br⋯Br contacts.

Magnetic coupling and spin topology in linear oxalato-bridged tetranuclear chromium(III)–copper(II) complexes with aromatic diimine ligands

Abstract A novel heterotetranuclear chromium(III)–copper(II) complex of formula {[CrIII(bpy)(ox)2]2CuII2(bpy)2(ox)}·6H2O (1) has been synthesized by the ligand exchange reaction between Ph4P[CrIII(bpy)(ox)2]·H2O and [CuII(bpy)2(NO3)]NO3·MeOH in methanol (bpy = 2,2′-bipyridine; ox2− = oxalate dianion). The X-ray crystal structure of 1 consists of neutral oxalato-bridged CrIII2Cu2II zigzag entities which are formed by the monodentate coordination of two [CrIII(bpy)(ox)2]− mononuclear anionic units through one of its two oxalato groups toward a [CuII2(bpy)2(ox)]2+ dinuclear cationic moiety featuring relatively long axial bonds at the square pyramidal CuII ions. Variable temperature (2.0–300 K)…

Intermolecular interactions in dictating the self-assembly of halogen derivatives of bis-(N-substituted oxamato)palladate(ii) complexes

Three palladium(II) complexes of formula (n-Bu4N)2[Pd(4-Fpma)2] (1), (n-Bu4N)2[Pd(4-Clpma)2]·4H2O (2) and (n-Bu4N)2[Pd(4-Brpma)2]·4H2O (3) [n-Bu4N+ = tetra-n-butylammonium cation, 4-Fpma = N-4-fluorophenyloxamate, 4-Clpma = N-4-chlorophenyloxamate and 4-Brpma = N-4-bromophenyloxamate] have been prepared and their structures determined by single crystal X-ray diffraction. Each palladium(II) ion in 1–3 is four-coordinate with two oxygen and two nitrogen atoms from two fully deprotonated oxamate ligands building PdO2N2 square planar surroundings, the oxamate ligands exhibiting trans (1 and 2) and cis (3) dispositions. The fluoro substituent and the organic counterion in 1 are involved in C–H⋯F…

Discrete trinuclear copper(II) compounds as building blocks: the influence of the peripheral substituents on the magnetic coupling in oxamato-bridged complexes.

Two new trinuclear copper(ii) complexes without end-capping ligands, (Bu4N)2[Cu(dmso)2{Cu(dnopba)(dmso)}2] () and (Bu4N)2[Cu(dmso)2{Cu(dcopba)(dmso)}2] () [dnopba = 4,5-dinitro-ortho-phenylenebis(oxamate), dcopba = 4,5-dichloro-ortho-phenylenebis(oxamate), Bu4N(+) = tetra-n-butylammonium and dmso = dimethylsulfoxide], were synthesized and their structures were determined by single crystal X-ray diffraction. The crystal structures of and consist of two outer bis(oxamato)(dmso)cuprate(ii) units which act as bidentate ligands toward a trans-bis(dmso)copper(ii) inner entity leading to centrosymmetric tricopper(ii) complexes with copper-copper separations across the oxamate bridges of 5.1916(3) …

Heterotrimetallic coordination polymers: {Cu(II)Ln(III)Fe(III)} chains and {Ni(II)Ln(III)Fe(III)} layers: synthesis, crystal structures, and magnetic properties.

The use of the [Fe(III) (AA)(CN)4](-) complex anion as metalloligand towards the preformed [Cu(II) (valpn)Ln(III)](3+) or [Ni(II) (valpn)Ln(III) ](3+) heterometallic complex cations (AA=2,2'-bipyridine (bipy) and 1,10-phenathroline (phen); H2 valpn=1,3-propanediyl-bis(2-iminomethylene-6-methoxyphenol)) allowed the preparation of two families of heterotrimetallic complexes: three isostructural 1D coordination polymers of general formula {[Cu(II) (valpn)Ln(III) (H2O)3 (μ-NC)2 Fe(III) (phen)(CN)2 {(μ-NC)Fe(III) (phen)(CN)3}]NO3 ⋅7 H2O}n (Ln=Gd (1), Tb (2), and Dy (3)) and the trinuclear complex [Cu(II) (valpn)La(III) (OH2 )3 (O2 NO)(μ-NC)Fe(III) (phen)(CN)3 ]⋅NO3 ⋅H2O⋅CH3 CN (4) were obtained …

Low-Dimensional 3d–4f Complexes Assembled by Low-Spin [FeIII(phen)(CN)4]− Anions

The synthesis, crystal structure, and magnetic properties of four new mixed 3d-4f complexes with formulas [{FeIII(phen)(CN)4} 4Gd2 III(bpym)(NO3) 2(H2O)4]·2CH3CN· 2H2O}n (1), [{FeIII(phen)(CN)4} 4Tb2 III(bpym)(H2O) 8]·(NO3)2·2CH3CN} n (2), [{FeIII(phen)(CN)4}4Sm III(bpym)(NO3)2(H2O) 5]·2CH3CN}n (3), and [{Fe III(phen)(CN)4}2Pr2 III(bpym)(NO3)4(H2O) 2]n (4) (phen = 1,10-phenanthroline and bpym = 2,2′-bipyrimidine) are discussed here. Compounds 1-3 are isomorphous and their structure consists of neutral ladder-like motifs where the rungs are made up by bpym-bridged dilanthanide(III) cations and the rods are defined by [Fe(phen)(CN)4]- units adopting a bis-monodentate coordination mode through…

Self-assembly of a chiral three-dimensional manganese(II)-copper(II) coordination polymer with a double helical architecture

The use of the anionic dicopper(ii) complex, [CuII(mpba) 2]4- [mpba = N,N′-1,3-phenylenebis(oxamate)], as tetrakis(bidentate) metalloligand toward MnII ions in the presence of oxalate and the chiral (S)-trimethyl-(1-phenylethyl)ammonium cation affords the first example of a mixed oxalato/oxamato-based chiral 3D metal-organic polymer. © 2013 The Royal Society of Chemistry.

All-cis-1,2,3,4,5,6-cyclohexanehexacarboxylate two-dimensional gadolinium(III) complexes: Synthesis, X-ray crystal structure and magnetic properties

Abstract The first gadolinium(III) complexes with the trideprotonated form of the 1,2,3,4,5,6-cyclohexanehexacarboxylic acid (H3clhex3−) of formulae [Gd(H3clhex)(H2O)4]n·3nH2O (1) and [Gd(H3clhex)(H2O)4]n·6nH2O (2) have been prepared through the gel technique and their structures determined by single crystal X-ray diffraction. The structure of 1 is made up of 63 honey-comb layers which are generated by [Gd(H2O)4]3+ cations and H3clhex3− anions acting as three-fold nodes and three-fold connectors, respectively. The structure of 2 consists of a [44,62] two-dimensional network extended in the ac plane where the H3clhex−3 groups act as four-fold connectors and the [Gd(H2O)4]3+ units as four-fol…

Copper(II)-methylmalonate complexes with unidentate N-donor ligands: Syntheses, structural characterization and magnetic properties

Abstract Two new methylmalonate-bridged copper(II) complexes with the formulas [Cu(3-Ipy)(Memal)(H 2 O)] ( 1 ) and [Cu(2,4′-bpy)(Memal)(H 2 O)] · 3H 2 O ( 2 ) [Memal = methylmalonate dianion, 3-Ipy = 3-iodopyridine, 2,4′-bpy = 2,4′-bipyridine] have been synthesized and characterized by X-ray diffraction. Both compounds crystallize in the monoclinic space group P 2 1 / n and Z  = 4, with unit cell parameters a  = 8.5874(13) A, b  = 7.1738(14) A, c  = 19.093(5) A, β  = 99.509(15)° in 1 and a  = 17.375(4) A, b  = 7.3305(14) A, c  = 14.247(3) A, β  = 111.409(15)° in 2 . The structures of 1 and 2 consist of zigzag chains of anti-syn carboxylate-bridged copper(II) ions running along the b directi…

Spin canting in an unprecedented three-dimensional pyrophosphate- and 2,2'-bipyrimidine-bridged cobalt(II) framework.

The three-dimensional cobalt(ii) compound of formula {[Co(2)(P(2)O(7))(bpym)(2)].12H(2)O}(n), where the pyrophosphate and 2,2'-bipyrimidine act as bridging ligands, is a new example of a spin-canted antiferromagnet with T(c) = 19 K.

Dimensionally controlled hydrogen-bonded nanostructures: synthesis, structure, thermal and magnetic behaviour of the tris-(chelated)nickel(II) complex [Ni(bipy)3]Cl2·5.5H2O (bipy=2,2′-bipyridyl)

Abstract Single crystals of the compound of formula [Ni(bipy)3]Cl2·5.5H2O (bipy=2,2′-bipyridine) have been prepared and structurally characterised by X-ray diffraction. The structure analysis reveals that the complex has an approximate D3 symmetry. The coordination sphere consists of six nitrogen atoms of the three-bipyridine ligands in an octahedral arrangement about the nickel. One of the chlorine ions is surrounded by twelve CH⋯Cl hydrogen bonds. Three kinds of layers are found in the crystal structure: (i) the Λ-[Ni(bipy)3]2+ cation; (ii) the water/chloride positions (O(1w)/Cl(21) to O(7w)/Cl(27)); (iii) the Δ-[Ni(bipy)3]2+ cation and a chloride ion (Cl(1)). The layers are stacked in t…

Synthesis crystal structure and magnetic properties of [Fe2(bpym)(C5O5)2(H2O)4]·2H2O and two polymorphs of [Fe2(bpym)(C4O4)2(H2O)6]·2H2O (bpym = 2,2′-bipyrimidine)

Abstract Two dinuclear iron(II) complexes of formulae [Fe2(bpym)(C5O5)2(H2O)4]·2H2O (1) and [Fe2(bpym)(C4O4)2(H2O)6]·2H2O (2) (bpym = 2,2-bipyrimidine, C5O52 = dianion of croconic acid (4,5-dihydroxycylopent-4-ene-1,2,3-trione) and C4O42 = dianion of squaric acid (3,4-dihydroxycyclobut-3-ene-1,2-dione)) were prepared and their crystal structures (at 103 K) determined by X-ray diffraction methods. The structure of 1 consists of neutral centrosymmetric [Fe2(bpym)(C5O5)2(H2O)4] units and water molecules of crystallization which are linked by an extensive network of hydrogen bonds. The coordination geometry around each iron atom is that of a compressed octahedron with bpym nitrogen atoms and cr…

[Fe(phen)(CN)4]−: a suitable metalloligand unit to build 3d–4f heterobimetallic complexes with mixed bpym-cyano bridges (phen = 1,10-phenantroline, bpym = 2,2′-bipyrimidine)

The synthesis, crystal structure and magnetic properties of a new series of mixed 3d–4f complexes with the formula [{FeIII(phen)(CN)3(μ-CN)}4Ln2III(NO3)2(H2O)6(μ-bpym)]·nH2O [Ln = Eu (1), Gd (2), Dy (3) and Ho (4); n = 8 (1, 3 and 4) and 11 (2); phen = 1,10-phenantroline; bpym = 2,2′-bipyrimidine] are discussed here. Compounds 1–4 are centrosymmetric hexanuclear species whose structure is made up of two cyano-bridged {Fe2IIILnIII} heterobimetallic moieties which are connected through a bis-bidentate bpym molecule between the two rare-earth centers. The values of the iron–lanthanide distance across the single cyano-bridge are Fe(1)⋯Eu(1) = 5.5587(8) and Fe(2)⋯Eu(1) = 5.4908(8) A (1), Fe(1)⋯G…

Ferromagnetic Coupling through Spin Polarization in a Dinuclear Copper(II) Metallacyclophane.

[DT] Von organischen Radikalen zu Metallkomplexen konnte das bekannte Konzept für Ferroelektrika erfolgreich ausgedehnt werden: Die Abbildung zeigt ein Cyclophan-artiges Molekül mit einem Triplett-Grundzustand, in dem zwei CuII-Zentren von einem doppelten m-Phenylendiamid-Gerüst zusammengehalten werden.

Europium(III), Terbium(III), and Gadolinium(III) Oxamato-Based Coordination Polymers: Visible Luminescence and Slow Magnetic Relaxation

The reaction of aqueous solutions of EuIII, TbIII, and GdIII ions with Na2Hpcpa [H3pcpa = N-(4-carboxyphenyl)oxamic acid] afforded three new isostructural oxamate-containing lanthanide(III) coordination polymers of general formula {LnIII2(Hpcpa)3(H2O)5·H2O}n [Ln = Eu (1),Tb (2), and Gd(3)]. Their structure is made up of neutral zigzag chains running parallel to the [101] direction where double syn-syn carboxylate(oxamate)-bridged dilanthanide(III) pairs (Ln1 and Ln2) are linked by three Hpcpa2- ligands, one of them with the μ-κ2O,O':κO″ coordination mode and the other two with the μ3-κ2O,O':κO″:κO'''. Additionally, two of those chains are interlinked through hydrogen bonding and π-π type in…

Topology and Spin Polarization in Sheetlike Metal(II) Polymers: [ML2X2] (M ˭ Mn, Fe, Co or Ni, L = Pyrimidine or Pyrazine and X = NCS or NCO)

The preparation and the structural and magnetic characterization of a series of sheetlike transition metal polymers of formula [ML2X2] [M ˭ Mn(II), Fe(II), Co(II) and Ni(II): L = pyrazine (pyz) and...

Cobalt(II)-Copper(II) Bimetallic Chains as a New Class of Single-Chain Magnets

Ferromagnetische Kopplung im zweikernigen Bis(μ-end-on-azido)eisen(III)-Komplexanion von [FeII(bpym)3]2[FeIII(N3)10] · 2H2O

ChemInform Abstract: Formation in Solution, Synthesis and Crystal Structure of μ-Oxalatobis(bis(2-pyridylcarbonyl)amido)dicopper(II).

Abstract The compound μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II), [Cu 2 {(NCsH 5 CO) 2 N} 2 - (C 2 O 4 )] was synthesized and characterized by spectroscopy, EPR and diffraction methods. It crystallizes in the triclinic space group P 1 with cell constants: a =7.6793(6), b =9.238(2), c =10.007(2) A, α=83.80(1), β=68.37(1) and γ=69.44(1)°; V =617.7(3) A 3 , D (calc., Z =2)=1.80 g cm −3 , M r =667.6, F (000)=336, λ, (Mo Kα)=0.71069 A, μ (Mo Kα)=17.895 cm −1 and T =295 K. A total of 3587 data were collected over the range of 1 ⩽ θ ⩽ 30°; of these, 2391 (independent and with I⩾2σ( I )) were used in the structural analysis. The final R and R w residuals were 0.049 and 0.053, respective…

Bis(oxamato)palladate(II) complexes: synthesis, crystal structure and application to catalytic Suzuki reaction

New bis(oxamato)palladate(II) complexes, [Pd(H2O)4][Pd(2,6-Me2pma)2]·2H2O (1), (n-Bu4N)2[Pd(2,6-Me2pma)2]·2H2O (2a), and (n-Bu4N)2[Pd(2,6-Me2pma)2]·2CHCl3 (2b) (2,6-Me2pma = N-2,6-dimethylphenyoxamate and n-Bu4N+ = tetra-n-butylammonium), have been synthesized and the structures of 1 and 2b characterized by single-crystal X-ray diffraction. Complex 1 is a double salt constituted by tetraaquapalladium(II) cations and bis(oxamato)palladate(II) anions interlinked by hydrogen bonds. The palladium(II) ions in 1 are four-coordinate with two oxygens and two nitrogens from two fully deprotonated oxamate ligands (anion), and four water molecules (cation) building centrosymmetric square-planar surrou…

Assembling Magnetic Blocks: A Strategy to Control the Nuclearity and Magnetic Properties of Polynuclear Complexes

Synthetic strategies dealing with the polymerization of either di-μ-hydroxocopper(II) complexes or 2,2′-bipyrimidine (bpym)-containing first row transition metal ions allow the preparation of polynuclear compounds whose structures and magnetic properties are presented here. The influence of structural and chemical parameters on the magnitude of the singlet-triplet energy gap (J) in di-μ-hydroxocopper(II) complexes [LCu(OH)2CuL]2+ with L = 2,2′-bipyridine (bpy) and bpym is analyzed and discussed. Special attention is devoted to nature of the counterion which allows the preparation of hydroxo-bridge copper(II) cubane and double cubane type complexes where all the intramolecular magnetic inter…

Dithiosquarate (dtsq) complexes of nickel(II). Syntheses and crystal structures of [Ni(phen)2(1,2-dtsq)]·3.5H2O, [Ni(phen)2(1,3-dtsq)] and [Ni(tren)(1,2-dtsq)] [phen=1,10-phenanthroline; tren=tris(2-aminoethyl)amine]

Abstract The new nickel(II) complexes [Ni(phen)2(1,2-dtsq)]·3.5H2O (1), [Ni(phen)2(1,3-dtsq)] (2) and [Ni(tren)(1,2-dtsq)] (3) [1,2-dtsq=dianion of 3,4-dimercapto-3-cyclobutene-1,2-dione, 1,3-dtsq=dianion of 3-hydroxy-4-mercapto-2-thioxo-3-cyclobuten-1-one, phen=1,10-phenanthroline and tren=tris(2-aminoethyl)amine] have been synthesized and characterized by single-crystal X-ray diffraction. Their structures are made up of neutral [Ni(phen)2(1,n-dtsq)] [1 (n=2) and 2 n=3)] and [Ni(tren)(1,2-dtsq)] (3) mononuclear units. The nickel atom is six-coordinated in all three cases: four nitrogen atoms from two bidentate phen (1 and 2) or a tetradentate tren (3) groups and either two sulfur (1 and 3)…

Crystal growth and structural remarks on malonate-based lanthanide coordination polymers

The synthesis, structural characterization and thermal study of new coordination polymers (CPs) of formula [Ln2(mal)3(H2O)5]·2H2O [Ln = Ho (1·2H2O), Tb (1a), Dy (1b), Er (1c) and Yb (1d); mal = malonate], [Ln2(mal)3(H2O)6] [Ln = Sm (2) and Ce (2a)], [Ce2(mal)3(H2O)6]·2H2O (3·2H2O) and [Ce2(mal)3(H2O)3]·2H2O (4·2H2O) are presented. Complexes 1–4 have been also characterized by single crystal X-ray diffraction. The structure of 2 was previously reported (Elsegood, M. R. J., Husain, S., Private Communication, 2014) and it is very close to that of 3. In the light of these results and those previously reported in the literature for malonate-containing lanthanide(III) complexes, a detailed overvi…

High-dimensional malonate-based materials: Synthesis, crystal structures and magnetic properties of [M2(mal)2(L)(H2O)2]n·n(H2O) M = Zn(ii), Co(ii); H2mal = malonic acid, L = pyrimidine, pyrazine

Four novel coordination polymers [M2(mal)2(pym)(H2O)]n·nH2O, M = Zn (1), Co (2) and [M2(mal)2(pyz)(H2O)]n·nH2O, M = Zn (3), Co (4) (H2mal = malonic acid, pym = pyrimidine, pyz = pyrazine), have been synthesized. Compounds 1 and 2 are isomorphous, as are compounds 3 and 4. X-ray diffraction experiments reveal that 1–4 exhibit an interesting 3D-network, containing malonate and either pyrimidine (1 and 2) and pyrazine (3 and 4) as organic ligands. Variable-temperature magnetic susceptibility measurements indicate the occurrence of weak antiferromagnetic interactions between Co(II) ions in 2 and 4.

Mononuclear lanthanide(III)-oxamate complexes as new photoluminescent field-induced single-molecule magnets: solid-state photophysical and magnetic properties.

Implementing additional optical (luminescent) properties into the well-known class of single-molecule magnets (SMMs) is considered as a promising route toward obtaining the next generation of optomagnetic materials for quantum information storage and computing. Herein, we report a joint optical and magneto-structural study for the two novel series of lanthanide(iii) complexes of general formula Bu4N[LnIII(HL)4(dmso)]·nH2O where H2L = N-(4-Xphenyl)oxamic acid with X = Cl and n = 2 [Ln = Eu (1_Cl), Gd (2_Cl), Dy (3_Cl), and Tb (4_Cl)] and X = F and n = 3 [Ln = Eu (1_F), Gd (2_F), Dy (3_F), and Tb (4_F)]. All these compounds are mononuclear species with each lanthanide(iii) cation in a low-sym…

Mono-, di- and trinuclear 2,3,5,6-tetrakis(2-pyridyl)pyrazine (tppz)-containing copper(II) complexes: syntheses, crystal structures and magnetic properties.

Three new copper(ii) complexes of formula [Cu(tppz)(NCO)(2)].0.4H(2)O (1), [Cu(2)(tppz)Br(4)](2) and [Cu(3)(tppz)(C(5)O(5))(3)(H(2)O)(3)].7H(2)O (3)[tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine; C(5)O(5)(2-) = croconate, dianion of 4,5-dihydroxycyclopent-4-ene-1,2,3-trione] have been synthesised and structurally characterized by X-ray diffraction methods. The structure of complex is made up of neutral [Cu(tppz)(NCO)(2)] mononuclear units and uncoordinated water molecules. The mononuclear units are grouped by pairs to give a rather short copper-copper distance of 3.9244(4) angstroms. The structure of complex 1 consists of neutral tppz-bridged [Cu(2)(tppz)Br(4)] dinuclear units, the copper-copp…

Novel malonate-containing coordination compounds with ligands having N-And NO-donors: Synthesis, structures, and magnetic properties

In our efforts to tune the structures of mixed-ligands malonate-containing coordination compounds, four copper(II) and two high-spin cobalt(II) complexes of formulas [Cu(mal)(H 2O)(dpo)] n (1), [Cu 2(mal) 2(H 2O) 2(dpp)] n · 7nH 2O (2), [Cu 2(mal) 2(H 2O) 2-(bpe)] n · 2nH 2O (3), {[Cu(mal) 2(H 2O) 2][Cu(dien)]} n · 4nH 2O (4)[Co 2(mal) 2(H 2O) 6(dpo)] ·2H 2O(5) and [Co(mal)(H 2O)(phen)] n · 2nH 2O (6) [H 2mal = malonic acid, dpo =4,4'-bipyridine-N,N'-dioxide, dpp = 2,3-bis(pyridyl)pyrazine, bpe =1,2-bis(4-pyridyl)ethylene, dien = diethylenetriamine and phen = 1,10-phenanthroline] have been synthesized and structurally characterized by X-ray diffraction on single crystals. Complexes 1, 2, 4,…

Towards a better understanding of honeycomb alternating magnetic networks.

Two new two-dimensional homometallic compounds {[M2(bpm)(ox)2]n·5nH2O} with M = Co(II) (1) and Zn(II) (2) and the mononuclear nickel(II) complex [Ni(bpm)2(ox)]·2H2O (3) [bpm = 2,2'-bipyrimidine and ox = oxalate] have been prepared and structurally characterized. 1 and 2 are isostructural compounds whose structures are made up of oxalate-bridged M(II) cations cross-linked by bis-bidentate bpm molecules to afford a honeycomb layered network extending in the crystallographic ab plane. The layers are eclipsed along the crystallographic c axis and show graphitic-like interactions between the bpm rings. The three-dimensional supramolecular network deriving from such interactions is characterized …

[Mnii2(bpym)(H2O)8]4+ and [Miv(CN)8]4– (M = Mo and W) as building blocks in designing bpym- and cyanide-bridged bimetallic three-dimensional networks (bpym = 2,2′-bipyrimidine)Electronic supplementary information (ESI) available: χMT vs. T for 2. See http://www.rsc.org/suppdata/nj/b2/b206124b/

One-pot reaction between the dinuclear [MnII2(bpym)(H2O)8]4+ complex and the mononuclear [MIV(CN)8]4− unit (M = Mo and W; bpym = 2,2′-bipyrimidine) in aqueous solution yields the novel heterobimetallic complexes of formula {(μ-bpym)[Mn(H2O)]2-(μ-NC)6M(CN)2} with M = Mo (1) and W (2). 1 and 2 are isostructural three-dimensional compounds where the manganese atoms are bridged by bisbidentate bpym and hexakismonodentate octacyanometalate units. Variable-temperature magnetic susceptibility data of 1 and 2 show the occurrence of a significant antiferromagnetic coupling between the high spin manganese(II) ions through bridging bpym (Jca. −1.1 cm−1, the exchange Hamiltonian being defined as H = −J…

Structural, spectral, and magnetic properties of end-to-end di-mu-thiocyanato-bridged polymeric complexes of Ni(II) and Co(II). X-ray crystal structure of di-mu-thiocyanatobis(imidazole)nickel(II).

Thiocyanatonickel(II) and thiocyanatocobalt(II) complexes of the composition Ni(NCS)(2)(HIm)(2) (1) and Co(NCS)(2)(HIm)(2) (2), where HIm = imidazole, were prepared and studied. In particular, the crystal structure of Ni(NCS)(2)(HIm)(2) was determined by X-ray methods. This compound crystallizes in the monoclinic system, space group P2(1)/n, with a = 7.720(1) A, b = 5.557(1) A, c = 13.774(3) A, beta = 102.54(3) degrees, and Z = 2. Its structure consists of a one-dimensional polymeric chain in which nickel(II) ions are bridged by two thiocyanate groups bonding in an end-to-end fashion in a trans arrangement. The Ni...Ni distance is 5.557(1) A. The crystal packing is determined by the intermo…

2D and 3D mixed MII/CuIImetal–organic frameworks (M = Ca and Sr) withN,N′-2,6-pyridinebis(oxamate) and oxalate: preparation and magneto-structural study

Three heterobimetallic complexes of formula [Ca2Cu3(mpyba)2(2-apyma)(H2O)7]·8.3H2O (1), [Sr2Cu3(mpyba)2(2-apyma)(H2O)8]·11.6H2O (2) and [Sr4.5Cu4(mpyba)4(ox)(H2O)20]·8.5H2O (3) [H4mpyba = N,N'-2,6-pyridinebis(oxamic acid), 2-apyma = 2-(6-aminopyridinyl)oxamate and ox = oxalate] have been synthesized and structurally characterized. Complexes 1 and 2 are isostructural compounds, with tricopper(ii) units having mpyba and its hydrolytic product (2-apyma) as ligands. They are interlinked through strontium(ii) (1) and calcium(ii) (2) ions to afford neutral two-dimensional networks. Two of the copper(ii) ions are five-coordinate in distorted square pyramidal (Cu3) and trigonal bipyramidal (Cu1) su…

Malonate-based copper(II) coordination compounds: Ferromagnetic coupling controlled by dicarboxylates

Studies on structural and magnetic properties of polynuclear transition metal complexes, aimed at understanding the structural and chemical factors governing electronic exchange coupling mediated by multiatom bridging ligands, are of continuing interest to design new molecular materials exhibiting unusual magnetic, optical and electrical properties, bound to their molecular nature. Looking at potentially flexible bridging ligands, the malonate group seems a suitable candidate. The occurrence of two carboxylate groups in the 1,3 positions allows this ligand to adopt simultaneously chelating bidentate and different carboxylato bridging modes (syn–syn, anti–anti and syn–anti trough one or two …

Synthesis and magnetic properties of bis(μ-hydroxo)bis[(2,2 ′-bipyridyl)copper(II)] squarate. Crystal structure of bis(μ-hydroxo)bis[(2,2′-bipyridyl)copper(II)] squarate tetrahydrate

Abstract The compound [Cu2(bipy)2(OH)2](C4O4)·5.5H2O, where bipy and C4O42− correspond to 2,2′-bipyridyl and squarate (dianion of 3,4-dihydroxy-3-cyclo- butene-1,3-dione) respectively, has been synthesized. Its magnetic properties have been investigated in the 2–300 K temperature range. The ground state is a spin-triplet state, with a singlet-triplet separation of 145 cm−1. The EPR powder spectrum confirms the nature of the ground state. Well-formed single crystals of the tetrahydrate, [Cu2(bipy)2(OH)2](C4O4)·4H2O, were grown from aqueous solutions and characterized by X-ray diffraction. The system is triclinic, space group P 1 , with a = 9.022(2), b = 9.040(2), c = 8.409(2) A, α = 103.51(2…

Synthesis, crystal structure and magnetic properties of an oxalato-bridged Re(IV)Mo(VI) heterobimetallic complex.

The Re(IV)-Mo(VI) compound of formula (PPh(4))(2)[ReCl(4)(μ-ox)MoO(2)Cl(2)] (1) constitutes the first example of a heterodinuclear oxalato-bridged complex in the coordination chemistry of molybdenum.

[Cr(phen)(ox)2]-: a versatile bis-oxalato building block for the design of heteropolymetallic systems. Crystal structures and magnetic properties of AsPh4[Cr(phen)(ox)2]·H2O, [NaCr(phen)(ox)2(H2O)]·2H2O and {[Cr(phen)(ox)2]2[Mn2(bpy)2(H2O)2(ox)]}·6H2O

The new complexes of formula AsPh4[Cr(phen)(ox)2]·H2O (1), [NaCr(phen)(ox)2(H2O)]·2H2O (2) and {[Cr(phen)(ox)2]2[Mn2(bpy)2(H2O)2(ox)]}·6H2O (3) (AsPh4=tetraphenylarsonium cation; phen=1,10-phenanthroline; ox=oxalate dianion; bpy=2,2′-bipyridine) have been prepared and characterized by single-crystal X-ray diffraction. The structure of 1 consists of discrete [Cr(phen)(ox)2]− anions, tetraphenylarsonium cations and uncoordinated water molecules. The chromium environment in 1 is distorted octahedral with Cr–O bond distances between 1.959(3) and 1.947(3) A and Cr–N bonds of 2.083(4) and 2.072(4) A. The angles subtended at the chromium atom by the two oxalates are 83.6(2) and 83.3(1)° whereas th…

Selective Guest Inclusion in Oxalate-Based Iron(III) Magnetic Coordination Polymers

The preparation and structural characterization of four novel oxalate-based iron(III) compounds of formulas {(MeNH3)2[Fe2(ox)2Cl4]·2.5H2O}n (1), K(MeNH3)[Fe(ox)Cl3(H2O)] (2), {MeNH3[Fe2(OH)(ox)2Cl2]·2H2O}n (3), and {(H3O)(MeNH3)[Fe2O(ox)2Cl2]·3H2O}n (4) (MeNH3+ = methylammonium cation and H2ox = oxalic acid) are reported here. 1 is an anionic waving chain of oxalato-bridged iron(III) ions with peripheral chloro ligands, the charge balance being ensured by methylammonium cations. 2 is a mononuclear complex with a bidentate oxalate, three terminal chloro ligands, and a coordinated water molecule achieving the six-coordination around each iron(III) ion. Its negative charge is balanced by potas…

Field-induced slow magnetic relaxation and magnetocaloric effects in an oxalato-bridged gadolinium(iii)-based 2D MOF

The coexistence of field-induced slow magnetic relaxation and moderately large magnetocaloric efficiency in the supra-Kelvin temperature region occurs in the 2D compound [GdIII2(ox)3(H2O)6]n·4nH2O (1), a feature that can be exploited in the proof-of-concept design of a new class of slow-relaxing magnetic materials for cryogenic magnetic refrigeration.

One-dimensional oxalato-bridged copper(II) complexes with 3-hydroxypyridine and 2-amino-4-methylpyridine

Two new one-dimensional oxalato-bridged copper(II) compounds of formula [Cu(ox)L2]n (1) and {[Cu2(ox)2L%3]·L%}n (2) [ox oxalate dianion, L3-hydroxypyridine (pyOH) and L% 2-amino-4-methylpyridine (ampy)] have been synthesized and characterized by FT-IR spectroscopy, variable-temperature magnetic measurements and single-crystal X-ray diffraction. The crystal structure of 1 comprises chains of copper atoms in which cis-[Cu(pyOH)2] 2 units are sequentially bridged by asymmetric bis-bidentate oxalato ligands with an intrachain copper‐copper separation of 5.548(1) A, . Each copper atom is six-coordinated: four oxygen atoms belonging to two bridging oxalato ligands and two nitrogen atoms from two …

Rational design of a new class of heterobimetallic molecule-based magnets: Synthesis, crystal structures, and magnetic properties of oxamato-bridged (M′=LiI and MnII; M=NiII and CoII) open-frameworks with a three-dimensional honeycomb architecture

Abstract Two new series of oxamato-bridged heterobimetallic coordination networks of general formula Li5[Li3M2(mpba)3(H2O)6] · 31H2O [M = NiII (1a) and CoII (1b)] and Li2[Mn3M2(mpba)3(H2O)6] · 22H2O [M = NiII (2a) and CoII (2b)] have been prepared from the metal-mediated self-assembly of the hexakis(bidentate), triple-stranded dinickel(II) and dicobalt(II) complexes [M2(mpba)3]8− [mpba = meta-phenylenebis(oxamato)] with either monovalent lithium(I) or divalent manganese(II) ions respectively, in water. X-ray structural analyses of 1a and 1b show an anionic three-dimensional network formed by an infinite parallel array of oxamato-bridged Li 3 I M 2 II (M = Ni and Co) hexagonal layers, which …

Polyvinylpolypyrrolidone‐Stabilized Copper Nanoparticles as an Efficient and Recyclable Heterogeneous Catalyst for the Click of 1,2,3‐Triazoles in Water

Ferromagnetic Coupling in “Double-Bridged” Dihydrogenpyrophosphate Complexes of Cobalt(II) and Nickel(II)

Three isostructural compounds of the formula {[M(bipy)(H2O)(H2P2O7)]2·2H2O} [bipy = 2,2'-bipyridine; M = Ni (1), Co (2), Mn (3)] have been isolated from aqueous solutions containing the corresponding metal(II) chloride hydrate with a bipy and sodium pyrophosphate solution in a 1:1:2 molar ratio, and their structures were determined by single-crystal X-ray diffraction. The structures of 1-3 consist of neutral aqua(2,2'-bipyridine)metal(II) dinuclear units bridged by two dihydrogenpyrophosphate groups adopting a bidentate/monodentate mode. Each metal ion in 1-3 is six-coordinate in a distorted octahedral geometry, with the reduced value of the angle subtended by the chelating bipy at the meta…

{[Cu(H2O)3][Cu(phmal)2]}n: a new two-dimensional copper(ii) complex with intralayer ferromagnetic interactions (phmal = phenylmalonate dianion)

The novel sheet-like copper(II) compound of formula {[Cu(H2O)3][Cu(Phmal)2]}n (1) (Phmal = dianion of phenylmalonic acid) has been synthesized and its crystal structure determined by X-ray diffraction. The structure of 1 consists of 21 chains of carboxylate(phenylmalonate)-bridged copper(II) ions which are linked through double μ-oxo(carboxylate) units to afford a two-dimensional network. The interlayer space is filled by the phenyl rings of the phenylmalonate ligands that exhibit offset face-to-face interactions. Variable-temperature magnetic measurements of 1 show the occurrence of significant intralayer ferromagnetic interactions between the copper(II) ions through anti–syn carboxylate- …

Metamorphosis of a butterfly: synthesis, structural, thermal, magnetic and DFT characterisation of a ferromagnetically coupled tetranuclear copper(ii) complex

The reaction in water of Cu(OH)(2) with 2,2'-bipyridine (bipy) and (NH(4))(2)HPO(4) in a 4 : 4 : 2 molar ratio under an inert atmosphere leads to the formation of a tetranuclear copper(II) complex of formula {[(H(2)O)(2)Cu(4)(bipy)(4)(mu(4)-PO(4))(2)(mu(2)-OH)] x 0.5 HPO(4) x 15.5 H(2)O}, 1, with butterfly topology. The structure of the tetranuclear core in 1 consists of four crystallographically unique copper(II) ions in approximate square-pyramidal geometry with each coordinated to a bipy ligand and interacting through two mu(4)-O,O',O''-phosphate bridges. Additional bridging between Cu(3) and Cu(4) is provided by a hydroxide ligand, whereas two water molecules cap the Cu(1) and Cu(2) squ…

Enantioselective self-assembly of antiferromagnetic hexacopper(ii) wheels with chiral amino acid oxamates

The Cu(2+)-mediated self-assembly of oxamato-based ligands derived from either the (S)- or (R)-enantiomers of the amino acid valine leads to the formation of two antiferromagnetically coupled homochiral anionic hexacopper(II) wheels in the presence of templating tetramethylammonium countercations.

ChemInform Abstract: Oxamato-Based Coordination Polymers: Recent Advances in Multifunctional Magnetic Materials

The design and synthesis of novel examples of multifunctional magnetic materials based on the so-called coordination polymers (CPs) have become very attractive for chemists and physicists due to their potential applications in nanoscience and nanotechnology. However, their preparation is still an experimental challenge, which requires a deep knowledge of coordination chemistry and large skills in organic chemistry. The recent advances in this field using a molecular-programmed approach based on rational self-assembly methods which fully exploit the versatility of the coordination chemistry of the barely explored and evergreen family of N-substituted aromatic oligo(oxamato) ligands are prese…

Ferromagnetic coupling through the oxalate bridge in heterobimetallic Cr(III)–M(II) (M = Mn and Co) assemblies

Abstract Two novel compounds, {[Cr(pyim)(ox)2]2Mn}n·2nCH3OH (1) and {[Cr(pyim)(ox)2]2Co(H2O)2}·7.5H2O (2) [pyim = 2-(2′-pyridyl)imidazole and H2ox = oxalic acid], were synthesized by using the mononuclear chromium(III) complex PPh4[Cr(pyim)(ox)2]·H2O (PPh4+ = tetraphenylphosphonium) as metalloligand towards the fully solvated manganese(II) (1) and cobalt(II) (2) ions as perchlorate salts. The structure of 1 consists of neutral double chains, with diamond-shaped units sharing the manganese(II) ions with the two other corners being occupied by the chromium(III) ions. The two metal centres in 1 are connected by bis-bidentate oxalate groups, each [CrIII(pyim)(ox)2]− unit being bound to two mang…

Phenylmalonate‐Containing Copper( II ) Complexes: Synthesis, Crystal Structure and Magnetic Properties

Three new copper(II) complexes of formula [Cu(2,2′-bpy)(Phmal)(H2O)]·2H2O (1), [{Cu(2,2′-bpym)(Phmal)}]n (2) and [{Cu(phen)(Phmal)}]n·3nH2O (3) (Phmal = phenylmalonate; 2,2′-bpy = 2,2′-bipyridine; 2,2′-bpym = 2,2′-bipyrimidine; phen = 1,10-phenanthroline) have been prepared and their structures determined by X-ray diffraction techniques. Complex 1 is mononuclear whereas 2 and 3 are uniform chain compounds. The copper atoms in 1−3 are distorted square-pyramidal: two nitrogen atoms from the bidentate nitrogen heterocycle and two carboxylate oxygen atoms from the phenylmalonate ligand build the equatorial plane; the axial position is filled either by a water molecule (1) or a carboxylate oxyge…

Iron(III), chromium(III) and cobalt(II) complexes with squarate: Synthesis, crystal structure and magnetic properties

The preparation and variable temperature-magnetic investigation of three squarate-containing complexes of formula [Fe 2 (OH) 2 (C 4 O 4 ) 2 (H 2 O) 4 ]·2H 2 O ( 1 ) [Cr 2 (OH) 2 (C 4 O 4 ) 2 (H 2 O) 4 ]·2H 2 O ( 2 ) and [Co(C 4 O 4 )(H 2 O) 4 ] n ( 3 ) [H 2 C 4 O 4  = 3.4-dihydroxycyclobutene-1,2-dione (squaric acid)] together with the crystal structures of 1 and 3 are reported. Complex 1 contains discrete centrosymmetric [Fe 2 (OH) 2 (C 4 O 4 ) 2 (H 2 O) 4 ] diiron(II) units where the iron pairs are joined by a di-μ-hydroxo bridge and two squarate ligands acting as bridging groups through adjacent oxygen atoms. Two coordinated water molecules in cis position complete the octahedral environ…

Heterobimetallic single-source precursors for MOCVD. Synthesis and characterization of volatile mixed ligand complexes of lanthanides, barium and magnesium β-diketonates with d-element containing ligands

Several heterobimetallic complexes of general formula [(M 1 Q) m M 2 (dik) n ], where (M 1 Q) is Cu(salen) or Ni(salen) and M 2 (dik) n is a lanthanide tris(β-diketonate) or an alkali-earth element bis(β-diketonate) with more or less fluorinated diketonato(-) ligands, have been prepared and structurally characterized. Some of them were submitted to thermal and mass spectrometry analyses, and to isothermal vacuum sublimation tests, in view of their potential use as MOCVD single-source precursors for the deposition of heterobimetallic materials. The study stresses upon the influence of the nature of the diketone. of the M 2 cation, and of chemical modification of the salen ligand on the therm…

Ligand Effects on the Structure and Magnetic Properties of Alternating Copper(II) Chains with 2,2′-Bipyrimidine- and Polymethyl-Substituted Pyrazolates as Bridging Ligands

A novel series of heteroleptic copper(II) compounds of formulas {[Cu2(μ-H2O)(μ-pz)2(μ-bpm)(ClO4)(H2O)]ClO4·2H2O}n (1), {[Cu2(μ-H2O)(μ-3-Mepz)2(μ-bpm)](ClO4)2·2H2O}n (2), and {[Cu2(μ-OH)(μ-3,5-Me2pz)(μ-bpm)(H-3,5-Me2pz)2](ClO4)2}n (3) [bpm = 2,2'-bipyrimidine, Hpz = pyrazole, H-3-Mepz = 3-methylpyrazole, and H-3,5-Me2pz = 3,5-dimethylpyrazole] have been synthesized and structurally characterized by X-ray diffraction methods. The crystal structures of 1 and 2 consist of copper(II) chains with regular alternating bpm and bis(pyrazolate)(aqua) bridges, whereas that of 3 is made up of copper(II) chains with regular alternating bpm and (pyrazolate)(hydroxo) bridges. The copper centers are six- (1…

{CoIIIMnIII}ncorrugated chains based on heteroleptic cyanido metalloligands

The use of the cyanide-bearing complexes PPh4[CoIII(4,4′-dmbipy)(CN)4] and PPh4[CoII(dmphen)(CN)3] as metalloligands towards [Mn(salen)(H2O)]ClO4 affords one-dimensional coordination polymers with the formulas {[MnIII(salen)(μ-NC)2CoIII(4,4-dmbipy)(CN)2]·H2O}n (1) and {[MnIII(salen)(μ-NC)2CoIII(dmphen)(CN)2]}n (2) [PPh4+ = tetraphenylphosphonium cation, 4,4′-dmbipy = 4,4′-dimethyl-2,2′-bipyridine, dmphen = 2,9-dimethyl-1,10-phenanthroline and H2salen = N,N′-ethylenebis(salicylideneimine)]. Compounds 1 and 2 were structurally characterized. Their structures consist of neutral chains with regular alternating [Mn(salen)]+ and [CoIII(4,4′-dmbipy)(CN)4]− (1)/[CoIII(dmphen)(CN)4]− (2) moieties, t…

A Copper(II)-Cytidine Complex as a Building Unit for the Construction of an Unusual Three-Dimensional Coordination Polymer

The chiral [Cu(cyd) 4 ] 6- anion acts as a multiarmed complex-ligand toward auxiliary copper(II) centers leading to the first example of cytidinate-bridged three-dimensional (3D) coordination polymer of formula [Cu 6 (H 2 O) 7 (ClO 4 ) 3 Cu(cyd) 4 ]-(ClO 4 ) 3 (1). Single crystal X-ray analysis of 1 shows a unique 3D covalent network supported by the exclusive hypercoordination of the cytidinate ligand that bridges four crystallographically independent copper(II) ions via the N3, O2, O2', O3', and O5' set of atoms. Magnetic susceptibility measurements in the temperature range 1.9-295 K reveal the coexistence of ferro- and antiferromagnetic interactions within the hexacopper(II) core of 1, t…

Hyperbranched polyethylenimine-supported copper(II) ions as a macroliganted homogenous catalyst for strict click reactions of azides and alkynes in water

Abstract Loading hyperbranched polyethylenimine (PEI) with copper(II) ions leads to the formation of a new water-soluble metallodendritic polymer Cu(II)-PEI that has been found to effectively catalyze the clickable azide-alkyne [3 + 2] cycloaddition reactions in water under ambient conditions, in the lack of any external reducing agent. A positive dendritic effect on the catalyst activity was observed in the click of 1,2,3-triazole by lowering the reduction potential of copper(II) into the in-situ generation of the catalytically active species copper(I). The reaction proceeds straightforwardly to afford the corresponding 1,4-disubstituted-1,2,3-triazole derivatives in a regioselective manne…

Synthesis, crystal structure and magnetic properties of the complex [ReCl3(tppz)]·MeCN

The reaction of the starting materials [ReIIICl3(MeCN)(PPh3)2] or [ReVOCl3(PPh3)2] with 2,3,5,6-tetrakis(2-pyridyl)pyrazine (tppz) in acetonitrile yielded the Re(III) complex [ReCl3(tppz)]·MeCN (1). This complex crystallizes in the monoclinic space group P21/n and its crystal structure consists of neutral mononuclear entities with meridional geometry of the chloride ligands, and the six-coordination of the Re(III) ion being completed by the tridentate tppz ligand. Each metal centre exhibits a highly distorted octahedral coordination with Re–Cl and Re–Ntppz bond lengths covering the ranges 2.3590(9)–2.3606(8) and 1.971(2)–2.096(2) A, respectively. The magnetic properties of 1 have been inves…

Malonic acid: A multi-modal bridging ligand for new architectures and properties on molecule-based magnets

Abstract In this work, we show how the design of one-, two- and three-dimensional materials can strongly benefit from the use of crystal engineering techniques, which can give rise to structures of different shapes, and how these differences can give rise to different properties. We will focus on the networks constructed by assembling malonate ligands and metal centres. The idea of using malonate (dianion of propanedioic acid, H 2 mal) is that they can give rise to different coordination modes with the metal ions bind. Extended magnetic networks of dimensionalities 1 (1D), 2 (2D) and 3 (3D) can be chemically constructed from malonato-bridged metallic complexes. These coordination polymers b…

Interaction between heterobinuclear molecules and nature of the ground spin state in oximato-bridged [CuIIMII]2 bis-binuclear complexes (M=Cu, Ni, Mn): crystal structure of [Cu(pdmg)Ni(Me3[12]N3)(EtOH)](ClO4)2

[EN] Two new heterobimetallic complexes [Cu(pdmg)Ni(Me-3[12]N-3)(CH3CH2OH)](ClO4)(2)(2) and [Cu(pdmg) Mn(bipy)(2)]-ClO4)(2) . H2O (3) (H(2)pdmg = 3,9-dimethyl-4,8-diazaundeca-3,8-diene-2 10-dione dioxime; Me-3[12]N-3 = 2,4,4-trimethyl-1,5,9-triazacyclododeca-1-ene; bipy = 2,2'-bipyridyl) have been prepared and characterized. The structure of 2 has been determined by single-crystal X-ray diffraction methods. It consists of [Cu(pdmg)Ni(Me-3[12]N-3)(CH3CH2OH)](2+) cations and non-coordinated perchlorate anions. The [Cu(pdmg)(CH3CH2OH)] complex coordinates to the [Ni(Me-3[12]N-3)](2+) fragment to afford the binuclear unit doubly-bridged by oximato groups in cis arrangement. The coordination geo…

Mononuclear and One-Dimensional Cobalt(II) Complexes with the 3,6-Bis(picolylamino)-1,2,4,5-tetrazine Ligand

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[Cr(dpa)(ox)2]–: a new bis-oxalato building block for the design of heteropolymetallic systems. Crystal structures and magnetic properties of PPh4[Cr(dpa)(ox)2], AsPh4[Cr(dpa)(ox)2], Hdpa[Cr(dpa)(ox)2]·4H2O, Rad[Cr(dpa)(ox)2]·H2O and Sr[Cr(dpa)(ox)2]2·8H2O (dpa = 2,2′-dipyridylamine)

[EN] The new complexes of formulae PPh4[Cr(dpa)(ox)(2)] (1), AsPh4[Cr(dpa)(OX)(2)] (2), Hdpa[Cr(dpa)(ox)(2)]-4H(2)O (3), Rad[Cr(dpa)(ox)(2)] . H2O (4) and Sr[Cr(dpa)(ox)(2)](2) . 8H(2)O (5) [PPh4 = tetraphenylphosphonium cation; AsPh4 = tetraphenylarsoniurn cation; dpa = 2,T-dipyridylamine; ox = oxalate dianion; Rad = 2-(4-N-methylpyridinium)4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-a-oxyl-3-N-oxide] have been prepared and characterised by single-crystal X-ray diffraction. The structures of 1-4 consist of discrete [Cr(dpa)(ox)(2)](-) anions, tetraphenylphosphonium. (1), tetraphenylarsonium (2), monoprotonated Hdpa (3) and univalent radical (4) cations and uncoordinated water molecules (2-…

Ligand substitution in hexahalorhenate(IV) complexes: Synthesis, crystal structures and magnetic properties of NBu4[ReX5(DMF)] (X=Cl and Br)

Abstract The preparation, crystal structures, and magnetic properties of two rhenium(IV) mononuclear compounds of formula NBu 4 [ReX 5 (DMF)] ( NBu 4 + = tetrabutylammonium cation and DMF = N , N - dimethylformamide ) with X = Cl ( 1 ) and Br ( 2 ) are reported. 1 and 2 are isostructural complexes which crystallize in the monoclinic system with the space group P 2 1 / n . The rhenium atom is six-coordinated with five X atoms and a DMF molecule forming a somewhat distorted octahedral surrounding [values of Re–X varying in the ranges 2.317(1)–2.358(1) ( 1 ) and 2.495(1)–2.518(1) A ( 2 )]. Magnetic susceptibility measurements on samples of 1 and 2 in the temperature range 1.9–300 K are interpr…

First Magnetostructural Study on a Heterodinuclear 2,2′-Bipyrimidine-Bridged Complex

The use of the [ReCl(4)(bpym)] precursor as a ligand toward the fully solvated nickel(II) metal ion affords the first example of a 2,2'-bipyrimidine-bridged Re(IV)-Ni(II) complex, [ReCl(4)(μ-bpym)NiBr(2)(H(2)O)(2)] (1), whose intramolecular ferromagnetic coupling has been substantiated from both experimental and theoretical studies.

Intramolecular ferro- and antiferromagnetic interactions in oxo-carboxylate bridged digadolinium(iii) complexes

Two new digadolinium(III) complexes with monocarboxylate ligands, [Gd2(pac)6(H2O)4] (1) and [Gd2(tpac)6(H2O)4] (2) (Hpac = pentanoic acid and Htpac = 3-thiopheneacetic acid), have been prepared and their structures determined by X-ray diffraction on single crystals. Their structures consist of neutral and isolated digadolinium(III) units, containing six monocarboxylate ligands and four coordinated water molecules, the bridging skeleton being built by a muO(1):kappa2O(1)O(2) framework. This structural pattern has already been observed in the parent acetate-containing compound [Gd2(ac)6(H2O)4] x 4 H2O (3) whose structure and magnetic properties were reported elsewhere (L. Cañadillas-Delgado, …

Magneto-structural correlations in asymmetric oxalato-bridged dicopper(II) complexes with polymethyl-substituted pyrazole ligands

Two oxalato-bridged dinuclear copper(II) complexes, [{Cu(Hdmpz)3}2(μ-ox)](ClO4)2·2H2O (1) and [{Cu(Htmpz)3}2(μ-ox)](ClO4)2·2H2O (2) (Hdmpz = 3,5-dimethyl-1H-pyrazole and Htmpz = 3,4,5-trimethyl-1H-pyrazole), have been synthesized and structurally and magnetically characterized. The crystal structures of 1 and 2 consist of asymmetric bis-bidentate μ-oxalatodicopper(II) complex cations with two short [Cu–O = 1.976(2) (1) and 1.973(2) Å (2)] and two long copper–oxygen bonds [Cu–O = 2.122(2) (1) and 2.110(2) Å (2)]. The environment at each CuII ion in 1 and 2 is closer to the trigonal bipyramidal geometry than to the square pyramidal [τ = 0.633 (1) and 0.711 (2)]. The magnetic properties of 1 a…

Ferromagnetic coupling in the malonato-bridged copper(ii) chains [Cu(Im)2(mal)]nand [Cu(2-MeIm)2(mal)]n(H2mal = malonic acid, Im = imidazole and 2-MeIm = 2-methylimidazole)

Two new malonato-bridged copper(II) complexes of formula [Cu(Im)2(mal)]n (1) and [Cu(2-MeIm)2(mal)]n (2) (Im=imidazole, 2-MeIm=2-methylimidazole and mal=malonate dianion) have been prepared and their structures solved by X-ray diffraction methods. The [Cu(Im)2(mal)] and [Cu(2-MeIm)2(mal)] neutral entities act as monodentate ligands towards the adjacent copper(II) units through one of the two carboxylate groups, the OCO bridge exhibiting an anti-anti conformation. The environment of each copper atom in 1 and 2 is distorted square pyramidal: two carboxylate oxygen atoms from a bidentate malonate and two nitrogen atoms from two imidazole (1) or 2-methylimidazole (2) ligands form the equatorial…

Synthesis and structural characterization of well-defined bis(oxamato)palladate(II) precatalysts for Suzuki and Heck reactions

Abstract A family of tetra-n-butylammonium salts of bis(oxamato)palladate(II) complexes of formula (n-Bu4N)2[Pd(Lm)2]·pH2O [m = 1–9; L1 = N-phenyloxamate (pma) and p = 2 (1), L2 = N-2-methylphenyloxamate (2-Mepma) and p = 4 (2), L3 = N-4-methylphenyloxamate (4-Mepma) and p = 2 (3), L4 = N-2,3-dimethylphenyloxamate (2,3-Me2pma) and p = 3 (4), L5 = N-2,4-dimethylphenyloxamate (Me2pma) and p = 4 (5), L6 = N-2,5-dimethylphenyloxamate (2,5-Me2pma) and p = 7 (6), L7 = N-3,4-dimethylphenyloxamate (3,4-Me2pma) and p = 6 (7), L8 = N-3,5-dimethylphenyloxamate (3,5-Me2pma) and p = 5 (8)] have been prepared and characterized by spectroscopic methods. The crystal structure of 1 that has been solved by s…

Synthesis, Structural, Thermal and Magnetic Characterization of a Pyrophosphato‐Bridged Cobalt(II) Complex

The reaction in water of CoII sulfate heptahydrate with 1,10-phenanthroline (phen) and sodium pyrophosphate (Na4P2O7) in a 2:4:1 stoichiometric ratio resulted in the crystallization of a neutral dinuclear CoII complex, {[Co(phen)2]2(μ-P2O7)}·6MeOH (1), as revealed by a single-crystal X-ray diffraction study. The bridging pyrophosphato ligand between the two [Co(phen)2]2+ units in a bis(bidentate) coordination mode places the adjacent metal centers at 4.857 A distance, and its conformation gives rise to intramolecular π–π stacking interaction between adjacent phen ligands. Indeed, intermolecular π–π stacking interactions between phen ligands from adjacent dinuclear complexes create a supramo…

A step further in the comprehension of the magnetic coupling in gadolinium(III)-based carboxylate complexes

Three new gadolinium(III) complexes of formula [Gd4(bta) 3(H2O)16]n·12nH2O (1), [Gd4(bta)3(H2O)12] n·18nH2O (2) and [Gd2(H 2bta)(bta)(H2O)2]n·4nH 2O (3) (H4bta = 1,2,4,5-benzenetetracarboxylic acid) have been synthesized and their structures determined by X-ray diffraction. 1 and 3 are three-dimensional compounds whereas 2 exhibits a two-dimensional structure. The ability of the bta4- to adopt different coordination modes accounts for these high dimensionalities although it precludes a rational structural design. The structures of 1-3 have in common the double oxo-carboxylate bridge between gadolinium(III) ions (μ-O: κ2O,O′) either as a discrete units (1 and 2) or as a chain (3) and one (3)…

Structural and Magnetic Characterization of a Novel Heptanuclear Hydroxo-Bridged Copper(II) Cluster of the Corner-Sharing Dicubane Type

New family of thiocyanate-bridged Re(IV)-SCN-M(II) (M = Ni, Co, Fe, and Mn) heterobimetallic compounds: synthesis, crystal structure, and magnetic properties.

The heterobimetallic complexes of formula [(Me(2)phen)(2)M(μ-NCS)Re(NCS)(5)]·CH(3)CN [Me(2)phen = 2,9-dimethyl-1,10-phenanthroline and M = Ni (1), Co (2), Fe (3), and Mn (4)] have been prepared, and their crystal structures have been determined by X-ray diffraction on single crystals. Compounds 1-4 crystallize in the monoclinic C2/c space group, and their structure consists of neutral [(Me(2)phen)(2)M(μ-NCS)Re(NCS)(5)] heterodinuclear units with a Re-SCN-M bridge. Each Re(IV) ion in this series is six-coordinated with one sulfur and five nitrogen atoms from six thiocyanate groups building a somewhat distorted octahedral environment, whereas the M(II) metal ions are five-coordinated with fou…

Coligand Effects on the Field-Induced Double Slow Magnetic Relaxation in Six-Coordinate Cobalt(II) Single-Ion Magnets (SIMs) with Positive Magnetic Anisotropy.

Two mononuclear cobalt(II) compounds of formula [Co(dmphen)2(OOCPh)]ClO4·1/2H2O·1/2CH3OH (1) and [Co(dmbipy)2(OOCPh)]ClO4 (2) (dmphen = 2,9-dimethyl-1,10-phenanthroline, dmbipy = 6,6'-dimethyl-2,2'-bipyridine and HOOCPh = benzoic acid) are prepared and magnetostructurally investigated. Each cobalt(II) ion is six-coordinate with a distorted octahedral CoN4O2 environment. The complex cations are interlinked leading to supramolecular chains (1) and pairs (2) that grow along the crystallographic c-axis with racemic mixtures of (Δ,Λ)-Co units. FIRMS allowed us to directly measure the zero-field splitting between the two lowest Kramers doublets, which led to axial anisotropy values of 58.3 cm-1 ≤…

Three different types of bridging ligands in a 3d-3d'-3d'' heterotrimetallic chain.

A one-pot synthesis of a 3d–3d′–3d′′ heterotrimetallic coordination polymer with double diphenoxido, single cyanido and bis-bidentate oxalate as alternating bridges which exhibits an overall antiferromagnetic behaviour has been developed.

Study of the mutual influence of ligands in cobalt(II) complexes containing thiocyanate and imidazole derivatives

Abstract The cobalt(II) complexes of formula [Co(NCS)2L2] and [Co(NCS)2L′4] (L = imidazole (iz) derivatives, I-Meiz (1), Z-Meiz (2), 2-Etiz (3), 2-Isopropiz (4), 2-Pheniz (5), 1,2-Me2iz (6), Biz (7), 2-Mebiz (8), 2-Etbiz (9); L′ = iz (10), 1-Meiz (11)) have been synthesized and characterized by spectroscopic methods and magnetic measurements. The crystal and molecular structures of complexes 6 and 11 have been determined by X-ray diffraction methods. Complex 6 crystallizes inthe orthorhombic space group Pnma with cell constants a=9.209 (3), b = 12.462 (5), c = 14.851(3) A ; V = 1704.3(9) A 3 , D ( calc ., Z = 4) = 1.43 g cm −3 , M r =367.35, F(000)=640 , λ( Mo K α)=0.71079 A , μ=11.2 cm−1 a…

Alternierende ferro- und antiferromagnetische Austauschwechselwirkungen in einem kettenförmigen CuII-Koordinationspolymer

Crystal Engineering Applied to Modulate the Structure and Magnetic Properties of Oxamate Complexes Containing the [Cu(bpca)]+ Cation

This work deals with the crystal engineering features of four related copper(II)-based compounds with formulas {[{Cu(bpca)}2(H2ppba)]·1.33DMF·0.66DMSO}n (2), [{Cu(bpca)(H2O)}2(H2ppba)] (3), [{Cu(bpca)}2(H2ppba)]·DMSO (4), and [{Cu(bpca)}2(H2ppba)]·6H2O (5) [H4ppba = N,N′-1,4-phenylenebis(oxamic acid) and Hbpca = bis(2-pyridylcarbonyl)amide] and how their distinct molecular and crystal structures translate into their different magnetic properties. 2 and 3 were obtained through the hydrolytic reaction of the double-stranded oxamato-based dipalladium(II) paracyclophane precursor of formula [{K4(H2O)2}{Pd2(ppba)2}] (1) with the mononuclear copper(II) complex [Cu(bpca)(H2O)2]+, either in a water…

Squarate and croconate in designing one- and two-dimensional oxamidato-bridged copper(II) complexes: synthesis, crystal structures and magnetic properties of 〚Cu 2 (apox)(C 4 O 4 )(H 2 O) 2 〛 n · n H 2 O and 〚Cu 4 (apox) 2 (C 5 O 5 ) 2 〛·6 H 2 O

Abstract The reaction of squarate (C4O42–, dianion of 3,4-dihydroxycyclobut-3-ene-1,2-dione) and croconate (C5O52–, dianion of 4,5-dihydroxycyclopent-4-ene-1,2,3-trione) with the dinuclear 〚Cu2(apox)〛2+ copper(II) complex 〚H2apox = N,N’-bis(3-aminopropyl)oxamide〛 in aqueous solution affords the compounds of formula 〚Cu2(apox)(C4O4)(H2O)2〛n·n H2O (1) and 〚Cu4(apox)2(C5O5)2〛·6 H2O (2). Crystals of 1 are monoclinic, space group C2/c, with a = 12.5527(9), b = 7.4161(6), c = 18.5198(12) A, β = 100.578(6)° and Z = 4. Crystals of 2 are triclinic, space group P 1 with a = 9.732(5), b = 9.795(2), c = 10.285(3) A, α = 84.95(2), β = 77.30(3), γ = 85.61(3)° and Z = 1. The structure of complex 1 consist…

Ferromagnetic coupling in a one-dimensional molecular railroad copper(II) azido compound containing a defective double cubane motif.

The compound [Cu2(bpm)2(N3)4]n (bpm = bis(pyrazol-1−yl)methane) shows three unique coordination modes (μ1,1-, μ1,1,1-, μ1,1,3-N3) and ferromagnetic interaction between the copper(II) ions. The structure of the compound exhibits a one-dimensional railroad polymer made up of repeating defective dicubane-type units linked by μ1,1,3-N3 bridges.

On the magneto-structural role of the coordinating anion in oxamato-bridged copper(ii) derivatives

We herein present the synthesis, spectroscopic analysis, description of the crystal structures and magnetic properties of four new complexes of the formula [{Cu(opba)(H2O)1.2}{Cu(dmphen)(SCN)}2]·dmf (1), [{Cu(opba)}2{Cu(dmphen)Cl}4]·1.5dmf·2.5dmso (2), [{Cu(opba)}2{Cu(dmphen)Br}4]·dmf·2.3dmso (3) and [{Cu(opba)}{Cu(dmphen)(dca)}2]n (4) [H4opba = N,N′-1,2-phenylenebis(oxamic acid), dmphen = 2,9-dimethyl-1,10-phenanthroline and dca = dicyanamide anion]. 1 is a neutral tricopper(II) complex where an inner [Cu(opba)]2− fragment adopts a bis-bidentate coordination mode towards two outer [Cu(dmphen)(NCS)]+ units. 2 and 3 are bis-trinuclear species where two oxamato-bridged [Cu(opba){Cu(dmphen)X}2…

[Cr(bpym)(C2O4)2]− in designing heterometallic complexes. Crystal structures and magnetic properties of PPh4[Cr(bpym)(C2O4)2]·H2O and [Ag(bpym)][Cr(C2O4)2](H2O)2]·2H2O (bpym=2,2′-bipyrimidine)

Abstract The preparation, crystal structure and magnetic properties of PPh 4 [Cr(bpym)(C 2 O 4 ) 2 ]·H 2 O ( 1 ) and [Ag(bpym)][Cr(C 2 O 4 ) 2 (H 2 O) 2 ]·2H 2 O ( 2 ) (C 2 O 4  2− =oxalate dianion, bpym=2,2′-bipyrimidine and PPh 4  + =tetraphenylphosphonium cation) are described. The structure of 1 is made up of discrete (2,2′-bipyrimidine)bis(oxalato)chromate(III) anions, teraphenylphosphonium cations and uncoordinated water molecules. The structure of 2 consists chains of univalent silver cations bridged by bis-chelating 2,2′-bypyrimidine, cis -diaquabis(oxalato)chromate(III) anions and crystallisation water molecules. The chromium atom in 1 and 2 has a slightly distorted octahedral geom…

Field-induced single ion magnet behaviour of discrete and one-dimensional complexes containing [bis(1-methylimidazol-2-yl)ketone]-cobalt(II) building units.

International audience; We describe herein the first examples of six-coordinate CoII single-ion magnets (SIMs) based on the β-diimine Mebik ligand [Mebik = bis(1-methylimidazol-2-yl)ketone]: two mononuclear [CoII(Rbik)2L2] complexes and one mixed-valence {CoIII2CoII}n chain of formulas [CoII(Mebik)(H2O)(dmso)(μ-NC)2CoIII2(μ-2,5-dpp)(CN)6]n·1.4nH2O (3) [L = NCS (1), NCSe (2) and 2,5-dpp = 2,5-bis(2-pyridyl)pyrazine (3)]. Two bidentate Mebik molecules plus two monodentate N-coordinated pseudohalide groups in cis positions build somewhat distorted octahedral surroundings around the high-spin cobalt(II) ions in 1 and 2. The diamagnetic [CoIII2(μ-2,5-dpp)(CN)8]2− metalloligand coordinates the pa…

Protonated malonate: the influence of the hydrogen bonds on the magnetic behaviour

One hydrogen malonato-bridged complex of formula [Cu(Hmal)2] (1) and two polymorphous malonato-bridged complexes of formula [Cu(H2O)(H2mal)(mal)] (2 and 3), in which the three species of the malonate (H2mal, Hmal−, and mal2−) are present, were synthesised and characterized by X-ray diffraction [H2mal = malonic acid]. Their structures consist of corrugated malonate layers of [Cu(Hmal)2] (1) and [Cu(H2O)(H2mal)(mal)] (2 and 3) units bridged by carboxylate–malonate groups. The layers are linked through hydrogen bonds leading to a three-dimensional network. Variable-temperature (1.9–290 K) magnetic susceptibility measurements indicate the occurrence of weak ferromagnetic interactions between th…

Crystal engineering of 3-D coordination polymers by pillaring ferromagnetic copper(ii)-methylmalonate layers

Three new copper(II) complexes of formula [Cu(Memal)(H2O)]n (1), [Cu2(pyz)(Memal)2] (2) and [Cu2(4,4′-bpy)(Memal)2(H2O)2] (3) (Memal = methylmalonate, pyz = pyrazine and 4,4′-bpy = 4,4′-bipyridine) were obtained and structurally characterized by X-ray diffraction. Complex 1 is a square grid of aquacopper(II) units which are linked by carboxylate-methylmalonate groups in the anti–syn (equatorial–equatorial) coordination mode. The crystal structures of 2 and 3 consist of corrugated layers of copper(II) (2) and aquacopper(II) (3) units with intralayer carboxylate-methylmalonate bridges in the anti–syn (equatorial–apical) coordination mode which are linked through pyrazine (2) and 4,4′-bipyridi…

Metamagnetism in hydrophobically induced carboxylate (phenylmalonate)-bridged copper(II) layers

Self-assembly of copper(II) ions, phenylmalonate and pyrimidine yields the layered compound [Cu(pym)(Phmal)]n ( 1) where intralayer ferro- and interlayer antiferromagnetic interactions occur with three-dimensional antiferromagnetic ordering at Tc = 2.15 K Lloret Pastor, Francisco, Francisco.Lloret@uv.es ; Julve Olcina, Miguel, Miguel.Julve@uv.es

A combined computational and experimental study on the mild steel corrosion inhibition in hydrochloric acid by new multifunctional phosphonic acid containing 1,2,3-triazoles

Two triazole derivatives with phosphonic acid as pendent group, namely [3-(4-phenyl-[1–3]triazol-1-yl)-propyl]-phosphonicaciddiethylester (PTP) and [3-[4-(4-dimethylamino-phenyl)-[1–3]triazol-1-yl]-propyl]-phosphonic acid diethylester (DMPTP) were synthesized and fully characterized using NMR spectroscopy, Mass spectrometry, Infra-Red (FT-IR) spectroscopy and elemental analysis. The synthesized multifunctional heterocycles were investigated to inhibit the corrosion of mild steel in acidic solution HCl (1 M) by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization (PDP) and weight loss measurements. The results of the different corrosion measurement techniques are in goo…

A heteropentanuclear oxalato-bridged [ReIV 4GdIII] complex: synthesis, crystal structure and magnetic properties

The compound (NBu 4) 5[Gd III{Re IVBr 4(μ-ox)} 4(H 2O)]·H 2O (1), with intramolecular antiferromagnetic coupling, is the first Re(iv) system incorporating a 4f ion. © 2012 The Royal Society of Chemistry.

Solid‐State Anion–Guest Encapsulation by Metallosupramolecular Capsules Made from Two Tetranuclear Copper(II) Complexes

A new cationic tetranuclear copper(II) complex self-assembles from one 1,3-phenylenebis(oxamato) (mpba) bridging ligand and four CuII ions partially blocked with N,N,N′,N′-tetramethylethylenediamine (tmen) terminal ligands. In the solid state, two of these tetracopper(II) oxamato complexes of bowl-like shape and helical conformation then serve as a building block for the generation of either hetero- (MP) or homochiral (MM/PP) dimeric capsules depending on the nature of the encapsulated anion guest, perchlorate or hexafluorophosphate. The overall magnetic behaviour of these metallosupramolecular capsules does not depend on the nature of the encapsulated anion guest, but it is consistent with…

Enhancing the Magnetic Coupling of Oxalato-Bridged ReIV2MII (M = Mn, Co, Ni, and Cu) Trinuclear Complexes via Peripheral Halide Ligand Effects

Four heterotrinuclear Re(IV)(2)M(II) compounds of general formula (NBu(4))(2)[{Re(IV)Br(4)(μ-ox)}(2)M(II)(Him)(2)] [NBu(4)(+) = tetra-n-butylammonium cation, ox = oxalate, Him = imidazole; M = Mn (1), Co (2), Ni (3), and Cu (4)] have been synthesized by using the novel mononuclear complex [Re(IV)Br(4)(ox)](2-) as a ligand toward divalent first-row transition metal ions in the presence of imidazole. Compounds 1-4 are isostructural complexes whose structure contains discrete trinuclear [{Re(IV)Br(4)(μ-ox)}(2)M(II)(Him)(2)](2-) anions and bulky NBu(4)(+) cations. The Re and M atoms are six-coordinated: four peripheral bromo and two oxalate-oxygens (at Re), and two cis-coordinated imidazole mol…

Ligand Design for Heterobimetallic Single-Chain Magnets: Synthesis, Crystal Structures, and Magnetic Properties of MIICuII (M=Mn, Co) Chains with Sterically Hindered Methyl-Substituted Phenyloxamate Bridging Ligands

Two new series of neutral ox-amato-bridged heterobimetallic chains of general formula [MCu(L x ) 2 ]- m DMSO (m=0-4) (L 1 =N-2-methyl-phenyloxamate, M=Mn (1a) and Co (1 b); L2 = N-2,6-dimethylphenyloxamate, M=Mn (2a) and Co (2b); L 3 = N-2,4,6-trimethylphenyloxamate, M= Mn (3a) and Co (3b)) have been prepared by reaction between the corresponding anionic oxamatocopper(II) complexes [Cu(L x ) 2 ] 2- with Mn 2+ or Co 2+ cations in DMSO. The crystal structures of [CoCu(L 2 ) 2 (H 2 O) 2 ] (2b') and [CoCu(L 3 ) 2 (H 2 O) 2 ]·4H 2 O (3b') have been solved by single-crystal X-ray diffraction methods. Compounds 2b' and 3b' adopt zigzag and linear chain structures, respectively. The intrachain Cu··…

Magnetic Molecular Conductors Based on Bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) and the Tris(chlorocyananilato)ferrate(III) Complex

Electrocrystallization of the bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) organic donor in the presence of the [Fe(ClCNAn)3]3– tris(chlorocyananilato)ferrate(III) paramagnetic anion in different stoichiometric ratios and solvent mixtures afforded two different hybrid systems formulated as [BEDT-TTF]4[Fe(ClCNAn)3]·3H2O (1) and [BEDT-TTF]5[Fe(ClCNAn)3]2·2CH3CN (2) (An = anilato). Compounds 1 and 2 present unusual structures without the typical segregated organic and inorganic layers, where layers of 1 are formed by Λ and Δ enantiomers of the anionic paramagnetic complex together with mixed-valence BEDT-TTF tetramers, while layers of 2 are formed by Λ and Δ enantiomers of the paramagnetic…

Ferromagnetic Coupling in the Bis(μ-end-on-azido)iron(III) Dinuclear Complex Anion of[FeII(bpym)3]2[Fe2III(N3)10]·2H2O

A two-dimensional oxamate- and oxalate-bridged Cu(II)Mn(II) motif: crystal structure and magnetic properties of (Bu4N)2[Mn2{Cu(opba)}2ox].

A new compound of formula (Bu4N)2[Mn2{Cu(opba)}2ox] (1) [Bu4N(+) = tetra-n-butylammonium cation, H4opba = 1,2-phenylenebis(oxamic acid), and H2ox = oxalic acid] has been synthesized and magneto-structurally investigated. The reaction of manganese(II) acetate, [Cu(opba)](2-), and ox(2-) in dimethyl sulfoxide yielded single crystals of 1. The structure of 1 consists of heterobimetallic oxamato-bridged Cu(II)Mn(II) chains which are connected through bis-bidentate oxalate coordinated to the manganese(II) ions to afford anionic heterobimetallic layers of 6(3)-hcb net topology. The layers are interleaved by n-Bu4N(+) counterions. Each copper(II) ion in 1 is four-coordinate in a square planar envi…

Recent advances in copper-based solid heterogeneous catalysts for azide-alkyne cycloaddition reactions

The copper(I)-catalyzed azide−alkyne cycloaddition (CuAAC) reaction is considered to be the most representative ligation process within the context of the “click chemistry” concept. This CuAAC reaction, which yields compounds containing a 1,2,3-triazole core, has become relevant in the construction of biologically complex systems, bioconjugation strategies, and supramolecular and material sciences. Although many CuAAC reactions are performed under homogenous conditions, heterogenous copper-based catalytic systems are gaining exponential interest, relying on the easy removal, recovery, and reusability of catalytically copper species. The present review covers the most recently developed copp…

Towards oxalate-bridged iron(ii), cobalt(ii), nickel(ii) and zinc(ii) complexes through oxotris(oxalato)niobate(v): an open air non-oxidizing synthetic route

Four compounds with the formula [M2(dmphen)4(μ-C2O4)](ClO4)2·2dmso [M = Fe (1), Co (2) and Zn (4); dmphen = 2,9-dimethyl-1,10-phenanthroline] and [Ni2(dmphen)4(μ-C2O4)]3[NbO(C2O4)3]2·16H2O (3) have been synthesized using the tris(oxalato)oxoniobate(V) complex anion as the oxalate source, and their structures have been determined by single crystal X-ray diffraction. X-ray quality crystals of highly insoluble oxalate-bridged species were obtained by taking advantage of the slow release of oxalate by the tris(oxalato)oxoniobate(V) complex anion. The structures of 1–4 all contain oxalate-bridged dimetal(II) units with didentate dmphen molecules acting as end-cap ligands; electroneutrality is ac…

Structural changes in the crystal packing of highly hindered symmetrical vicinal bis-amides

The crystal structures of 1,4-bis(3,5-di-tert-butyl-2-hydroxybenzamido)butane (1) and 1,3-bis(3,5-di-tert-butyl-2-hydroxybenzamido)-2,2-dimethylpropane (2) have being characterized by single crystal X-ray diffraction. Their crystal packing is discussed in terms of the different interactions they exhibit. A brief discussion, based on hydrogen bonds, on the structural features of bis-(3,5-di-tert-butyl-2-hydroxybenzamide) compounds is carried out.

Neutron diffraction studies of the molecular compound [Co 2(bta)]n (H4bta =1,2,4,5-benzenetetracarboxylic acid): In the quest of canted ferromagnetism

The exchange mechanism and magnetic structure of the organic-inorganic layered molecule-based magnet [Co2(bta)]n (1) (H 4bta =1,2,4,5-benzenetetracarboxylic acid) have been investigated through variable-temperature magnetic susceptibility measurements and supported with a series of neutron diffraction experiments. Cryomagnetic studies have shown an antiferromagnetic ordering at a transition temperature of 16 K that is followed by the appearance of a weak ferromagnetism below 11 K. The weak antiferromagnetic interlayer interaction plays an important role in this system in spite of the long interlayer separation. A ferromagnetic ordering is induced by applied magnetic fields greater than 1800…

Dicopper(II) Metallacyclophanes with Electroswitchable Polymethyl-Substitutedpara-Phenylene Spacers

Double-stranded anionic dinuclear copper(II) metallacyclic complexes of the paracyclophane type [Cu2L2]4- have been prepared by the CuII-mediated self-assembly of different para-phenylenebis(oxamato) bridging ligands with either zero-, one-, or four-electron-donating methyl substituents (L=N,N′-para- phenylenebis(oxamate) (ppba; 1), 2-methyl- N,N′-para-phenylenebis(oxamate) (Meppba; 2), and 2,3,5,6-tetramethyl- N,N′-para-phenylenebis(oxamate) (Me4ppba; 3)). These complexes have been isolated as their tetra-n-butylammonium (1 a-3 a), lithium(I) (1 b-3 b), and tetraphenylphosphonium salts (1 c-3 c). The X-ray crystal structures of 1 a and 3 c show a parallel-displaced π-stacked conformation w…

Dicopper(II) Anthraquinophanes as Multielectron Reservoirs for Oxidation and Reduction: A Joint Experimental and Theoretical Study

Two new dinuclear copper(II) metallacyclophanes with 1,4-disubstituted 9,10-anthraquinonebis(oxamate) bridging ligands are reported that can reversibly take and release electrons at the redox-active ligand and metal sites, respectively, to give the corresponding mono- and bis(semiquinonate and/or catecholate) Cu(II)2 species and mixed-valent Cu(II)/Cu(III) and high-valent Cu(III)2 ones. Density functional calculations allow us to give further insights on the dual ligand- and metal-based character of the redox processes in this novel family of antiferromagnetically coupled di- copper(II) anthraquinophanes. This unique ability for charge storage could be the basis for the development of new k…

Building-block process for the synthesis of new chromium(iii) malonate complexes

We describe the crystal structures of two bimetallic compounds with the malonate and an exo-polydentate N-donor ligand {[Cu(tren)]4[Cr2(mal)4(OH)2]}(ClO4)4·8H2O (3) and [Ni(Htren)2][Cr2(mal)4(OH)2]·8H2O (4) which are prepared from the dinuclear K4[Cr2(mal)4(OH)2]·6H2O precursor (2) [tren = tris(2-aminoethyl)amine and H2mal = malonic acid]. Their crystal packing and supramolecular structures are analyzed in the context of the influence of the dichromium(III) [Cr2(mal)4(OH)2]4− unit, which acts as a building-block. Different supramolecular motifs built up from hydrogen bonds are discussed, and their self-assembly to yield a 3D arrangement is described. The magnetic properties of the compounds…

Coordinating and hydrogen bonding ability of a bifunctional 2D paddle-wheel copper(II) coordination polymer

abstract A new copper(II) complex of formula {[Cu 2 (H 2 btc) 2 (dmf) 2 ] 4dmf} n (1)[H 4 btc = 1,2,4,5-benzenetetracarb-oxylic acid, dmf = dimethylformamide] has been synthesised and its structure determined by X-raydiffraction. The structure displays a new square grid of ‘‘paddle-wheel’’ tetracarboxylate-bridgeddicopper(II) units with an intradimer copper–copper separation of 2.619(2) A. The dmf molecules areretained through weak axial coordinative bonds and hydrogen bonding interactions with the carboxylicgroups of the porous neutral network of 4 4 net topology. The magnetic behaviour of 1 corresponds to astrong antiferromagnetic coupling within each dicopper(II) unit (J = 343 cm 1 with …

Synthesis, X‐ray Crystal Structure and Magnetic Properties of Oxalato‐Bridged Copper( II ) Complexes with 2,3‐Bis(2‐pyridyl)pyrazine, 2,3‐Bis(2‐pyridyl)quinoxaline and 2,2′‐Bipyrazine as Peripheral Ligands

Five oxalate-containing copper(II) complexes of formula [Cu(dpq)(H2O)(ox)]·5H2O (1), [Cu(dpp)(H2O)(ox)]·H2O (2), [Cu(bpz)(ox)]n (3), [Cu2(dpp)2(H2O)2(NO3)2(ox)]·4H2O (4) and [Cu2Cl2(bpz)2(H2O)2(ox)][Cu(bpz)(H2O)2(ox)]·2H2O (5) [dpq = 2,3-bis(2-pyridyl)quinoxaline; dpp = 2,3-bis(2-pyridyl)pyrazine; bpz = 2,2′-bipyrazine; ox = oxalate] were prepared and their structures were determined by X-ray diffraction on single crystals. Complexes 1 and 2 are discrete mononuclear complexes with oxalate and dpq (1)/dpp (2) acting as bidentate ligands. Complex 3 is a neutral oxalato-bridged (2,2′-bipyrazine)copper(II) chain where the oxalate adopts a bidentate/monodentate coordination mode, whereas 4 is an…

Mono- and Binuclear Copper(II) and Nickel(II) Complexes with the 3,6-Bis(picolylamino)-1,2,4,5-Tetrazine Ligand

Four new compounds of formulas [Cu(hfac)2(L)] (1), [Ni(hfac)2(L)] (2), [{Cu(hfac)2}2(µ-L)]·2CH3OH (3) and [{Ni(hfac)2}2(µ-L)]·2CH3CN (4) [Hhfac = hexafluoroacetylacetone and L = 3,6-bis(picolylamino)-1,2,4,5-tetrazine] have been prepared and their structures determined by X-ray diffraction on single crystals. Compounds 1 and 2 are isostructural mononuclear complexes where the metal ions [copper(II) (1) and nickel(II) (2)] are six-coordinated in distorted octahedral MN2O4 surroundings which are built by two bidentate hfac ligands plus another bidentate L molecule. This last ligand coordinates to the metal ions through the nitrogen atoms of the picolylamine fragment. Compounds 3 and 4 are cen…

Synthesis Crystal Structure and Magnetic Properties of the Trinuclear Nickel(II) Complex Bis[(μ-thiocyanato-N)bis(μ-pyridazine-N1,N2)bis(thiocyanato-N)(pyridazine-N1)nickel(II)- N,N1,N1‘]nickel(II)

Unusual single N-bridging thiocyanato and double pyridazine (pdz) bridges occur in the linear trinuclear nickel(II) complex of formula [Ni3(pdz)6(NCS)6]. The compound exhibits a quasi Curie law behavior, the antiferromagnetic coupling through the double 1,2-diazine links being nearly compensated by the ferromagnetic exchange through the single N-bridging thiocyanato.

Two-Dimensional Assembling of (2,2‘-Bipyrimidine)bis(oxalato)chromate(III) Units through Alkaline Cations

Self-assembling of the tris-chelated [Cr(bpm)(ox)2]- complex with Na+ in aqueous solution leads to the remarkable bimetallic honeycomb layered compound of formula [NaICrIII(bpm)(ox)2]·5H2O (2) (bpm...

[Fe(III)(dmbpy)(CN)4]-: a new building block for designing single-chain magnets.

We herein present the synthesis and magneto-structural study of a new family of heterobimetallic chains of general formula {[Fe(III)(dmbpy)(CN)(4)](2)M(II)(H(2)O)(2)}(n)·pnH(2)O [dmbpy = 4,4'-dimethyl-2,2'-bipyridine; M = Mn (2), Cu (3), Ni (4) and Co (5) with p = 4 (2), 3 (3), 9 (4) and 3.5 (5)] which were prepared by using the mononuclear PPh(4)[Fe(III)(dmbpy)(CN)(4)]·3H(2)O (1) building block (PPh(4)(+) = tetraphenylphosphonium) as a ligand toward fully solvated M(II) ions. The structure of 1 consists of discrete [Fe(III)(dmbpy)(CN)(4)](-) anions, tetraphenylphosphonium cations and noncoordinated water molecules. Complexes 2-5 are isostructural compounds whose structure consists of neutr…

Copper(II) complexes with 2,5-bis(2-pyridyl)pyrazine and oxalate and croconate: Synthesis, crystal structure and magnetic properties

Abstract Two new copper(II) complexes of formula [Cu2(2,5-dpp)(C2O4)2(H2O)4] (1) and [Cu2(2,5-dpp)(C5O5)2(H2O)4]·3H2O (2) [2,5-dpp = 2,5-bis(2-pyridyl)pyrazine, C2O42− = oxalate and C5O52− = croconate (dianion of 4,5-dihydroxycyclopent-4-ene-1,2,3-trione)] have been prepared and their structures determined by X-ray crystallographic methods. Compounds 1 and 2 are dinuclear complexes where the 2,5-dpp molecule acts as a bis-bidentate bridge between the two copper(II) ions, the electroneutrality being achieved by the presence of bidentate oxalate (1) and croconate (2) ligands. Each copper(II) ion exhibits an elongated octahedral CuN2O4 environment with two nitrogen atoms from 2,5-dpp and two o…

Supramolecular coordination chemistry of aromatic polyoxalamide ligands: A metallosupramolecular approach toward functional magnetic materials

Abstract The impressive potential of the metallosupramolecular approach in designing new functional magnetic materials constitutes a great scientific challenge for the chemical research community that requires an interdisciplinary collaboration. New fundamental concepts and future applications in nanoscience and nanotechnology will emerge from the study of magnetism as a supramolecular function in metallosupramolecular chemistry. Our recent work on the rich supramolecular coordination chemistry of a novel family of aromatic polyoxalamide (APOXA) ligands with first-row transition metal ions has allowed us to move one step further in the rational design of metallosupramolecular assemblies of …

Cobalt(II) and copper(II) assembling through a functionalized oxamate-type ligand

Two new metal complexes of formula {[Co(Hpcpa)(H2O)3]n� 3/2nH2O} (1) and [Cu2(MeHpcpa)4(MeOH)2] � H2O� 3.68 MeOH (2 )[ H 3pcpa = N-(4-carboxyphenyl)oxamic acid and MeH2pcpa = methyl ester derivative of H3pcpa] have been synthesized and their structures determined by X-ray diffraction. 1 is a neutral zigzag chain of cobalt(II) ions bridged by Hpcpa 2� ligands exhibiting the bidentate/monodentate coordination mode. Each cobalt(II) ion is six-coordinate with three mer positioned water molecules, two oxamate-oxygens from a Hpcpa 2� ligand and a carboxylate-oxygen from another Hpcpa 2� group building a somewhat distorted octahedral surrounding. The intrachain cobalt–cobalt separation is 11.326(2…

Dicopper(II) Metallacyclophanes with Oligo(p-phenylene-ethynylene) Spacers: Experimental Foundations and Theoretical Predictions on Potential Molecular Magnetic Wires

Two novel double-stranded dicopper(II) metallacyclophanes of formula (nBu4N)4[Cu2(dpeba)2]·4MeOH·2Et2O (1) and (nBu4N)4[Cu2(tpeba)2]·12H2O (2) have been prepared by the Cu(II)-mediated self-assembly of the rigid ('rod-like') bridging ligands N,N'-4,4'-diphenylethynebis(oxamate) (dpeba) and N,N'-1,4-di(4-phenylethynyl)phenylenebis(oxamate) (tpeba), respectively. Single crystal X-ray diffraction analysis of 1 confirms the presence of a dicopper(II)tetraaza[3.3]4,4'-diphenylethynophane metallacyclic structure featuring a very long intermetallic distance between the two square planar Cu(II) ions [r = 14.95(1) Å]. The overall parallel-displaced π-stacked conformation of the two nearly planar par…

[Cu3(Hmesox)3]3−: a Precursor for the Rational Design of Chiral Molecule-Based Magnets (H4mesox = 2-dihydroxymalonic acid)

Two new compounds K(3)[Cu(3)(Hmesox)(3)(H(2)O)] x 4 H(2)O (1) and {(PPh(4))(2)[CoCu(3)(Hmesox)(3)Cl]} (2) [H(4)mesox = mesoxalic acid (2-dihydroxymalonic acid) and PPh(4)(+) = tetraphenylphosphonium cation] have been prepared and magneto-structurally characterized. Compound 1 contains the [Cu(3)(Hmesox)(3)](3-) entity which can be considered as a new precursor for molecular magnetism. In 1 the triangular arrangement of three copper(II) ions bridged by alkoxo groups are further connected to a symmetry-related tricopper(II) unit through a double oxo(carboxylate) bridge. The resulting hexacopper(II) entities are joined further through anti-syn carboxylate groups into an anionic three-dimension…

ChemInform Abstract: Synthesis and Magnetic Properties of Bis(μ-hydroxo)bis((2,2′-bipyridyl)copper(II)) Squarate. Crystal Structure of Bis(μ-hydroxo)bis((2,2′-bipyridyl)copper(II)) Squarate Tetrahydrate.

Abstract The compound [Cu2(bipy)2(OH)2](C4O4)·5.5H2O, where bipy and C4O42− correspond to 2,2′-bipyridyl and squarate (dianion of 3,4-dihydroxy-3-cyclo- butene-1,3-dione) respectively, has been synthesized. Its magnetic properties have been investigated in the 2–300 K temperature range. The ground state is a spin-triplet state, with a singlet-triplet separation of 145 cm−1. The EPR powder spectrum confirms the nature of the ground state. Well-formed single crystals of the tetrahydrate, [Cu2(bipy)2(OH)2](C4O4)·4H2O, were grown from aqueous solutions and characterized by X-ray diffraction. The system is triclinic, space group P 1 , with a = 9.022(2), b = 9.040(2), c = 8.409(2) A, α = 103.51(2…

Oxalate, squarate and croconate complexes with bis(2-pyrimidylcarbonyl)amidatecopper(II): synthesis, crystal structures and magnetic properties

Abstract The preparation and magnetic properties of three copper(II) compounds of formulae [Cu2(bpcam)2(H2O)2(C2O4)] (1), [Cu2(bpcam)2(H2O)4(C4O4)] · 10 H2O (2) and Cu2(bpcam)2(C5O5)(H2O)3 (3) [bpcam = bis(2-pyrimidyl)amidate, C 2 O 4 2 - = dianion of oxalic acid , C 4 O 4 2 - = dianion of 3 , 4 - dihydroxycyclobut - 3 - ene - 1 , 2 - dione and C 5 O 5 2 - = dianion of 4 , 5 - dihydroxycyclopent - 4 - ene - 1 , 2 , 3 - trione ] are reported. The structures of two of them (1 and 2) have been solved by single crystal X-ray diffraction and consists of centrosymmetric discrete copper(II) dinuclear units bridged by bis-bidentate oxalate (1) and bis-monodentate squarate (2), with the bpcam group …

Copper(II)-phenylmalonate complexes with the bifunctional ligands nicotinamide and isonicotinamide

Abstract The use as coligands of the nicotinamide (nia) and isonicotinamide (inia) molecules in the complex formation between copper(II) and phenylmalonate [Phmal = dianion of phenylmalonic acid] yielded the compounds of formula [Cu(inia)(Phmal)(H2O)] (1) and [Cu(inia)(Phmal)(H2O)]n (2). Although single crystals of 1 of appropriate size were grown, their unresolved twinning and space group ambiguity prevented a satisfactory X-ray structure determination. The crystal structure 2 consists of corrugated layers of copper(II) ions with intralayer carboxylate–phenylmalonate bridges in the anti-syn (equatorial-apical) coordination mode. A water molecule and the isonicotinamide group are coordinate…

Relatively strong intramolecular antiferromagnetic coupling in a neutral Cr(III)2Nb(V)2 heterobimetallic molecular square.

A relatively large antiferromagnetic interaction between the two chromium(III) ions from the molecular square [{Cr(dmso)4}2{Nb(μ-O)2(C2O4)2}2] () (J = -12.0 cm(-1)) is mediated by the diamagnetic oxo-Nb(V)-oxo pathway, its nature and magnitude being substantiated by DFT type theoretical calculations.

Spin control in oxamato-based manganese(II)-copper(II) coordination polymers with brick-wall layer architectures.

Two new heterobimetallic manganese(II)-copper(II) coordination polymers of formulas [Mn(2)Cu(2)(Me(3)mpba)(2)(H(2)O)(6)]·8H(2)O (1) and [Mn(2)Cu(2)(Me(4)ppba)(2)(H(2)O)(6)]·8H(2)O (2) [Me(3)mpba = 2,4,6-trimethyl-N,N'-1,3-phenylenebis(oxamate) and Me(4)ppba = 2,3,5,6-tetramethyl-N,N'-1,4-phenylenebis(oxamate)] have been synthesized following a molecular-programmed self-assembly method from the corresponding dicopper(II) complexes acting as metalloligands toward Mn(II) ions. 1 and 2 consist of neutral Mn(II)(2)Cu(II)(2) layers with a brick-wall structure made up of oxamato-bridged Mn(II)Cu(II) chains connected through double meta- (1) and para-substituted (2) permethylated phenylene spacers.…

Cyanido‐Bearing Cobalt(II/III) Metalloligands – Synthesis, Crystal Structure, and Magnetic Properties

New examples of cyanido-bearing cobalt(III/II) complexes have been obtained by treatment of CoCl2·6H2O with bidentate nitrogen donors and potassium cyanide in a methanol/water mixture. Depending on the chelating ligand, the cobalt(III) complexes PPh4[Co(en)(CN)4] (1, en = ethylenediamine), PPh4[Co(ampy)(CN)4]·1.5H2O [2, ampy = 2-(aminomethyl)pyridine], and PPh4[Co(phen)(CN)4]·CH3OH·0.25H2O (3, phen = 1,10-phenanthroline) and the cobalt(II) complex PPh4[Co(dmphen)(CN)3]·3H2O (4, dmphen = 2,9-dimethyl-1,10-phenanthroline) were obtained. The complexes were characterized by single-crystal X-ray diffraction and variable-temperature magnetic measurements. They are all mononuclear species with six…

A heterobimetallic [MnII5CuII5] nanowheel modulated by a flexible bis-oxamate type ligand

The synthesis, crystal structure and preliminary magnetic characterization of a new heterobimetallic [MnII5CuII5] wheel containing a flexible bis-oxamate type ligand are described. This decanuclear compound exhibits a relatively strong intra-wheel antiferromagnetic interaction leading to a ground spin state S = 10.

Well-resolved unusual alternating cyclic water tetramers embedded in a crystal host

Infinite network involving two hydrogen-bonded tetrameric water rings (S4 and D2h) in a (4,4)-square grid crystal host

Hexakis(diethylacetamide)iron(II) hexahalorhenate(IV) ionic salts: X-ray structures and magnetic properties

Two novel Fe<sup>II</sup>-Re<sup>IV</sup> compounds of general formula [Fe<sup>II</sup>(DEA)<inf>6</inf>][Re<sup>IV</sup>X<inf>6</inf>] where DEA = diethylacetamide and X = Cl (1) and Br (2) have been prepared and magnetostructurally characterised. Complexes 1 and 2 are isomorphic ionic salts that crystallise in the trigonal crystal system with space group R(-3). The rhenium(IV) ion in 1 and 2 is six-coordinate with six chloro (1) or bromo (2) ligands building a regular octahedral chromophore. The Fe<sup>II</sup> ion is also six-coordinate, and bonded to six oxygen atoms from six DEA molecules. [Fe<sup&gt…

Magneto-structural correlations in Ni(ii) [2 × 2] metallogrids featuring a variable number of μ-aquo or μ-hydroxo extra bridges

Four new [2 × 2] grid-type metallosupramolecular species have been obtained by using the ditopic 3,6-bis(2′-pyridyl)pyridazine ligand (dppn) and nickel(II) salts containing poorly coordinating anions. Three of them have the formula [Ni4(μ-dppn)4(μ-OH)2(μ-H2O)2]X6·nH2O [with X = ClO4− (1), NO3− (2) and CF3SO3− (3), and n = 6.5 (1), 14 (2) and 4 (3)]. Their crystal structure shows the same tetranuclear core, constituted by four six-coordinate metal ions and four dppn molecules. Two hydroxo groups and two water molecules efficiently interact forming two hydrated hydroxide (H3O2−) supramolecular bridging anions, further stabilizing the grid. The other compound, [Ni4(μ-dppn)4(μ-OH)3(μ-H2O)](ClO4…

Thermodynamics of the two-dimensional Heisenberg classical honeycomb lattice

In this article we adapt a previous work concerning the two-dimensional (2D) Heisenberg classical square lattice [Physica B 245, 263 (1998)] to the case of a honeycomb lattice. Closed-form expressions of the main thermodynamic functions of interest are derived in the zero-field limit. Notably, near absolute zero (i.e., the critical temperature), we derive the values of the critical exponents $\ensuremath{\alpha}=0,\ensuremath{\eta}=\ensuremath{-}1,\ensuremath{\gamma}=3,$ and $\ensuremath{\nu}=1,$ as for the square lattice, thus proving their universal character. A very simple model allows one to give a good description of the low-temperature behaviors of the product $\ensuremath{\chi}T.$ Fo…

Ferromagnetic coupling and spin canting behaviour in heterobimetallic ReIVMII/III(M = CoII/III, NiII) species

Three novel heterobimetallic Re(IV) compounds of formulae [ReBr(4)(μ-ox)M(4,7-Cl(2)phen)(2)]·CH(3)CN·CH(3)NO(2) [M = Co(II) (1) and Ni(II) (2)] and [ReBr(4)(ox)](3)[Co(III)(5,6-dmphen)(3)](2)·CH(3)CN·2CH(3)NO(2)·4H(2)O (3) [ox = oxalate, 4,7-Cl(2)phen = 4,7-dichloro-1,10-phenanthroline and 5,6-dmphen = 5,6-dimethyl-1,10-phenanthroline] have been synthesised and the structures of 1 and 3 determined by single crystal X-ray diffraction. Compound 1 is an oxalato-bridged Re(IV)Co(II) heterodinuclear complex where the [ReBr(4)(ox)](2-) unit acts as a bidentate ligand towards the [Co(4,7-Cl(2)phen)(2)](2+) entity, the separation between Re(IV) and Co(II) across the oxalate being 5.482(1) Å. Compou…

Study of the influence of the bridge on the magnetic coupling in cobalt(II) complexes.

Two new cobalt(II) complexes of formula [Co(2)(bta)(H(2)O)(6)](n) x 2nH(2)O (1) and [Co(phda)(H(2)O)](n) x nH(2)O (2) [H(4)bta = 1,2,4,5-benzenetetracarboxylic acid, H(2)phda = 1,4-phenylenediacetic acid] have been characterized by single crystal X-ray diffraction. Compound 1 is a one-dimensional compound where the bta(4-) ligand acts as 2-fold connector between the cobalt(II) ions through two carboxylate groups in para-conformation. Triply bridged dicobalt(II) units occur within each chain, a water molecule, a carboxylate group in the syn-syn conformation, and an oxo-carboxylate with the mu(2)O(1);kappa(2)O(1),O(2) coordination mode acting as bridges. Compound 2 is a three-dimensional comp…

An approach to polymer-supported triplet benzophenone photocatalysts. Application to sustainable photocatalysis of an α-diazocarbonyl compound

Covalent immobilization of 4-hydroxybenzophenone on Merrifield resins affords new heterogeneous polymeric triplet photocatalysts. Their successful application in the intramolecular triplet-sensitized photolysis of a α-diazo β-keto ester has been achieved under sustainable criteria. Remarkably, the simple recovery and reuse for up to five sequential applications have been performed, although resulting in a slightly decreasing activity.

Oligo-m-phenyleneoxalamide Copper(II) Mesocates as Electro-Switchable Ferromagnetic Metal–Organic Wires

Double-stranded copper(II) string complexes of varying nuclearity, from di- to tetranuclear species, have been prepared by the CuII-mediated self-assembly of a novel family of linear homo- and heteropolytopic ligands that contain two outer oxamato and either zero (1 b), one (2 b), or two (3 b) inner oxamidato donor groups separated by rigid 2-methyl-1,3-phenylene spacers. The X-ray crystal structures of these CuIIn complexes (n=2 (1 d), 3 (2 d), and 4 (3 d)) show a linear array of metal atoms with an overall twisted coordination geometry for both the outer CuN2O2 and inner CuN4 chromophores. Two such nonplanar all-syn bridging ligands 1 b–3 b in an anti arrangement clamp around the metal ce…

Oxalate and 2,2′-bipyrimidine as bis-chelating ligands in the honeycomb layered compound {[Fe2(bpym)(ox)2]·5H2O}n

The novel two-dimensional iron(II) compound of formula {[Fe2(bpym)(ox)2]·5H2O}n (1) [bpym = 2,2′-bipyrimidine and ox = oxalate dianion] is obtained by reaction of oxalic acid, iron(II) chloride and 2,2′-bipyrimidine in aqueous solution. The structure of 1 is made up of oxalato-bridged iron(II) chains cross-linked by bischelating bpym affording a honeycomb lattice. Variable-temperature magnetic susceptibility data of 1 show the occurrence of relatively large antiferromagnetic interactions between the high spin iron(II) ions separated by more than 5.5 A through bridging bpym [Jbpym = −4.0(2) cm−1] and ox [Jox = ca. −7.8(2) cm−1] ligands. These values compare well with those obtained in the ir…

Coordination chemistry of N,N′-bis(coordinating group substituted)oxamides: a rational design of nuclearity tailored polynuclear complexes

Abstract The coordinating properties of N , N ′-bis(coordinating group substituted)oxamides have been thoroughly investigated both in aqueous solution and in the solid state. The easy cis – trans isomerization equilibria that they exhibit together with the great variety of N , N ′-substituents which can be used to play on the overall charge, complexing ability and polarity, make them very suitable ligands in designing homo- and heterometallic species. The knowledge of their complex formation in aqueous solution by potentiometry and using the hydrogen ion concentration as a probe, allowed us to settle the basis of a rational design of oxamidate-containing polynuclear species whose nuclearity…

A new mixed-valence hexanuclear cobalt complex, [Co4IICo2III(dea)2(Hdea)4)(piv)4](ClO4)2·H2O: Synthesis, crystal structure and magnetic properties

A new Co II /Co III hexanuclear complex, [Co 4 II Co 2 III (dea) 2 (Hdea) 4 )(piv) 4 ](ClO 4 ) 2 ·H 2 O 1 , has been obtained by reacting cobalt(II) perchlorate, diethanolamine, and pivalic acid (H 2 dea = diethanolamine and piv = pivalato anion). The cobalt ions are held together by four μ 3 and four μ 2 alkoxo bridges as well as by four syn – syn carboxylato groups. The hexanuclear motif contains four Co(II) and two Co(III) ions. The {Co II 4 Co III 2 (μ 2 -O) 4 (μ 3 -O) 4 } core can be described as a four face-sharing monovacant and bivacant distorted heterocubane units. The cobalt(III) ions are hexacoordinated. Two of the cobalt(II) are hexacoordinated, while the two others are pentacoo…

2,2′-Bipyrimidin(oxalato)kupfer(II)-Komplexe: vom einkernigen Komplex zum zweidimensionalen Schichtpolymer

Synthesis, crystal structure and magnetic properties of a novel heterobimetallic rhenium(IV)-dysprosium(III) chain.

The use of the mononuclear rhenium(IV) precursor [ReBr5 (H2 pydc)](-) (H2 pydc=3,5-pyridinedicarboxylic acid) as a metalloligand towards dysprosium(III) afforded the first heterobimetallic Re(IV) -Dy(III) complex. Crystal structures and static and dynamic magnetic properties of both rhenium-containing species are reported herein. The 5d-4f compound shows an extended 1D structure and the AC magnetic measurements reveal frequency dependence at low temperature suggesting slow relaxation of the magnetization.

Magnetostructural relationships in polymorphic ethylmalonate-containing copper(ii) coordination polymers

Three ethylmalonate-containing copper(II) chiral complexes of the formula {[Cu(H2O)4][Cu(Etmal)2(H2O)]}n (1), [Cu(Etmal)(H2O)]n (2) and {[Cu(Etmal)(H2O)]·H2O}n (3) (H2Etmal = ethylmalonic acid) were obtained by reacting copper(II) nitrate trihydrate, ethylmalonic acid and sodium carbonate in water. Compound 1 is a chiral zigzag chain with regular alternation of [Cu(Etmal)2(H2O)]2− and [Cu(H2O)4]2+ units, the former acting as bis-monodentate ligands toward the latter ones through the two carboxylate groups. The chirality of 1 is a result of the [Cu(Etmal)2(H2O)]2− fragment whose five-coordinate copper(II) surrounding exhibits the Δ or Λ conformation within the Δ or Λ-crystals. The structure …

Metal-organic coordination frameworks based on mixed methylmalonate and 4,4′-bipiridine ligands: synthesis, crystal structure and magnetic properties

Five new complexes of formulae [M2(4,4′-bpy)(Memal)2X2]n [M = Fe(III) (2), Mn(II) (3), Co(II) (4), Ni(II) (5) and Zn(II) (6), and X = Cl−/OH− (2) and H2O (3–6); 4,4′-bpy = 4,4′-bipyridine and Memal = methylmalonate dianion] have been synthesized by following the previously reported procedure for [Cu2(4,4′-bpy)(Memal)2(H2O)2]n (1). Moreover, two new phases of the Cu(II)/Memal/4,4′-bpy system, namely {[Cu(4,4′-bpy)2][Cu(4,4′-bpy)2(Memal)(NO3)(H2O)]}n·nNO3·3.5nH2O (7) and [Cu(4,4′-bpy)2(Memal)(H2O)]n·nH2O (8), were obtained by varying the synthetic conditions. They were all structurally characterized by single crystal X-ray diffraction, and the magnetic properties of 2–5, 7 and 8 were investig…

Slow magnetic relaxation in a hydrogen-bonded 2D array of mononuclear dysprosium(III) oxamates.

The reaction of N-(2,6-dimethylphenyl)oxamic acid with dysprosium(III) ions in a controlled basic media afforded the first example of a mononuclear lanthanide oxamate complex exhibiting a field-induced slow magnetic relaxation behavior typical of single-ion magnets (SIMs). The hydrogen-bond-mediated self-assembly of this new bifunctional dysprosium(III) SIM in the solid state provides a unique example of 2D hydrogen-bonded polymer with a herringbone net topology.

Slow relaxation of the magnetization in a 4,2-wavelike Fe(III)2Co(II) heterobimetallic chain.

The reaction of the low-spin iron(III) complex [Fe(dmbpy)(CN)(4)](-) (1) with fully solvated cobalt(II) ions affords the cyanide-bridged heterobimetallic chain {[Fe(III)(dmbpy)(CN)(4)](2)Co(II)(H(2)O)(2)}(n) · 4nH(2)O (2), which exhibits intrachain ferromagnetic coupling and double slow relaxation of the magnetization.

Reversible solvatomagnetic switching in a single-ion magnet from an entatic state

We have developed a new strategy for the design and synthesis of multifunctional molecular materials showing reversible magnetic and optical switching.

Alternating cationic–anionic layers in the [Mii(H2O)6][Cuii(mal)2(H2O)] complexes linked through hydrogen bonds (M = Mn, Co, Ni, Cu and Zn; H2mal = malonic acid)

The compounds of formula [MII(H2O)6][CuII(mal)2(H2O)2] [M = Mn (1), Co (2), Ni (3), Cu (4), Zn (5) and H2mal = malonic acid] have been prepared and structurally characterised. Each compound adopts a structure where the layers of [Cu(mal)2(H2O)2]2− anions alternate with layers of [M(H2O)6]2+ cations. The layers are linked to each other through hydrogen bonds affording a three-dimensional network. A quasi-Curie law behaviour is observed for the complexes 1–5 in the temperature range 2.0–298 K.

Synthesis, crystal structure and magnetic properties of the helical oxalate-bridged copper(II) chain {[(CH3)4N]2[Cu(C2O4)2] · H2O}n

Abstract The preparation, crystal structure and magnetic properties of a new oxalate-containing copper(II) chain of formula {[(CH3)4N]2[Cu(C2O4)2] · H2O}n (1) [(CH3)4N+ = tetramethylammonium cation] are reported. The structure of 1 consists of anionic oxalate-bridged copper(II) chains, tetramethylammoniun cations and crystallization water molecules. Each copper(II) ion in 1 is surrounded by three oxalate ligands, one being bidentate and the other two exhibiting bis-bidenate coordination modes. Although all the tris-chelated copper(II) units from a given chain exhibit the same helicity, adjacent chains have opposite helicities and then an achiral structure results. Variable-temperature magne…

Titelbild: Cyanide-Bridged Iron(III)–Cobalt(II) Double Zigzag Ferromagnetic Chains: Two New Molecular Magnetic Nanowires (Angew. Chem. 13/2003)

Nuclearity controlled cyanide-bridged bimetallic CrIII-MnII compounds: synthesis, crystal structures, magnetic properties and theoretical calculations.

The preparation, X-ray crystallography and magnetic investigation of the compounds PPh4[Cr(bipy)(CN)4].2 CH3CN.H2O (1) (mononuclear), [[Cr(bipy)(CN)4]2Mn-(H2O)4].4H2O (2) (trinuclear), [[Cr(bipy)(CN)4]2Mn(H2O)2] (3) (chain) and [[Cr(bipy)(CN)4]2Mn(H2O)].H2O.CH3CN (4) (double chain) [bipy=2,2'-bipyridine; PPh4 (+)=tetraphenylphosphonium] are described herein. The [Cr(bipy)(CN)4]- unit act either as a monodentate (2) or bis-monodentate (3) ligand toward the manganese atom through one (2) or two (3) of its four cyanide groups. The manganese atom is six-coordinate with two (2) or four (3) cyanide nitrogens and four (2) or two (3) water molecules building a distorted octahedral environment. In 4…

From Mononuclear Compounds to [2 × 2] Metallogrids: Ferromagnetically Coupled Systems Built by Nickel(II) and 3,6-Bis(2′-pyridyl)pyridazine (dppn)

Mono-, di-, tri-, and tetranuclear compounds of nickel(II) of formula [Ni(dppn)3](NCS)2·0.5dppn (1), [{Ni(dppn)(NCS)}2(μ-dppn)(μ-NCS)]NCS (2), [Ni3(dppn)2(N3)2(μ-dppn)2(μ-N3)2](ClO4)2·CH3CH2OH·2H2O...

Ligand effects on the structures and magnetic properties of tricyanomethanide-containing copper(II) complexes.

The preparation, crystal structure and magnetic properties of four heteroleptic copper(II) complexes with the tricyanomethanide (tcm(-)) and the heterocyclic nitrogen donors 3,6-bis(2-pyridyl)pyridazine (dppn), 2,5-bis(2-pyridyl)pyrazine (2,5-dpp), 2,3-bis(2-pyridyl)pyrazine (2,3-dpp) and 2,3-bis(2-pyridyl)quinoxaline (2,3-dpq) are reported, {[Cu(2)(dppn)(OH)(tcm)(2)] x tcm}(n) (1), {[Cu(2,5-dpp)(tcm)] x tcm}(n) (2), {[Cu(2)(2,3-dpp)(2)(tcm)(3)(H(2)O)(0.5)] x tcm x 0.5H(2)O}(n) (3) and [Cu(2,3-dpq)(tcm)(2)](n) (4). 1 has a ladder-like structure with single mu-1,5-tcm ligands forming the sides and a bis-bidentate dppn and a single mu-hydroxo providing the rung. Each copper atom in 1 exhibits…

Field-Induced Hysteresis and Quantum Tunneling of the Magnetization in a Mononuclear Manganese(III) Complex

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Synthesis, crystal structure and magnetic properties of [Cu(bipy)2(CH3COO)][Cu(bipy)2(Cr(C2O4)3)]·∼10.5H2O, the first compound containing the [Cr(C2O4)3]3− building block acting as a monodentate ligand

Abstract The reaction between copper(II) acetate with 2,2′-bipyridine and K3[Cr(C2O4)3] leads to the novel salt [Cu(bipy)2(CH3COO)][Cu(bipy)2(Cr(C2O4)3)]·∼10.5H2O, 1 (bipy=2,2′-bipyridine). The crystal structure of 1 consists of mononuclear cationic species [Cu(bipy)2(CH3COO)]+ and heterobinuclear anionic units, [Cu(bipy)2(Cr(C2O4)3)]−. The tris-oxalato-chromium entity behaves as a monodentate ligand toward the copper(II) ion within the complex anion. The distance between Cr(III) and Cu(II) across the bridging oxalato group is 5.056(2) A. The copper(II) ions exhibit a distorted trigonal bipyramidal surrounding in both cationic and anionic species. The π–π stacking interaction between bipy l…

Polycatenane systems from Co(II) and trans-1,2-bis(4-pyridyl)ethene (bpe). Synthesis and structure of Co(bpe)2(NCS)2·CH3OH, [Co(bpe)2(H2O)2](ClO4)2·2CH3OH and [Co(bpe)2(H2O)2(CH3OH)2](ClO4)2·bpe·H2O

Three new compounds of formulae Co(bpe)2(NCS)2·CH3OH, 1, [Co(bpe)2(H2O)2](ClO4)2·2CH3OH, 2 and [Co(bpe)2(H2O)2(CH3OH)2](ClO4)2·bpe·H2O, 3, [bpe =  trans-1,2-bis(4-pyridyl)ethene] have been synthesised and characterised by single crystal X-ray diffraction. The metal environment in 1–3 is distorted octahedral. Compound 1 is a polycatenane. Its structure consists of parallel layers containing Co2+ ions linked by bpe ligands, the Co···Co distance through the bpe bridge being 13.65(3) A. Each metal ion, in a layer, defines the edges of a rhombus. Two thiocyanate groups trans-coordinated to the metal atoms are perpendicular to the sheets. Each sheet has an infinite number of perpendicular sheets …

Magneto-structural correlations in a family of ReIVCuII chains based on the hexachlororhenate(IV) metalloligand

Six novel one-dimensional chloro-bridged ReIVCuII complexes of formula {[Cu(L)4][ReCl6]}n, where L = imidazole (Imi, 1), 1-methylimidazole (Meim, 2), 1-vinylimidazole (Vim, 3), 1-butylimidazole (Buim, 4), 1-vinyl-1,2,4-triazole (Vtri, 5) and N,N’-dimethylformamide (DMF, 6) are characterised structurally, magnetically and theoretically. The structures exhibit significant differences in Cu–Cl bond lengths and Re–Cl–Cu bridging angles, resulting in large differences in the nature and magnitude of magnetic exchange interactions between the ReIV and CuII ions. Theoretical calculations reveal the coupling to be primarily ferromagnetic, increasing in magnitude as the bridging angle becomes smaller…

Variation of the ground spin state in homo- and hetero-octanuclear copper(II) and nickel(II) double-star complexes with a meso-helicate-type metallacryptand core.

Homo- and heterometallic octanuclear complexes of formula Na₂{[Cu₂(mpba)₃][Cu(Me₅dien)]₆}-(ClO₄)₆·12H₂O (1), Na₂{[Cu₂(Mempba)₃][Cu(Me₅dien)]₆}(ClO₄)₆·12H₂O (2), Na₂{[Ni₂(mpba)₃]-[Cu(Me₅dien)]₆}(ClO₄)₆·12H₂O (3), Na₂{[Ni₂(Mempba)₃][Cu(Me₅dien)]₆}(ClO₄)₆·9H₂O (4), {[Ni₂(mpba)₃][Ni(dipn)(H₂O)]₆}(ClO₄)₄·12.5H₂O (5), and {[Ni₂(Mempba)₃][Ni(dipn)-(H₂O)]₆}(ClO₄)₄·12H₂O (6) [mpba = 1,3-phenylenebis(oxamate), Mempba = 4-methyl-1,3-phenylenebis(oxamate), Me₅dien = N,N,N',N'',N''-pentamethyldiethylenetriamine, and dipn = dipropylenetriamine] have been synthesized through the "complex-as-ligand/complex-as-metal" strategy. Single-crystal X-ray diffraction analyses of 1, 3, and 5 show cationic M(II)₂M'(I…

Solid-state cis–trans isomerism in bis(oxamato)palladate(ii) complexes: synthesis, structural studies and catalytic activity

A new generation of bis(oxamato)palladate(II) monomeric complexes has been prepared by using N-2,6-dimethylphenyloxamate (2,6-Me2pma) as the ligand. Four alkaline salts of the complex, namely {[Na(H2O)]2trans-[PdII(2,6-Me2pma)2]}n (1a), {[Na4(H2O)2]cis-[PdII(2,6-Me2pma)2]2}n (1b), {[K4(H2O)3]cis-[PdII(2,6-Me2pma)2]2}n (2), {[Rb4(H2O)3]cis-[PdII(2,6-Me2pma)2]2}n (3) and {[Cs6(H2O)7]trans-[PdII(2,6-Me2pma)2]2cis-[PdII(2,6-Me2pma)2]}n·3nH2O (4), were obtained and structurally characterized by single crystal X-ray diffraction. Both the cis and trans stereoisomers of the [PdII(2,6-Me2pma)2]2− complex anion were isolated in the solid state, in a cation-dependent manner. The trans-isomer as the so…

Synthesis, crystal structures and magnetic properties of single and double cyanide-bridged bimetallic Fe2(III)Cu(II) zigzag chains.

The bimetallic complexes [[Fe(III)(phen)(CN)4]2Cu(II)(H2O)2].4H2O (1), [[Fe(III)(phen)(CN)4]2Cu(II)].H2O (2) and [[Fe(III)(bipy)(CN)4]2Cu(II)].2H2O (3) and [[Fe(III)(bipy)(CN)4]2Cu(II)(H2O)2].4H2O (4) (phen = 1,10-phenanthroline and bipy = 2,2'-bipyridine) have been prepared and the structures of 1-3 determined by X-ray diffraction. The structure of 1 is made up of neutral cyanide-bridged Fe(III)-Cu(II) zigzag chains of formula [[Fe(III)(phen)(CN)4]2Cu(II)(H2O)2] and uncoordinated water molecules with the [Fe(phen)(CN)4]- entity acting as a bis-monodentate bridging ligand toward two trans-diaquacopper(II) units through two of its four cyanide groups in cis positions. The structure of 2 can …

Heteropolymetallic Supramolecular Solid-State Architectures Constructed from [Cr(AA)(C2O4)2]- Tectons, and Sustained by Coordinative, Hydrogen Bond and π−π Stacking Interactions (AA = 2,2‘-Bipyridine; 1,10-Phenanthroline)

The paper reports on four novel solid-state architectures constructed by using tectons having the general formula:  [Cr(AA)(C2O4)2]- [AA = 2,2‘-bipyridine (bipy) and 1,10-phenanthroline (phen)]. These building blocks are involved in various intermolecular interactions:  coordinative, hydrogen bonds, and π−π contacts. Two new crystallohydrates in the Ba[Cr(AA)(C2O4)2]2·nH2O family have been characterized:  [BaCr2(bipy)2(C2O4)4(H2O)2]·4H2O (1) and [BaCr2(phen)2(C2O4)4(H2O)2] (2). Because of the different numbers of water molecules, their crystal structures are completely different from those of two others previously reported, [BaCr2(bipy)2(C2O4)4(H2O)]·H2O and [BaCr2(phen)2(C2O4)4(H2O)2]·4H2O…

Reversible Solvatomagnetic Switching in a Spongelike Manganese(II)-Copper(II) 3D Open Framework with a Pillared Square/Octagonal Layer Architecture

The concept of "molecular magnetic sponges" was introduced for the first time in 1999 by the creative imagination of the late Olivier Kahn. It refers to the exotic spongelike behavior of certain molecule-based materials that undergo a dramatic change of their magnetic properties upon reversible dehydration/rehydration processes. Here we report a unique example of a manganese(II)-copper(II) mixed-metal-organic framework of formula [Na(H(2)O)(4)](4)[Mn(4){Cu(2)(mpba)(2)(H(2)O)(4)}(3)]·56.5H(2)O (1) (mpba=N,N'-1,3-phenylenebis(oxamate)). Compound 1 possesses a 3D Mn(II)(4)Cu(II)(6) pillared layer structure with mixed square and octagonal pores of approximate dimensions 1.2×1.2 nm and 2.1×3.0 n…

Syntheses, crystal structures and magnetic properties of tricyanomethanide-containing bis(2-pyrimidylcarbonyl)amidate copper(II) complexes

Abstract Three new copper(II) complexes of formulae [Cu(bpcam)(tcm)(H2O)] · 2H2O (1), [Cu(bpcam)(tcm)(H2O)] (2) and [Cu(bpcam)(tcm)]n (3) [bpcam = bis(2-pyrimidylcarbonyl)amidate and tcm = tricyanomethanide] have been prepared and their structures determined by single crystal X-ray diffraction. Complexes 1 and 2 are mononuclear species where each copper atom is five-coordinated in a somewhat distorted square pyramidal environment with a tridentate bpcam ligand and a terminally bound tcm group building the basal plane and a water molecule in the apical position. Compound 3 is a uniform copper(II) chain where the [Cu(bpcam)]+ units are connected through single μ-1,5-tcm bridges which link one…

From Paramagnetic to Single‐Molecule Magnet Behaviour in Heterobimetallic Compounds Containing the Tetrakis(thiocyanato‐ κN )cobaltate(II) Anion

Syntheses, crystal structures and magnetic properties of copper(II) polynuclear and dinuclear compounds with 2,3-bis(2-pyridyl)pyrazine (dpp) and pseudohalide as ligands

Abstract The preparation, crystal structures and magnetic properties of four heteroleptic copper(II) complexes with 2,3-bis(2-pyridyl)pyrazine (dpp) and azide, cyanate or thiocyanate as ligands are reported, [Cu(dpp)(N3)2]n (1), [Cu(dpp)(NCO)2]n (2), [Cu(dpp)(NCS)2]2 (3) and [Cu(H2O)(dpp)(NCS)2]2·2H2O (4). Compounds 1 and 2 are isomorphous, triclinic, space group P1, and consist of mononuclear building blocks featuring copper atoms with close to square planar coordination geometries. The mononuclear units are, however, associated into chains through weak axial Cu–N bonds formed by end-on asymmetrically bridging azido/cyanato groups and by pyridyl nitrogen atoms. Taking these contacts into a…

Pyrophosphate-mediated magnetic interactions in Cu(II) coordination complexes.

The reaction in water of Cu(NO(3))(2)·2.5H(2)O with 2,2'-bipyridine (bipy), 1,10-phenanthroline (phen), or 1,10-phenanthroline-5-amine (phenam), and sodium pyrophosphate (Na(4)P(2)O(7)), at various pHs, afforded three new copper(II)-pyrophosphate complexes, namely, {[Cu(bipy)(cis-H(2)P(2)O(7))](2)}·3H(2)O (1a), {[Cu(phen)(H(2)O)](4)(HP(2)O(7))(2)}(ClO(4))(2)·4H(2)O (2), and {[Cu(2)(phenam)(2)(P(2)O(7))](2)·25H(2)O}(n) (3). A solvent free crystalline phase of 1a was also isolated with formula {[Cu(bipy)(trans-H(2)P(2)O(7))](2)} (1b), which can be regarded as a pseudo-polymorph of 1a. Single crystal X-ray analyses revealed these compounds to have uncommon molecular architectures, with 3 being…

Formation in solution, synthesis and crystal structure of μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II)

Abstract The compound μ-oxalatobis[bis(2-pyridylcarbonyl)amido] dicopper(II), [Cu 2 {(NCsH 5 CO) 2 N} 2 - (C 2 O 4 )] was synthesized and characterized by spectroscopy, EPR and diffraction methods. It crystallizes in the triclinic space group P 1 with cell constants: a =7.6793(6), b =9.238(2), c =10.007(2) A, α=83.80(1), β=68.37(1) and γ=69.44(1)°; V =617.7(3) A 3 , D (calc., Z =2)=1.80 g cm −3 , M r =667.6, F (000)=336, λ, (Mo Kα)=0.71069 A, μ (Mo Kα)=17.895 cm −1 and T =295 K. A total of 3587 data were collected over the range of 1 ⩽ θ ⩽ 30°; of these, 2391 (independent and with I⩾2σ( I )) were used in the structural analysis. The final R and R w residuals were 0.049 and 0.053, respective…

A self-assembled tetrameric water cluster stabilized by the hexachlororhenate(IV) anion and diprotonated 2,2′-biimidazole: X-ray structure and magnetic properties

A self-assembled tetrameric water cluster stabilized by [ReCl6]2− anions and [H4biim]2+ cations occurs in the new compound [H4biim][ReCl6]·4H2O, which exhibits a weak ferromagnetic coupling between the Re(IV) centers through an unusual ReIV–Cl⋯(H2O)⋯Cl–ReIV pathway.

Molecular-Programmed Self-Assembly of Homo- and Heterometallic Tetranuclear Coordination Compounds: Synthesis, Crystal Structures, and Magnetic Properties of Rack-Type CuII2MII2 Complexes (M = Cu and Ni) with Tetranucleating Phenylenedioxamato Bridging Ligands

New homo- and heterobimetallic tetranuclear complexes of formula [Cu4(mpba)(Me4en)4(H2O)4](ClO4)4·3H2O (1), [Cu4(mpba)(Me4en)4(H2O)4](PF6)4·2H2O (2), [Cu4(ppba)(Me4en)4(H2O)4](ClO4)4·2H2O (3), [Cu4(mpba)(dipn)4](ClO4)4·3H2O (4), [Cu4(ppba)(dipn)4](ClO4)4·2H2O (5), and [Cu2Ni2(ppba)(dipn)4(H2O)2](PF6)4 (6) [mpba = N,N′-1,3-phenylenebis(oxamate), ppba = N,N′-1,4-phenylenebis(oxamate), Me4en = N,N,N′,N′-tetramethylethylenediamine, and dipn = dipropylenetriamine] have been synthesized and structurally and magnetically characterized. Complexes 1−6 have been prepared following a molecular-programmed self-assembly method, where a heteropolytopic tetranucleating phenylenedioxamato bridging ligand (…

Trans-dicyanobis(acetylacetonato)ruthenate(III) as a precursor to build novel cyanide-bridged RuIII–MII bimetallic compounds [M=Co and Ni]

Abstract The use of the mononuclear complex trans-[Ru(acac)2(CN)2]− as a ligand towards the preformed species [Ni2L(H2O)2Cl2], [Co(dmphen)](NO3)2, [Ni(dmphen)](NO3)2 and [Co(H2O)6](NO3)2 afforded the novel cyanide-bridged bimetallic compounds of formula [{Ru(acac)2(CN)2}{Ni2(L)(H2O)2}]{Ru(acac)2(CN)2}·2H2O (1), [{Ru(acac)2(CN)2}{Co(dmphen)(NO3)}]·H2O (2) and [{Ru(acac)2(CN)2}{Ni(dmphen)(NO3)}]·H2O (3) and [{Ru(acac)2(CN)2}2Co] (4) [Hacac = acetylacetone, dmphen = 2,9-dimethylphenanthroline and H2L = 11,23-dimethyl-3,7,15,19-tetrazatricyclo[19.3.1.19,13]hexacosa-2,7,9,11,13(26),14,19,21(25),22,24-decaene-25,26-diol]. Their syntheses, X-ray crystal structures and magnetic properties are repor…

Rational enantioselective design of chiral heterobimetallic single-chain magnets: synthesis, crystal structures and magnetic properties of oxamato-bridged M(II)Cu(II) chains (M=Mn, Co).

A new series of neutral oxamato-bridged M(II)Cu(II) chiral chains of general formula [MCuL(x)(S)(m)(H(2)O)(n)]·aS·bH(2)O [L(1)=(M)-1,1'-binaphthalene-2,2'-bis(oxamate) with M=Mn (1a) and Co (1b); L(2)=(P)-1,1'-binaphthalene-2,2'-bis(oxamate) with M=Mn (2a) and Co (2b)] and the analogous racemic chains of formula [MCuL(3)(S)(m)(H(2)O)(n)]·aS·bH(2)O [L(3)=1,1'-binaphthalene-2,2'-bis(oxamate) with M=Mn (3a) and Co (3b)] have been prepared by reaction of the corresponding dianionic oxamatocopper(II) complex [Cu(L(x))](2-) with Mn(2+) or Co(2+) cations in either dimethylformamide (DMF) or dimethyl sulfoxide (DMSO). Solid circular dichroism (CD) spectra of the bimetallic chain compounds were reco…

Ferromagnetic coupling through a carbonate bridge in the copper (II) chain [Cu(CO3)(4-apy)2] · H2O (4-apy = 4-aminopyridine)

Abstract Atmospheric CO2 fixation by aqueous solutions containing copper(II) bromide and 4-aminopyridine (4-apy) yields the first carbonatobridged copper(II) chain of formula [Cu(CO3)(4-apy)2] · H2O that exhibits an intrachain ferromagnetic coupling.

Novel Three-Dimensional Cage Assembly of amgr;(4)-Carbonato-Bridged Cobalt(II) Compound [Co(2)(bpm)(H(2)O)(2)(CO(3))(OH)]NO(3).4H(2)O.

The new three-dimensional cobalt(II) complex of formula [Co2(bpm)(H2O)2(CO3)(OH)]NO3·4H2O (1) is obtained from aqueous solutions containing cobalt(II) nitrate hexahydrate, 2,2‘-bipyrimidine (bpm), ...

Supramolecular arrangements of novel clickable 4-substituted 3,6-bis(2′-pyridyl)pyridazine molecules

Abstract The clickable reaction between the starting 3,6-bis(2′-pyridyl)-1,2,4,5-tetrazine (bptz) with a series of terminal alkynes-containing functional biomolecules [prop-2-yn-1-ol, 4-(prop-2′-yn-1′-yl)morpholine and D-galactose] by means of an inverse electron demand Diels-Alder pathway has been studied and four new 4-substituted 3,6-bis(2′-pyridyl)pyridazine derivatives (4-Rdppn) were isolated, namely 4-(hydroxymethyl)-3,6-di(pyridin-2-yl)pyridazine (1), 4-((prop-2-yn-1-yloxy)methyl)-3,6-di(pyridin-2-yl)pyridazine (2) obtained by post-etherification reaction of 1, 4-(morpholinemethyl)-(3,6-dipyridin-2-yl)pyridazine monohydrate (3) and 3,6-di(pyridin-2-yl)-4-((2,2,7,7-tetramethyltetrahyd…

Synthesis, crystal structure and magnetic properties of the first structurally characterized 1,2-dithiocroconato-containing Cu(II) complex, [Cu(bpca)(H2O)]2[Cu(1,2-dtcr)2]·2H2O

Abstract The first crystal and molecular structure of a transition metal complex containing 1,2-dithiocroconate (1,2-dtcr, dianion of 1,2-dimercaptocylopent-1-ene-3,4,5-trione), [Cu(bpca)(H2O)]2[Cu(1,2-dtcr)2]·2H2O (where bpca is the bis(2-pyrdidylcarbonyl)amide anion), has been determined by single crystal X-ray diffraction methods. The compound crystallizesin the monoclinic syste, space group P21/c, with a = 11.661(3), b = 20.255(6), c = 8.265(3) A , s = 107.26(2)° and Z = 2. The structure is formally built of [Cu(1,2-dtcr)2]2− and [Cu(bpca)(H2O)]+ ions and water of hydration. The copper atom of the anion is situated at a crystallographic inversion centre, bonded to four sulfur atoms in a…

The influence of pseudohalide ligands on the SIM behaviour of four-coordinate benzylimidazole-containing cobalt(ii) complexes.

Three, mononuclear complexes of the formula [Co(bmim)2(SCN)2] (1), [Co(bmim)2(NCO)2] (2) and [Co(bmim)2(N3)2] (3) [bmim = 1-benzyl-2-methylimidazole] were prepared and structurally analyzed by single-crystal X-ray crystallography. The cobalt(ii) ions in 1-3 are tetrahedrally coordinated with two bmim molecules and two pseudohalide anions. The angular distortion parameter δ was calculated and the SHAPE program (based on the CShM concept) was used for 1-3 to estimate the angular distortion from an ideal tetrahedron. The molecules of 1-3 are effectively separated, and the values of the shortest distance of cobalt-cobalt are 8.442(6) and 6.774(8) A for 1, 10.349(8) and 10.716(8) A for 2 and 6.7…

Synthesis, Structure, and Magnetic Properties of Regular Alternating μ-bpm/di-μ-X Copper(II) Chains (bpm = 2,2′-bipyrimidine; X = OH, F)

The preparation and X-ray crystal structure of four 2,2'-bipyrimidine (bpm)-containing copper(II) complexes of formula {[Cu(2)(μ-bpm)(H(2)O)(4)(μ-OH)(2)][Mn(H(2)O)(6)](SO(4))(2)}(n) (1), {[Cu(2)(μ-bpm)(H(2)O)(4)(μ-OH)(2)]SiF(6)}(n) (2), {Cu(2)(μ-bpm)(H(2)O)(2)(μ-F)(2)F(2)}(n) (3), and [Cu(bpm)(H(2)O)(2)F(NO(3))][Cu(bpm)(H(2)O)(3)F]NO(3)·2H(2)O (4) are reported. The structures of 1-3 consist of chains of copper(II) ions with regular alternation of bis-bidentate bpm and di-μ-hydroxo (1 and 2) or di-μ-fluoro (3) groups, the electroneutrality being achieved by either hexaaqua manganese(II) cations plus uncoordinated sulfate anions (1), uncoordinated hexafluorosilicate anions (2), or terminally …

Systematic investigation of the adsorption and inhibition properties of a new clickable 1,2,3‐triazole compound for mild steel in 1 M HCl medium

Crystal Structure and Magnetic Properties of 3,5-Pyridinedicarboxylate-Bridged Re(Ii)M(Ii) Heterodinuclear Complexes (M = Cu, Ni and Co)

Abstract The use of the mononuclear rhenium(II) precursor NBu4[Re(NO)Br4(H2pydc)]·i-PrOH (1) (H2pydc = 3,5-pyridinedicarboxylic acid) as a metalloligand towards Cu(II), Ni(II) and Co(II) afforded three new heterobimetallic complexes [Re(NO)Br4(μ-Hpydc)Cu(4,4′-dmbipy)2]·(CH3)2CO·0.25MeCN (2), [Re(NO)Br4(μ-Hpydc)Ni(dmphen)2]·MeCN (3) and [Re(NO)Br4(μ-Hpydc)Co(dmphen)2]·2H2O (4), respectively [4,4′-dmbipy = 4,4′-dimethyl-2,2′-bipyridine, dmphen = 2,9-dimethyl-1,10-phenanthroline and Bu4N+ = tetra-n-butylammonium]. The crystal structures of 1 and 2 are reported herein together with the cryomagnetic investigation of 1–4 in the temperature range of 2.0–300 K. 1 is a mononuclear compound whose str…

Synthesis, crystal structures and magnetic properties of M(II)Cu(II) chains (M = Mn and Co) with sterically hindered alkyl-substituted phenyloxamate bridging ligands.

A series of neutral oxamato-bridged heterobimetallic chains of general formula [MCu(L(x)2 (S)2] · p S · q H2O [p = 0-1, q = 0-2.5; L1 = N-2,6-dimethylphenyloxamate, S = DMF with M = Mn (1a) and Co (1b); L2 = N-2,6-diethylphenyloxamate, S = DMF with M = Mn (2a) and Co (2b) or S = DMSO with M = Mn (2c) and Co (2 d); L3 = N-2,6-diisopropylphenyloxamate, S = DMF with M = Mn (3a) and Co (3b) or S = DMSO with M = Mn (3c) and Co (3d)] were prepared by treating the corresponding anionic oxamatocopper(II) complexes [Cu(L(x))(2)]2- (x = 1-3) with M(2+) cations (M = Mn and Co) in DMF or DMSO as the solvent. The single-crystal X-ray structures of 2a and 3a reveal the occurrence of well-isolated, zigzag…

Ferromagnetic coupling and magnetic anisotropy in oxalato-bridged trinuclear chromium(iii)-cobalt(ii) complexes with aromatic diimine ligands

Two novel heterotrinuclear chromium(III)-cobalt(II) complexes of formula {[Cr(III)(bpy)(ox)(2)](2)Co(II)(Me(2)bpy)}.2H(2)O (1) and {[Cr(III)(phen)(ox)(2)](2)Co(II)(Me(2)bpy)}.1.5H(2)O (2) [ox = oxalato, bpy = 2,2'-bipyridine, Me(2)bpy = 6,6'-dimethyl-2,2'-bipyridine, and phen = 1,10-phenanthroline] have been synthesized using the "complex-as-ligand/complex-as-metal" strategy. The X-ray crystal structure of 2 consists of neutral oxalato-bridged Cr(III)(2)Co(II) bent entities formed by the coordination of two anionic [Cr(III)(phen)(ox)(2)](-) complexes through one of their oxalato groups toward a cationic cis-[Co(II)(Me(2)bpy)](2+) complex. The three tris(chelated), six-coordinated metal atom…

A study of the exchange interaction through phenolato, oximato and oxamidato bridges in MnIICuII dimers. Crystal structure of [Cu(salen)Mn(hfa)2]

Abstract Three new heterodinuclear CuIIMnII complexes of formula [Cu(salen)Mn(hfa)2] (1), [Cu(pdmg)Mn(phen)2](ClO4)2·2.5H2O (2) and [Cu(apox)Mn(bpy)2](ClO4]2·0.5H2O (3) (salen=N,N′-ethylenebis(salicylideneiminate), hfa=hexafluoroacetylacetonate, pdmg=3,9-dimethyl-4,8-diazaundeca-3,8-diene-2,10-dione dioximate, phen=1,10- phenanthroline, apox=N,N′-bis(3-aminopropyl)oxamidate and bipy=2,2′-bipyridyl) have been synthesized. The crystal and molecular structure of 1 has been determined by X-ray diffraction methods. It crystallizes in the triclinic system, space group P 1 with cell constants a=15.584(4), b=12.039(3), c=9.470(2) A, α=113.83(2), β=107.17(3), γ=84.28(3)°; V=1552(1) A3, D (calc., Z=2…

2,3,5,6-Tetrakis(2-pyridyl)pyrazine (tppz)-containing iron(II) complexes: Syntheses and crystal structures

Abstract The preparation and crystal structure of two iron(II) complexes of formula PPh4-mer-[Fe(tppz)(CN)3] · 7H2O (1) and [Fe(tppz)2][Fe(NCS)4] (2) [tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine; PPh 4 + = tetraphenylphosphonium cation ] are reported here. The structure of 1 consists of mononuclear mer-tricyano[2,3,5,6-tetrakis(2-pyridyl)pyrazine]ferrate(II) anions, tetraphenylphosphonium cations and crystallization water molecules. Three carbon atoms from three cyanide groups in a mer arrangement and three nitrogen atoms from a tridentate tppz ligand build a somewhat distorted octahedral surrounding around the iron atom in 1. The values of the Fe–C [1.925(6)–1.947(5) A] and Fe–N [1.870(4)–1…

A two-dimensional coordination polymer constructed from binuclear copper(II) metalloligands and manganese(II) ions: Synthesis, crystal structure and magnetic properties

Abstract The self-assembly process between the binuclear [Cu2(HL)(L)]− complex and the manganese(II) ion affords a two-dimensional coordination polymer of formula [Mn{Cu2(HL)(L)}2(H2O)2]n (1) (H3L = 3-hydroxyiminomethylsalicylic acid) where parallel ladder-like motifs of defective double cubanes of bis(phenoxo)dicopper(II) units as rods and anti-syn carboxylato bridges as rungs act as ligands towards tetraaqua-manganese(II) entities through the deprotonated oxime groups. The topology of 1 is compared with the one of another compound, [Mn{Cu2(HL)(L)}2(H2O)4]·4H2O·2DMF (1′) which was obtained in different conditions by Okawa et al. (J. Chem. Soc., Dalton Trans. (2001) 3119). Magnetic suscepti…

Topological control of the spin coupling in dinuclear copper(II) complexes with meta- and para-phenylenediamine bridging ligands

Abstract A novel series of copper(II) complexes of formula [Cu(tren)(mpda)](ClO4)2 · 1/2H2O (1), [Cu2(tren)2(mpda)](ClO4)4 · 2H2O (2), and [Cu2(tren)2(ppda)](ClO4)4 · 2H2O (3) containing the tetradentate tris(2-aminoethyl)amine (tren) terminal ligand and the potentially bridging 1,n-phenylenediamine [n = 3 (mpda) and 4 (ppda)] ligand have been prepared and spectroscopically characterized. X-ray diffraction on single crystals of 1 and 3 show the presence of mono- (1) and dinuclear (3) copper(II) units where the mpda (1) and ppda (3) ligands adopt terminal monodentate (1) and bridging bis(monodentate) (3) coordination modes toward [Cu(tren)]2+ cations with an overall non-planar, orthogonal di…

Self-assembly, metal binding ability, and magnetic properties of dinickel(II) and dicobalt(II) triple mesocates

Two metallacyclic complexes of general formula Na-8[(M2L3)-L-II]center dot xH(2)O [M = Ni (4) and Co (5) with x = 15 (4) and 17 (5)] have been self-assembled in aqueous solution from N,N'-1,3-phenylenebis(oxamic acid) (H4L) and M2+ ions in a ligand/metal molar ratio of 3 : 2 in the presence of NaOH acting as base. X-Ray structural analyses of 4 and 5 show triple-stranded, dinuclear anions of the meso-helicate-type (so-called mesocates) with C-3h molecular symmetry. The two octahedral metal-tris(oxamate) moieties of opposite chiralities (Delta, Lambda form) are connected by three m-phenylene spacers at intermetallic distances of 6.822(2) (4) and 6.868(2) angstrom (5) to give a metallacryptan…

Synthesis, crystal structures and magnetic properties of tricyanomethanide-containing copper(II) complexes

The preparation, crystal structures and magnetic properties of the copper(II) complexes of formula [Cu(pyim)(tcm)(2)](n) (1), [Cu(bpy)(tcm)(2)](n) (2), [Cu(4)(bpz)(4)(tcm)(8)] (3), {[Cu(terpy)(tcm)].tcm}(n) (4) and {[Cu(2)(tppz)(tcm)(4)].3/2H(2)O}(n) (5) [pyim = 2-(2-pyridyl)imidazole, tcm = tricyanomethanide, bpy = 2,2'-bipyridine, bpz = 2,2'-bipyrazine, terpy = 2,2':6',2''-terpyridine and tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine] are reported. Complexes, 1, 2 and 4 are uniform copper(II) chains with single- (1 and 4) and double-(2) micro-1,5-tcm bridges with values of the intrachain copper-copper separation of 7.489(1) (1), 7.520(1) and 7.758(1) (2) and 7.469(1) A (4). Each copper atom …

Very Long-Distance Magnetic Coupling in a Dicopper(II) Metallacyclophane with Extended π-Conjugated Diphenylethyne Bridges

Self-assembly of the rigid rodlike ligand N,N'-4,4'-diphenylethynebis(oxamate) (dpeba) and Cu(2+) ions affords a novel dinuclear copper(II) metallacyclophane (nBu(4)N)(4)[Cu(2)(dpeba)(2)]·4MeOH·2Et(2)O (1) featuring a very long intermetallic distance (r = 15.0 Å). Magnetic susceptibility measurements for 1 reveal a moderately weak but nonnegligible intramolecular antiferromagnetic coupling between the two metal centers across the double para-substituted diphenylethynediamidate bridge (J = -3.9 cm(-1); H = -JS(1)S(2), where S(1) = S(2) = S(Cu) = (1)/(2)). Density functional electronic structure calculations on 1 support the occurrence of a spin polarization mechanism.

The heterodinuclear iron(III) and copper(II) molecule Cu(salen)Fe(acac)2NO3 and its iron precursor Fe(acac)2NO3. Synthesis, magnetic susceptibility, EPR and Mössbauer investigations

Abstract The synthesis, EPR, magnetic and Mossbauer properties of two iron(III) complexes are reported. The heterodinuclear iron(III)-copper(II) complex Cu(salen)Fe(acac)2NO3 is obtained as an adduct from the reaction of the two mononuclear moieties, the Cu(salen) molecule and the mononuclear iron(III) molecule Fe(acac)2NO3 acting as a precursor of the dinuclear unit. The latter molecule itself has been prepared by ligand substitution from the tris-acetylacetonate Fe(acac)3. The dinuclear complex is characterized by comparing the properties of the mono- and the dinuclear complex. Fe(acac)2NO3 is identified from its typical IR spectrum with the main nitrate vibrations at 1380, 1250 and 1010 …

Cellulose‑copper as bio-supported recyclable catalyst for the clickable azide-alkyne [3 + 2] cycloaddition reaction in water.

Abstract Naturally-occurring cellulose has been employed as a bio-support macromolecule for the immobilization of either copper(I) or copper(II) ions in order to click azide and alkyne derivatives in water. Under such a click regime, 1,4-disubstitued-1,2,3-triazoles were obtained regioselectively in excellent yields at room temperature. The reaction work-up is simple and the bio-heterogeneous catalyst that has been fully characterized by AAS, SEM, EDX and FT-IR can be easily separated and reused at least five times without any significant decrease in its activity and selectivity, particularly in the case of the very stable CuI-Cellulose.

Synthesis, crystal structure and magnetic properties of the Re(II) complexes NBu4[Re(NO)Br4(L)] (L = pyridine and diazine type ligands).

Four novel Re(II) complexes of formula NBu4[Re(NO)Br4(L)] [NBu4(+) = tetra-n-butylammonium cation and L = pyridine (1), pyrazine (2), pyrimidine (3), pyridazine (4)] have been prepared by a substitution reaction involving NBu4[Re(NO)Br4(EtOH)] and L. Their crystal structures have been determined by single crystal X-ray diffraction. They are all mononuclear complexes whose structure is made up of [Re(NO)Br4L](-) anions and NBu4(+) cations. Each Re(II) ion is six-coordinate with four bromide ligands, a linear nitrosyl group and one monodentate nitrogen donor L building a tetragonally distorted octahedral surrounding. The Re-Br bond distances cover a narrow range [2.5048(8)-2.5333(5) Å] and th…

Synthesis, crystal structure and magnetic properties of [Co(bpcam)2]ClO4·dmso·H2O, [Co(bpcam)2]2[Co(NCS)4]·dmso·H2O and [Ni(bpcam)2]·H2O [Hbpcam = bis(2-pyrimidylcarbonyl)amide]

The preparation, spectroscopic characterization, structural study and magnetic investigation of three new complexes of formula [Co(bpcam)2]ClO4·dmso·H2O (1), [Co(bpcam)2]2[Co(NCS)4]·dmso·H2O (2) and [Ni(bpcam)2]·H2O (3) [Hbpcam = bis(2-pyrimidylcarbonyl)amide] are reported. Each bpcam group in 1–3 acts as a tridentate ligand being coordinated to the cobalt(III) (1 and 2)/nickel(II) (3) ions through three nitrogen atoms in a mer-arrangement. Six-coordinate cobalt(III) and nickel(II) occur in 1 and 3 respectively, whereas six-coordinate cobalt(III) and four-coordinate cobalt(II) coexist in 2. Cyclic voltammetry of 1 in acetonitrile shows the occurrence of one quasi reversible CoIII ↔ CoII pro…

Monitoring the hydrogen bond net configuration and the dimensionality of aniline and phenyloxamate by adding 1 H -pyrazole and isoxazole as substituents for molecular self-recognition

This work describes the synthesis and characterization of a new class of oxamic acid derivatives containing pyrazole and isoxazole as substituents to investigate their ability to form hydrogen bonds aiming at applying them in crystal engineering and molecular self-recognition. In this respect, we report a new synthesis of 2-(4-nitrophenyl)-1,3-propanedial (1) in high yield using SOCl2 as a chlorinating agent. The new oxamic esters 4-(1H-pyrazol-4-yl)phenylene-N-(ethyloxamate) (2d) and 4-(1,2-oxazol-4-yl)phenylene-N-(ethyloxamate) (3d) were prepared from 1. The synthetic route consists of the cyclisation of 1 either with hydrazine to afford 4-(-aminophenyl)-1H-pyrazole (2a) or with hydroxyla…

Dinuclear and two- and three-dimensional gadolinium(III) complexes with mono- and dicarboxylate ligands: synthesis, structure and magnetic properties

Three new gadolinium(III) complexes with carboxylate ligands of formula [Gd2(ac)6(H2O)4]·2H2O (1), [Gd2(ac)2(fum)2(H2O)4]n (2) and [Gd2(ox)(fum)2(H2O)4]n·4nH2O (3) (ac = acetate, fum = fumarate and ox = oxalate) have been prepared and their structures determined by X-ray diffraction on single crystals. The structure of 1 is made up of discrete centrosymmetric di-µ-oxo(carboxylate acetate)digadolinium(III) units with an intramolecular Gd⋯Gd separation of 4.1589(3) A. Each gadolinium atom in 1 is nine-coordinated with two water molecules and seven carboxylate-oxygen atoms from four acetate ligands building a monocapped square antiprism environment. Compound 2 exhibits a sheet-like structure, …

Synthesis, crystal structure and magnetic properties of the dinuclear manganese(II) complexes [Mn2(bpym)3(NCX)4] (bpym = 2,2′-bipyrimidine; X = S, Se)

Abstract The dinuclear manganese(II) compounds of formula [Mn2(bpym)3(NCX)4], where bpym = 2,2′-bipyrimidine and X = S(1) and Se(2), have been prepared and their crystal structures determined by X-ray diffraction methods. 1 and 2 are isostructural. They crystallize in the triclinic P 1 space group with Z = 1, γ ( Mo K α ) = 0.71073 A , T = 295 K and a = 9.141(2), b = 9.248(2), c = 11.733(2) A , α = 74.88(2), β = 80.29(2), γ = 61.03(2)°, V = 836.7(3) A 3 , D c = 1.621 g cm −3 , M r = 316.7, F(000) = 412, and μ( Mo K α) = 10.54 cm −1 for 1 and a = 9.244(2), b = 9.278(2) A , c = 11.887(2) A , α = 75.19(2), β = 80.83(2), γ = 61.54(2)°, V = 865.7(3) A 3 , D c = 1.926 g cm −3 , M r = 1004.3, F(00…

Influence of the presence of divalent first-row transition metal ions on the structure of sodium(i) salts of 1,2,3,4-benzenetetracarboxylic acid (H4bta)

Three different sodium(I)-containing salts of 1,2,4,5-benzenetetracarboxylic (H4bta) of formula [Na4(bta)(H2O)12] (1), [Na2M(H2bta)2(H2O)8]·2H2O] [M = Mn (2) and Ni (3)] were synthesized and their structures were solved by single crystal X-ray diffraction methods. Compound 1 crystallises in orthorhombic system, space group Pc21b with a = 6.9997(4) A, b = 16.4260(9) A, c = 20.3312(18) A, V = 476.30(15) A3 and Z = 4. Compounds 2 and 3 crystallize in the monoclinic system, space group C2/m with a = 7.3778(4) A, b = 20.1493(6) A, c = 10.4963(4) A, β = 103.466(8)°, V = 1517.5(11) A3 and Z = 2 for 1 and a = 7.2862(4) A, b = 20.1165(7) A, c = 10.4032(3) A, β = 103.366(9)°, V = 1483.52(11) A3 and Z…

Highly Anisotropic Rhenium(IV) Complexes: New Examples of Mononuclear Single-Molecule Magnets

The rhenium(IV) complex (NBu4)2[ReBr4(ox)] (1) (ox = oxalate and NBu4(+) = tetra-n-butylammonium cation) has been prepared and its crystal structure determined by X-ray diffraction. The structure is made up of discrete [ReBr4(ox)](2-) anions and bulky NBu4(+) cations. Each [ReBr4(ox)](2-) anion is surrounded by six NBu4(+) cations, which preclude any significant intermolecular contact between the anionic entities, the shortest rhenium···rhenium distance being 9.373(1) Å. Variable temperature dc and ac magnetic susceptibility measurements and field-dependent magnetization experiments on polycrystalline samples of 1 reveal the occurrence of highly anisotropic magnetically isolated Re(IV) cent…

4,2-Ribbon like ferromagnetic cyano-bridged FeIII2NiII chains: a magneto-structural study

The low-spin iron(III) complex AsPh(4)[Fe(III)(bpy)(CN)(4)].CH(3)CN (1) [AsPh(4) = tetraphenylarsonium cation] and the heterobimetallic chains [{Fe(III)(L)(CN)(4)}(2)Ni(II)(H(2)O)(2)].4H(2)O with L = bpy (2) and phen (3) [bpy = 2,2'-bipyridine and phen = 1,10-phenanthroline] have been prepared and their structures determined by X-ray diffraction methods. The structure of 1 consists of mononuclear [Fe(bpy)(CN)(4)](-) anions, tetraphenylarsonium cations and acetonitrile molecules of crystallization. The iron(III) is hexacoordinated with two nitrogen atoms of the bidentate bpy and four carbon atoms of four terminal cyanide groups building a distorted octahedral surrounding around the metal ato…

ChemInform Abstract: Sustainable Carbon-Carbon Bond Formation Catalyzed by New Oxamate-Containing Palladium(II) Complexes in Ionic Liquids.

New and versatile bis(oxamato)palladate(II) complexes (I) are synthesized and investigated for both Suzuki and Heck coupling reactions in molten tetra-n-butylammonium bromide as ionic liquid.

A methylenediphosphonate bridged copper(II) tetramer: Synthesis, structural, thermal, and magnetic characterization of [Cu4(H2O)2(phen)4(μ-P2O6CH2)2]·21H2O

Abstract A novel tetracopper(II) complex namely, [Cu4(H2O)2(phen)4(μ-P2O6CH2)2]·21H2O (1) was synthesized by using copper(II) chloride, 1,10-phenanthroline (phen), and methylene diphosphonic acid (MDP). The structure of 1 was characterized by single crystal X-ray diffraction and spectroscopy. Compound 1 crystallizes in the triclinic system, P 1 ¯ space group and its crystal structure consists of neutral centrosymmetric tetranuclear copper(II)-methylene diphosphonate units where each peripheral {Cu(phen)(P2O6CH2)}2− fragment adopts the bidentate(Oeq-P-Oeq)/monodentate (Oax) bridging mode towards each of the two inner {Cu(phen)}2+ entities resulting in a “clamshell”-like orientation. The two …

Crystal Structure and Magnetic Properties of an Oxamato‐Bridged Heterobimetallic Tetranuclear [Ni II Cu II ] 2 Complex of the Rack Type

Synthesis, structural analysis, and magnetic properties of ethylmalonate-manganese(II) complexes

12 páginas, 10 figuras, 6 tablas.-- et al.

Photomagnetic effect in a cyanide-bridged mixed-valence {FeII2FeIII2} molecular square

The self-assembly of [Fe(III)(Tp)(CN)(3)](-) and [Fe(II)(bik)(2)(S)(2)](2+) affords the cyanide-bridged mixed valence {Fe(III)(2)Fe(II)(2)}(2+) molecular square, which exhibits a photomagnetic effect under laser light irradiation at low temperature and also shows thermal spin-state conversion near ambient temperature.

Magnetic properties of six-coordinated high-spin cobalt(II) complexes: Theoretical background and its application

Abstract In this contribution we study and analyse the influence of the different parameters involved in the magnetic susceptibility of six-coordinated high-spin Co(II) complexes. We propose an empirical expression to fit the magnetic susceptibility of polycrystalline samples of mononuclear Co(II) complexes with an axial distortion, the variable parameters being Δ (axial distortion), α (orbital reduction factor) and λ (spin–orbit coupling). This expression avoids solving the 12 × 12 matrix associated to the distortion of the 4 T 1g term. In order to take into account the magnetic coupling ( J ) in the polynuclear Co(II) complexes, a perturbational approach is proposed to describe their magn…

Structurally characterized dipalladium(ii)-oxamate metallacyclophanes as efficient catalysts for sustainable Heck and Suzuki reactions in ionic liquids

A new generation of dipalladium-oxamate metallacyclophanes of formulas (n-NBu4)4 [Pd2(ppba)2] (1), (n-NBu4)4[Pd2(dpvba)2] (2), (n-NBu4)4[Pd2(dpazba)2] (3), (n-NBu4)4[Pd2(dpeba)2] (4) and (n-NBu4)4[Pd2(tpeba)2] (5) [n-NBu4+ = tetra-n-butylammonium cation, H4ppba = N,N′-1,4-phenylenebis(oxamic acid), H4dpvba = N,N′-4,4′-diphenylethenebis(oxamic acid), H4dpazba = N,N′-4,4′-diphenylazobis(oxamic acid), H4dpeba = N,N′-4,4′-diphenylethynebis(oxamic acid) and H4tpeba = N,N′-1,4-di(4-phenylethynyl)phenylenebis(oxamic acid)] was prepared. The crystal structure of the solvated species of 2–4, namely (n-NBu4)4[Pd2(dpvba)2]·6MeOH·2Et2O (2a), (n-NBu4)4[Pd2(dpazba)2]·8MeOH (3a), and (n-NBu4)2[Pd2(dpeba)2…

Solid-State Aggregation of Metallacyclophane-Based MnIICuII One-Dimensional Ladders

Two distinct one-dimensional (1) and two-dimensional (2) mixed-metal-organic polymers have been synthesized by using the "complex-as-ligand" strategy. The structure of 1 consists of isolated ladderlike Mn(II)(2)Cu(II)(2) chains separated from each other by neutral Mn(II)(2) dimers, whereas 2 possesses an overall corrugated layer structure built from additional coordinative interactions between adjacent Mn(II)(2)Cu(II)(2) ladders. Interestingly, 1 and 2 show overall ferri- and antiferromagnetic behavior, respectively, as a result of their distinct crystalline aggregation in the solid state.

Synthesis, structural, thermal, and magnetic investigations of Co(II), Ni(II), and Mn(II) pyrophosphate chains

The reaction in water of cobalt(II), nickel(II) or manganese(II) chloride with 1,10-phenanthroline (phen) and sodium pyrophosphate (Na 4 P 2 O 7 ) at low pH (∼2) afforded three isostructural pyrophosphate complexes of an unprecedented one-dimensional typology, namely, {[M(phen)(H 2 O)(H 2 P 2 O 7 )]·H 2 O} n with M = Co( 1 ), Ni( 2 ) and Mn( 3 ). The di-hydrogen-pyrophosphate anion featured in these complexes adopts a rare bidentate/monodentate bridging mode leading to chain propagation. This unusual bridging pathway produces a metal–metal intra-chain separation of about 6.6–6.7 A for 1 – 3 , values much larger than the metal–metal distance across the classic bis-bidentate PPi in the parent…

Synthesis, crystal structure, and magnetic characterization of the three-dimensional compound [Co2(cbut)(H2O) 3]n (H4cbut = 1,2,3,4- cyclobutanetetracarboxylic acid)

A novel cobalt(II) complex of formula [Co2(cbut)(H 2O)3]n (1) (H4cbut = 1,2,3,4-cyclobutanetetracarboxylic acid) has been synthesized under hydrothermal conditions and its crystal structure has been determined by means of synchrotron radiation and neutron powder diffraction. The crystal structure of 1 consists of layers of cobalt(II) ions extending in the bc-plane which are pillared along the crystallographic a-axis through the skeleton of the cbut 4- ligand. Three crystallographically independent cobalt(II) ions [Co(1), Co(2), and Co(3)] occur in 1. They are all six-coordinate with four carboxylate-oxygens [Co(1)-Co(3)] and two cis-[Co(1)] or trans-water molecules [Co(2) and Co(3)] buildin…

Crystal structure and magnetic properties of the single-μ-chloro copper(II) chain [Cu(bipy)Cl2] (bipy = 2,2′-bipyridine)

Abstract The crystal and molecular structure of the copper(II) chain [Cu(bipy)Cl2] (1) (bipy = 2,2′-bipyridine) has been determined by X-ray diffraction methods. The crystal structure of 1 consists of neutral single chloro-bridged copper(II) chains with alternating short and long Cu–Cl distances through a screw axis parallel to a. The copper surrounding is best described as distorted square pyramidal, the equatorial plane being built by the two nitrogen atoms of the chelating bipy and two chlorine atoms (one terminal and the other bridging), whereas the apical position is filled by the bridging chlorine atom from the symmetry-related adjacent unit. The equatorial Cu–Cl bonds (2.291(3) and 2…

Generation of lanthanide coordination polymers with dicarboxylate ligands: synthesis, structure, thermal decomposition and magnetic properties of the two-dimensional triaquatris(malonato)dipraseodymium(III) dihydrate {[Pr2(C3H2O4)3(H2O)3]·2H2O}

The malonate complex of formula [Pr2(C3H2O4)3(H2O)3]·2H2O (1) was prepared and his crystal structure determined by X-ray diffraction methods. 1 crystallizes in the monoclinic space group P21, Z = 4, with unit cell parameters a = 7.631(2), b = 12.899(4), c = 8.923(2) A and β = 101.11(3)°. 1 is a polymer which grows in the (110) plane. The hydrogen bond stabilizes the crystal structure forming a three-dimensional network. The two non-equivalent praseodymium(III) ions have different environments. Finally, the thermal behaviour and magnetic properties were investigated.

Heterobimetallic Oxalate‐Bridged M II Re IV (M = Zn, Cu, Ni, Co and Mn) Complexes Incorporating Bis(3,5‐dimethylpyrazol‐1‐yl)methane: Synthesis and Magneto‐Structural Studies

Five oxalato-bridged heterobimetallic compounds of general formula [ReCl4(ox)M(bdmpzm)2].2MeCN [ox = oxalate, bdmpzm = bis(3,5-dimethylpyrazol-1-yl)methane and M = Zn (1),Cu (2), Ni (3), Co (4) and Mn (5)] have been successfully synthesized in self-assembly reactions of the [ReCl4(ox)]2- metalloligand with the coordinatively unsaturated [M(bdmpzm)2]2+ complex generated in situ by the reaction of the suitable metal(II) salt with the bdmpzm ligand. 1-5 are isostructural compounds whose crystal structures consist of neutral heterodinuclear [ReCl4(ox)M(bdmpzm)2] units and free acetonitrile molecules. The magnetic properties of 1-5 were investigated in the temperature range 2.0-300 K. The nature…

Synthesis, crystal structure and magnetic properties of the three-dimensional compound [Na2Ni(mal)2(H2O)6]n (H2mal=malonic acid)

Abstract A new three-dimensional nickel–sodium compound of formula [Na 2 Ni(mal) 2 (H 2 O) 6 ] n (H 2 mal=malonic acid) was prepared and its structure was determined by X-ray diffraction methods. Four malonate–oxygen atoms and two trans -(Ni) or cis -(Na) coordinated water molecules build distorted octahedral surroundings around the metal atoms. The malonate group exhibits bidentate (Ni) and tetrakis-monodentate (Na) coordination modes. The structure can be described as corrugated sheets of malonato-containing Ni(II) and Na(I) cations which grow in the (101) plane, each sheet being linked to the adjacent one in the [101] direction through bis(μ-aqua)disodium(I) units. Within each corrugated…

Dinuclear, tetranuclear and one-dimensional pyrazine-based copper(II) complexes: preparation, X-ray structure and magnetic properties.

The preparation, crystal structures and magnetic properties of the copper(II) complexes of formula [Cu(2)(tppz)(H(2)O)(2)(CF(3)SO(3))(4)] (1), [Cu(tppz)(CrO(4))](n) x 3nH(2)O (2) and [Cu(4)(tppz)(4)(H(2)O)(4)(MoO(4))(2)](CF(3)SO(3))(4) x 7 H(2)O (3) [tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine] are reported. Complex 1 is a dinuclear species where tppz adopts a bis-tridentate bridging mode with an intramolecular copper-copper separation of 6.5221(6) A. Each copper(II) ion in 1 has an elongated octahedral geometry with three tppz nitrogen atoms and a water molecule in the equatorial positions and two triflate oxygen atoms occupying the axial sites. Complex 2 is a uniform copper(II) chain where…

Synthesis, crystal structures and magnetic properties of cyanide- and phenolate-bridged [MIIINiII]2tetranuclear complexes (M = Fe and Cr)

The binuclear complex NiII2L(H2O)2(ClO4)2 (1) and the neutral tetranuclear bimetallic compounds [{MIII(phen)(CN)4}2{NiII2L(H2O)2}]·2CH3CN with M = Fe (2) and Cr (3) [H2L = 11,23-dimethyl-3,7,15,19-tetraazatricyclo[19.3.1.19,13]hexacosa-2,7,9,11,13(26),14,19,21(25),22,24-decaene-25,26-diol] have been synthesized and the structures of 2 and 3 determined by single crystal X-ray diffraction. 2 and 3 are isostructural compounds whose structure is made up of centrosymmetric binuclear cations [Ni2(L)(H2O)2]2+ and two peripheral [M(phen)(CN)4]− anions [M = Fe (2) and Cr (3)] acting as monodentate ligands towards the nickel atoms through one of their four cyanide nitrogen atoms. The environment of t…

One-dimensional oxalato-bridged heterobimetallic coordination polymers by using [the [Cr(pyim)(C2O4)2]− complex as metalloligand [pyim = 2-(2′-pyridyl)imidazole]

Abstract Four new coordination polymers based on the use of the [Cr(pyim)(C2O4)2]− species as a metalloligand, namely [LiCr(pyim)(C2O4)2(MeOH)]n (1), {[CaCr2(pyim)2(C2O4)4]·2MeOH}n (2), {[SrCr2(pyim)2(C2O4)4(H2O)]·0.45MeOH·4.55H2O}n (3) and {[CdCr2(pyim)2(C2O4)4]·MeOH}n (4) [pyim = 2-(2′-pyridyl)imidazole] have been synthesized and characterized by elemental analyses, IR spectra and X-ray diffraction on single crystals. Complex 1 is a neutral heterobimetallic chain where the tris(chelated) chromium(III) unit acts as a bis-bidentate ligand towards {Li(MeOH)}+ fragments through its two oxalate ligands, each lithium ion being five-coordinate in a intermediate surrounding between square pyramid…

Coordination complexes incorporating pyrophosphate: Structural overview and exploration of their diverse magnetic, catalytic and biological properties

Abstract Current attention continues to revolve around the chemistry and biochemistry associated with polyphosphate anions because of their importance in biology. A pivotal intermediate within this family is the pyrophosphate tetraanion, P2O74−. Considering its biological relevance and the multidentate nature that makes it an ideal ligand in the field of the coordination chemistry, there is a growing interest in the use of this anion in building new class of molecules/compounds for different purposes. While the total number of characterized structures still remains modest, several new pyrophosphate-containing coordination complexes have been reported in the last decade, as well as different…

Synthesis, Crystal Structure and Magnetic Properties of Heteropolynuclear Re IV M II Complexes Based on the Robust [ReCl 5 (pyzCOO)] 2– Unit (pyzCOO = 2‐pyrazinecarboxylate)

The syntheses, crystal structures and magnetic properties of four rhenium(IV) compounds of formulae NBu4[ReCl5(pyzCOOH)]·H2O (1), [ReCl5(µ-pyzCOO)M(dmphen)2]·2CH3CN [M = Ni (2) and Co (3)] and {[ReCl5(µ3-pyzCOO)]2Mn2(dmphen)3}n (4) (NBu4 = tetra-n-butylammonium cation, pyzCOOH = 2-pyrazinecarboxylic acid, dmphen = 2,9-dimethyl-1,10-phenanthroline) are reported herein. Compound 1 was obtained by the reaction of NBu4[ReCl5(dmf)] (dmf = dimethylformamide) with pyzCOOH in acetone, whereas the other complexes were obtained by the reaction of 1 with M(ClO4)2·6H2O [M = Ni (2), Co (3), Mn (4)] and dmphen in acetonitrile. Complex 1 is a mononuclear compound, 2 and 3 are neutral heterodinuclear compl…

Azido- und 2,2′-Bipyrimidin-Liganden als nützliche Werkzeuge zur Synthese zwei- und dreidimensionaler Mangan(II)-Netzwerke

Syntheses, crystal structures and magnetic properties of one- and two-dimensional pap-containing copper(II) complexes (pap = pyrazino[2,3-  f  ][4,7]phenanthroline)

Three polynuclear complexes containing copper(II) and pyrazino[2,3-f][4,7]phenanthroline (pap) as the basic building blocks have been prepared [Cu2(pap)(H2O)2(NO3)3]n[NO3]n1, [Cu4(pap)4Cl7]nCln·15nH2O 2, and [Cu4(pap)4(H2O)4(C4O4)2]n[C4O4]n[NO3]2n·12nH2O 3, and their crystal structures and variable-temperature magnetic susceptibilities determined. Compound 1 is a single stranded zigzag chain where pap and nitrate alternate as bridges between the copper atoms. The copper coordination geometry is to a first approximation distorted square pyramidal, but with an additional semi-coordinated oxygen from non-bridging nitrate groups. The bridging nitrate coordinates in the apical position to both c…

Design of single chain magnets through cyanide-bearing six-coordinate complexes

Abstract The design and preparation of stable cyanide-bearing six-coordinate complexes of formula [MIII(L)(CN)x](x + l − m)− (M = trivalent transition metal ion and L = polydentate blocking ligand) are summarized here. Their use as ligands towards either fully hydrated metal ions or coordinatively unsaturated preformed species, to afford a wide variety of low-dimensional metal assemblies whose nuclearity, dimensionality and magnetic properties can be tuned, is also reviewed. Special emphasis is put on the appropriate choice of the end-cap ligand L whose denticity determines the number of coordinated cyanide groups in the mononuclear precursors. Among the different new spin topologies obtain…

Co-existence of ferro- and antiferromagnetic interactions in a hexanuclear mixed-valence CoIII2MnII2MnIV2 cluster sustained by a multidentate Schiff base ligand

The successful utilization of the “direct synthesis” approach yielded the unprecedented hexanuclear complex of formula [Co2MnII2MnIV2(L1)4Cl2(μ3-O)2(dmf)4]·2dmf (1) (H3L is the Schiff base derived from the condensation of salicylaldehyde and 3-aminopropane-1,2-diol). Single crystal X-ray analysis revealed that 1 crystallizes in the monoclinic system P21/c and it contains a rare mixed-valence {CoIII2MnII2MnIV2(μ2-O)8(μ3-O)2} core where all metal ions are linked through the phenolato and alkoxo groups of the L3− ligand. Besides the charge balance resulting from the X-ray structure, the oxidation state of the metal ions has been confirmed by XPS spectroscopy. Cryomagnetic studies indicate the …

Guanine-containing copper(ii) complexes: synthesis, X-ray structures and magnetic properties

Three new compounds of formula {[Cu(gua)(H(2)O)(3)](BF(4))(SiF(6))(1/2)}(n) (1), {[Cu(gua)(H(2)O)(3)](CF(3)SO(3))(2).H(2)O}(n) (2) and [Cu(gua)(2)(H(2)O)(HCOO)]ClO(4).H(2)O.1/2HCOOH] (3) [gua = 2-amino-1H-purin-6(9H)-one] showing the unprecedented coordination of neutral guanine, have been synthesised and structurally characterized. The structures of the compounds 1 and 2 contain uniform copper(II) chains of formula [Cu(gua)(H(2)O)(3)](n)(2n+), where the copper atoms are bridged by guanine ligands coordinated via N(3) and N(7). The electroneutrality is achieved by uncoordinated tetrafluoroborate and hexafluorosilicate (1) and triflate (2). Each copper atom in 1 and 2 is five-coordinated in …

Slow magnetic relaxation in carbonato-bridged dinuclear lanthanide(iii) complexes with 2,3-quinoxalinediolate ligands

The coordination chemistry of the 2,3-quinoxalinediolate ligand with different lanthanide(iii) ions in basic media in air affords a new family of carbonato-bridged M 2 III compounds (M = Pr, Gd and Dy), the Dy 2 III analogue exhibiting slow magnetic relaxation behaviour typical of single-molecule magnets. This journal is © 2012 The Royal Society of Chemistry.

New 3d–4f supramolecular systems constructed by [Fe(bipy)(CN)4]− and partially blocked lanthanide cations

Abstract The reaction of acetonitrile (1–5) and mixed acetonitrile/water 1:1 (6–9) solutions containing the cyanide-bearing [Fe(bipy)(CN)4]− building block (bipy = 2,2′-bipyridine) and the partially blocked [Ln(bpym)]3+ cation (Ln = lanthanide trivalent cation and bpym = 2,2′-bipyrimidine) has afforded two new families of 3d–4f supramolecular assemblies of formula [Ln(bpym)(NO3)2(H2O)3][Fe(bipy)(CN)4] · H2O · CH3CN [Ln = Sm (1), Gd (2), Tb (3), Dy (4) and Ho (5)] and [Ln(bpym)(NO3)2(H2O)4][Fe(bipy)(CN)4] [Ln = Pr (6), Nd (7), Sm (8), Gd (9)]. They crystallize in the P21/c (1–5) and P2/c (6–9) space groups and their structures are made up of [Fe(bipy)(CN)4]− anions (1–9) and [Ln(bpym)(NO3)2(…

Effect of Protonated Organic Cations and Anion−π Interactions on the Magnetic Behavior of Hexabromorhenate(IV) Salts

Two novel Re-IV compounds of formula (Hbpym)(2)[(ReBr6)-Br-IV]center dot 4H(2)O (1) and (H(4)biim)[(ReBr6)-Br-IV]center dot 4H(2)O (2) [Hbpym(+) = 2,2'-bipyrimidinium cation and H(4)biim(2+) = 2,2'-biimidazolium dication] have been prepared and magnetostructurally characterized. 1 and 2 exhibit distinct crystal packing, and the presence of weak intermolecular contacts, such as Re-Br...B-rRe (1 and 2), Re-Br center dot center dot center dot(H2O)center dot center dot center dot BrRe (1 and 2), and Re-Br center dot center dot center dot pi center dot center dot center dot Br-Re (2), lead to different magnetic behaviors. While 1 is antiferromagnetic, 2 is a ferromagnetic compound and indeed the…

Enantiopure Conducting Salts of Dimethylbis(ethylenedithio)tetrathiafulvalene (DM‐BEDT‐TTF) with the Hexachlororhenate(IV) Anion

Invited for the cover of this issue is the group of Narcis Avarvari (CIMI team) at the Laboratory MOLTECH-Anjou, UMR 6200 CNRS – Universite d'Angers, France. The cover image shows the enantiopure tetrathiafulvalene precursors used for the preparation of chiral radical cation conducting salts, together with an artwork of their packing diagrams and the suggested mirror image relationship between them.

Heterometallic CoII-CoIII-MII alkoxido-bridged heptanuclear motifs (M = Cu, Zn). Syntheses, crystal structures and magnetic properties

Two new alkoxido-bridged heterometallic complexes of formula [CoIICoIII 3CuII 3(dea)6(CH3COO)3](ClO4)0.75(CH3COO)1.25 (1) and [CoII 2CoIII 2ZnII 3(tea)2(piv)6(CH3O)2(OH)2(CH3OH)2]·H2O 2 (H2dea=diethanolamine, H3tea=triethanolamine and Hpiv=pivalic acid) have been assembled using aminoalcohol ligands. The cationic core in 1 possesses a threefold crystallographic axis, and it exhibits a set of three copper(II), one cobalt(II) and three cobalt(III) ions arranged as a hexagon of alternating copper(II) and cobalt(III) ions around the central cobalt(II) ion. Each edge of the hexagon is defined by a double alkoxido bridge, the outer one being bis-monodentate with copper(II)-cobalt(III) pair wherea…

Palladium(II)–Copper(II) Assembling with Bis(2-pyridylcarbonyl)amidate and Bis(oxamate) Type Ligands

Five new complexes of formula K4[Pd2(mpba)2] · 4H2O (1), {[K4(H2O)(dmso)][Pd2(mpba)2]} (2), {[Cu(bpca)]4[Pd2(mpba)2]} · 6H2O (3), {[Cu(bpca)]2[Pd(opba)]} · 1.75dmso · 0.25H2O (4), {[Cu(bpca)]2[Pd(opba)]}n · ndmso (5) [H4mpba =1,3-phenylenebis(oxamic acid), H4opba = 1,2-phenylenebis(oxamic acid), Hbpca = bis(2-pyridylcarbonyl)amide, and dmso = dimethyl sulfoxide] have been prepared and investigated by infrared spectroscopy, thermal analysis, single crystal X-ray diffraction, and magnetic susceptibility techniques. The structure of 2 consists of a [Pd2(mpba)2]4– anionic entity in which the palladium(II) cations are coordinated by two mpba ligands resulting in a dipalladium(II) unit that acts …

[Mn2(bipym)(H2O)8]4+and [Fe(bipy)(CN)4]−as building blocks in designing novel bipym- and cyanide-bridged heterobimetallic complexes (bipym = 2,2′-bipyrimidine and bipy = 2,2′-bipyridine)

Two new cyano complexes, K[Fe(bipy)(CN)4]·H2O (1) and (μ-bipym)[Mn(H2O)3{Fe(bipy)(CN)4}]2[Fe(bipy)(CN)4]2·12H2O (2), have been synthesised and their structures determined by single-crystal X-ray diffraction. Complex 1 is made up of mononuclear [Fe(bipy)(CN)4]− anions, potassium cations and water molecules of crystallization. The iron(III) is six-coordinated, being surrounded by two nitrogen atoms of a chelating bipy and four carbon atoms of four cyanide groups [Fe–N and Fe–C 1.991(3)–1.990(3) and 1.958(5)–1.914(5) A, respectively]. Complex 2 consists of centrosymmetric tetranuclear (μ-bipym)[Fe(H2O)3{Fe(bipy)(CN)4}]22+ cations, [Fe(bipy)(CN)4]− anions and water molecules of crystallization.…

Enantiopure Conducting Salts of Dimethylbis(ethylenedithio)tetrathiafulvalene (DM‐BEDT‐TTF) with the Hexachlororhenate(IV) Anion (Eur. J. Inorg. Chem. 24/2014)

A dihydrogen arsenate-mediated supramolecular network: crystal structure and magnetic properties of {[(bipy)Cu(μ-H2AsO4)(H2AsO4)]2}n

Treatment of an aqueous suspension of Cu(OH)2 and 2,2′-bipyridine (bipy) with either Na2HAsO4·7H2O (1∶1∶2) or As2O5 (1∶1∶1) yields single crystals of {[(bipy)Cu(μ-H2AsO4)(H2AsO4)]2}n, 1, on standing. The solid-state structure of 1 consists of a three dimensional supramolecular network, supported by a combination of coordination covalent, hydrogen bonding and face-to-face π–π interactions. Variable temperature magnetic susceptibility measurements reveal very weak antiferromagnetic coupling between Cu(II) centres across the dihydrogen arsenate bridges (J = −0.58 cm−1).

Polymorphic Derivatives of NiII and CoII Mesocates with 3D Networks and “Brick and Mortar” Structures: Preparation, Structural Characterization, and Cryomagnetic Investigation of New Single-Molecule Magnets

In this work we describe the preparation, spectroscopic, thermal and structural characterization, and cryomagnetic investigation of four new polymorphic derivatives of the [M2(H2mpba)3]2– mesocate ...

Structural versatility in cobalt(ii) complexes with 1,2,4,5-benzenetetracarboxylic acid (H4bta) and 4,4′-bipyridine-N,N′-dioxide (dpo)

Four new high-spin cobalt(II) complexes of formula [Co(H2O)6](H2bta)·dpo·4H2O (1), [{Co(H2O)4(dpo)}2(bta)]·4H2O·(2), [Co(H2O)2)(dpo)2(H2bta)]n (3) and [Co(H2O)3(dpo)(bta)1/2]n (4) (H4bta = 1,2,4,5-benzenetetracarboxylic acid and dpo = 4,4′-bipyridine-N,N′-dioxide) have been synthesized and their structures solved by single crystal X-ray diffraction methods. Compound 1 is an ionic salt whose structure is made up of [Co(H2O)6]2+ cations, H2bta2− anions, uncoordinated dpo groups and crystallization water molecules, which are linked by extensive hydrogen bonds to afford a three-dimensional network. The structure of 2 consists of bta-bridged dinuclear cobalt(II) complexes where four coordinated …

A three-dimensional copper(ii) 12-metallacrown-4 complex with malonomonohydroxamic acid (H3mmh) as a ligand

Slow diffusion of an ethanolic solution of copper(ii) into an aqueous solution of partially deprotonated malonodihydroxamic acid (H4mdh) affords the pentanuclear complex of formula {[K(H2O) 2]2[Cu5(mmh)4]}n (1) (H3mmh = malonomonohydroxamic acid) which is formed by 12-MC-4 metallacrown units with the fifth copper(ii) ion being placed at the center of the square metallacrown unit. The dianionic pentacopper(ii) planar entity interacts with diaquapotassium(i) counterions through the carboxylate-oxygen atoms resulting in a neutral three-dimensional structure. Magnetic susceptibility measurements in the temperature range 1.9-300 K for 1 show the occurrence of relatively strong antiferromagnetic …

Synthesis, Structural, Magnetic and Thermal Characterization of {[Cu(bipy)] 2 (μ‐HP 2 O 7 )(μ‐Cl)}·H 2 O

Copper(II) hydroxide reacts with 2,2′-bipyridine (bipy) and sodium pyrophosphate in a 2:2:1 stoichiometric ratio under ambient conditions at pH 1.6 in water. The resulting neutral dinuclear CuII complex features a bridging set containing bridging monoprotonated pyrophosphate and a monoatomic chloro bridge (making this the first pyrophosphate bridged coordination complex containing an alternate, additional halide bridge between the metal centers). Single-crystal X-ray diffraction studies revealed the complex to be {[Cu(bipy)]2(μ-HP2O7)(μ-Cl)}·H2O. The structure consists of a dimeric copper(II) system with each metal ion in a square pyramidal geometry. The asymmetric [Cu(bipy)]2+ units are br…

Structure and magnetic properties of a linear oximato-bridged tetranuclear copper(II) complex

Abstract The tetranuclear copper(II) complex of formula [Cu2(dmg)(Hdmg)(terpy)]2(ClO4)2 (1) (H2dmg = dimethylglyoxime and terpy = 2,2′:6′,2″-terpyridine) has been synthesized and its crystal structure determined by X-ray diffraction methods. It crystallizes in the triclinic system, space group P(−1), with a = 14.382(3), b = 13.728(3), c = 8.979(2) A, α = 96.99(2), β = 111.85(2), γ = 111.22(3)°, V = 1465.0(9) A3, Z = 1, Dc = 1.607 g cm−3, Mr = 1418.0, F(000) = 719, λ(Mo Kα) = 0.71073 A, μ(Mo Kα) = 16.61 cm−1 and T = 298 K. A total of 4891 reflections were measured over the range 2 ≤ θ ≤ 25° and 4393 of them were unique (I > 2.5σ(I) and used in the structural analysis. The structure of 1 may …

A reusable polymer-supported copper(I) catalyst for triazole click reaction on water: An experimental and computational study

Copper(II) assembling with bis(2-pyridylcarbonyl)amidate and N,N'-2,2-phenylenebis(oxamate).

We herein present the synthesis and X-ray structures of five copper(II) complexes of formulae [Cu(bpca)(CF3SO3)(H2O)]·H2O (1), [Cu(bpca)(Phpr)(H2O)]·3/2H2O (2), {[Cu(bpca)]2[Cu(opba)(H2O)]}·H2O (3), {[Cu(bpca)]2(H2opba)}2·6H2O (4) and [Cu(bpca)(EtH2opba)]n (5), where bpca = bis(2-pyridylcarbonyl)amidate, Phpr = 3-phenylpropionate, CF3SO3(−) = triflate (anion of the trifluoromethanesulphonic acid), H4opba = N,N′-1,2-phenylenebis(oxamic acid), and EtH3opba = monoethyl ester derivative of the H4opba. 1 and 2 are mononuclear copper(II) complexes where the copper atom is five-coordinate in distorted square pyramidal surroundings with a tridentate bpca and a water molecule (1)/carboxylate oxygen …

Syntheses, crystal structures and magnetic properties of polynuclear 1,4,5,8,9,12-hexaazatriphenylene (hat)-bridged copper(II) complexes

Three polynuclear compounds containing copper(II) and 1,4,5,8,9,12-hexaazatriphenylene (hat) as the basic building blocks have been prepared, [Cu4(hat)2Cl8]n·6nH2O 1, [Cu(hat)(H2O)2]n[NO3]2n2, and [Cu2(hat)(H2O)6]n[SO4]2n·2nH2O 3, their crystal structures determined and variable-temperature magnetic susceptibility data measured. The basic building block in 1 is the dinuclear [Cu2(hat)Cl4] entity, two such units being connected to tetranuclear units through relatively strong axial Cu–Cl bonds (out-of-plane di-μ-chloro bridges). Weaker axial Cu⋯Cl interactions link the units into a sheet structure. In 2 and 3 hat-bridged copper(II) chains extending along glide planes are present. hat serves a…

Ferromagnetic Coupling between Low- and High-Spin Iron(III) Ions in the Tetranuclear Complex fac-{[FeIII{HB(pz)3}(CN)2(μ-CN)]3FeIII(H2O)3}· 6H2O ([HB(pz)3]- = Hydrotris(1-pyrazolyl)borate)

The novel mononuclear PPh4-fac-[FeIII{HB(pz)3}(CN)3]·H2O (1) [PPh4+= tetraphenylphosphonium cation; (HB(pz)3)- = hydrotris(1-pyrazolyl)borate] and tetranuclear fac-{[FeIII{HB(pz)3}(CN)2(μ-CN)]3FeIII(H2O)3}·6H2O (2) have been prepared and characterized by X-ray diffraction analysis. Crystal data for compound 1:  monoclinic, space group P21/c, a = 9.575(3) A, b = 21.984(4) A, c = 16.863(3) A, β = 100.34(2)°, U = 3486(1) A3, Z = 4. Crystal data for compound 2:  orthorhombic, space group Pnam, a = 14.084(3) A, b = 14.799(4) A, c = 25.725(5) A, U = 5362(2) A3, Z = 4. Compound 1 is a low-spin iron(III) compound with three cyanide ligands in fac arrangement and a tridentate pyrazolylborate ligand …

Geometric isomeric pairs: synthesis, structure, thermal decomposition and magnetic properties of cis- and trans-[Cr(mal)(bpy)(H2O)2][NO3]·xH2O (H2mal=malonic acid, bpy=2,2′-bipyridine)

Abstract Procedures are given for the preparation and isolation of cis-[Cr(mal)(bpy)(H2O)2][NO3]·3H2O (I) and trans-[Cr(mal)(bpy)(H2O)2][NO3]·H2O (II) (H2mal=malonic acid, bpy=2,2′-bipyridine). The single crystals X-ray structure of cis-compound reveals that the cations and anions as well as cations between cations are linked into hydrogen-bonded chains. Unfortunately, little structural information is available for the trans compound II (only isotropic cation refinement), nevertheless, from this result is observed that there also exists a hydrogen-bonded network between anion units. Thermal analysis and magnetic behaviour for both compounds were studied.

Bis(oxalato)chromium(III) complexes: Versatile tectons in designing heterometallic coordination compounds

Abstract The mononuclear oxalato-containing chromium(III) complexes of general formula [Cr(AA)(C2O4)2]− (AA = α-diimine type ligand) are able to produce a large variety of heterometallic complexes by acting as ligands towards either fully solvated metal ions or preformed cationic complexes with available coordination sites. This review focuses on the structural diversity of the polynuclear complexes (oligonuclear and coordination polymers) which are generated by the bis(oxalato)chromate(III) species, with a special emphasis to their magnetic properties.

New cyanide-bridged Mn(III)-M(III) heterometallic dinuclear complexes constructed from [M(III)(AA)(CN)4]- building blocks (M = Cr and Fe): synthesis, crystal structures and magnetic properties.

Three Mn(III)-M(III) (M = Cr and Fe) dinuclear complexes have been obtained by assembling [Mn(III)(SB)(H(2)O)](+) and [M(III)(AA)(CN)(4)](-) ions, where SB is the dianion of the Schiff-base resulting from the condensation of 3-methoxysalicylaldehyde with ethylenediamine (3-MeOsalen(2-)) or 1,2-cyclohexanediamine (3-MeOsalcyen(2-)): [Mn(3-MeOsalen)(H(2)O)(µ-NC)Cr(bipy)(CN)(3)]·2H(2)O (1), [Mn(3-MeOsalen)(H(2)O)(µ-NC)Cr(ampy)(CN)(3)][Mn(3-MeOsalen)(H(2)O)(2)]ClO(4)·2H(2)O (2) and [Mn(3-MeOsalcyen)(H(2)O)(µ-NC)Fe(bpym)(CN)(3)]·3H(2)O (3) (bipy = 2,2'-bipyridine, ampy = 2-aminomethylpyridine and bpym = 2,2'-bipyrimidine). The [M(AA)(CN)(4)](-) unit in 1-3 acts as a monodentate ligand towards th…

Exchange Coupling in Cyano-Bridged Homodinuclear Cu(II) and Ni(II) Complexes:  Synthesis, Structure, Magnetism, and Density Functional Theoretical Study

The synthesis and structural characterization of several new cyano-bridged copper(II) and nickel(II) homodinuclear complexes is presented. The measure of magnetic properties for these complexes is complemented with a computational study of the exchange coupling for several model structures representing this family of compounds. The influence of several factors on the coupling constant has been examined, coordination position occupied by the bridging ligand, distortions of the coordination environment, and relative disposition of the cyanide ion with respect to the M-M vector. Comparison of experimental and calculated coupling constants allows for the rationalization of the most relevant fea…

Highly selective chemical sensing in a luminescent nanoporous magnet.

Among the wide variety of properties of interest that a given material can exhibit, luminescence is attracting an increasing attention due to its potential application in optical devices for lighting equipment and optical storage, [ 1a − c] optical switching, [ 1d ,e] and sensing. [ 1f − i ] At this respect, many scientists, working in the multidisciplinary fi eld of the materials science, have directed their efforts to the obtention of luminescent materials with potential sensing applications. For instance, sensitive and selective detection of gas and vapor phase analytes can result specially interesting because of the variety of applications that can be found in many different fi elds. A …

Photoswitching of the antiferromagnetic coupling in an oxamato-based dicopper(ii) anthracenophane

Thermally reversible photomagnetic (ON/OFF) switching behavior has been observed in a dinuclear oxamatocopper(ii) anthracenophane upon UV light irradiation and heating; the two CuII ions (SCu = 1/2) that are antiferromagnetically coupled in the dicopper(ii) metallacyclic precursor (ON state) become uncoupled in the corresponding [4+4] photocycloaddition product (OFF state), as substantiated from both experimental and theoretical studies. © 2011 The Royal Society of Chemistry.

Postsynthetic Improvement of the Physical Properties in a Metal-Organic Framework through a Single Crystal to Single Crystal Transmetallation

As ingle crystal to single crystal transmetallation process takes place in the three-dimensional (3D) metal- organic framework (MOF) of formula Mg II 2{Mg II 4(Cu II 2- (Me3mpba)2)3}·45 H2 O( 1 ;M e 3mpba 4¢ = N,N'-2,4,6-trimethyl- 1,3-phenylenebis(oxamate)). After complete replacement of the Mg II ions within the coordination network and those hosted in the channels by either Co II or Ni II ions, 1 is transmetallated to yield two novel MOFs of formulae Co2 II {Co II 4(Cu II 2(Me3- mpba)2)3}·56 H2 O( 2 )a nd Ni2 II {Ni II 4(Cu II 2(Me3mpba)2)3}· 54 H2 O( 3). This unique postsynthetic metal substitution affords materials with higher structural stability leading to enhanced gas sorption and m…

Syntheses, Structures, and Magnetic Properties of Copper( II ) Complexes with 1,3‐[Bis(2‐pyridylmethyl)amino]benzene (1,3‐tpbd) as Ligand

The dinuclear copper(II) complexes {[Cu2(1,3-tpbd)(H2O)(OAc)2](ClO4)2}0.23{[Cu2(1,3-tpbd)(H2O)2(OAc)](ClO4)3}0.77·0.77H2O (1), [Cu2(1,3-tpbd)(H2O)2(OAc)2](ClO4)2·2H2O (2), and the tetranuclear copper(II) complex [Cu4(1,3-tpbd)2(H2O)2(SO4)4]·8H2O (3) {1,3-tpbd = 1,3-bis[bis(2-pyridylmethyl)amino]benzene} were synthesised and structurally characterised by X-ray diffraction. Variable-temperature (2.0−290 K) magnetic susceptibility measurements on these complexes as well as on the dinuclear copper(II) complex [Cu2(1,3-tpbd)(H2O)2(ClO4)3]ClO4 (4) (whose structure was published earlier) were performed. In contrast to 2 and 3, significant ferromagnetic coupling with J = +9.3 cm−1 was observed for …

Cobalt(II) Sheet-Like Systems Based on Diacetic Ligands: from Subtle Structural Variances to Different Magnetic Behaviors

The preparation, X-ray crystallography, and magnetic investigation of the compounds [Co(H(2)O)(2)(phda)](n) (1), [Co(phda)](n) (2), and [Co(chda)](n) (3) [H(2)phda = 1,4-phenylenediacetic acid and H(2)chda = 1,1-cyclohexanediacetic acid] are described herein. The cobalt atoms in this series are six- (1) and four-coordinated (2 and 3) in distorted octahedral (CoO(6)) and tetrahedral (CoO(4)) environments. The structures of 1-3 consists of rectangular-grids which are built up by sheets of cobalt atoms linked through anti-syn carboxylate bridges, giving rise to either a three-dimensional structure across the phenyl ring (1 and 2) or to regularly stacked layers with the cyclohexyl groups acting…

Synthesis, X‐ray Structure, Thermal and Magnetic Behavior of [(bipy) 2 Ni 2 (μ‐Cl) 2 Cl 2 (H 2 O) 2 ]: The First Neutral Ferromagnetically Coupled Six‐Coordinate Dichlorido‐Bridged Nickel(II) Dimer

NiCl2·6H2O and 2,2′-bipyridine (bipy) (1:1) were allowed to react under ambient conditions in dimethyl sulfoxide in the presence of acetylacetone (Hacac). The resulting green solution was concentrated in vacuo, and a green solid was isolated by precipitation with cold acetone. X-ray quality crystals of [(bipy)2Ni2(μ-Cl)2(Cl)2(H2O)2] (1) were grown by subsequent vapor/liquid diffusion of acetonitrile into a methanolic solution for one week. The structure of 1 consists of a dimeric nickel system with each metal atom in an octahedral geometry. Both equatorial bridging and axial chlorine atoms are present in this neutral species. The nickel–nickel distance (3.441 A) is the shortest reported to …

1,2,4,5‐Benzenetetracarboxylic Acid and 4,4′‐Bipyridine as Ligands in Designing Low‐Dimensional Coordination Polymers

The combined use of 1,2,4,5-benzenetetracarboxylic acid (H4bta) and 4,4′-bipyridine (bpy) as ligands with MnII and CoII ions afforded two polymeric compounds with the formulae [Mn(Hbta)(Hbpy)(H2O)2] (1) and [H2bpy][Co(bta)(bpy)(H2O)2] (2). 1 and 2 were prepared under hydrothermal conditions (145 °C, 3 h) and characterized by elemental analysis, IR spectroscopy, TG-DTA analysis and single-crystal X-ray diffraction methods. 1 exhibits a novel double chain structure growing along the b axis where the manganese atoms are linked by tris-monodentate Hbta3− ligands. The values of the manganese···manganese intrachain separations are 7.627(2) A [Mn(1)···Mn(1c); c = −x + 1/2, y − 1/2, −z] and 9.274(4…

Dimensionality Switching Through a Thermally Induced Reversible Single-Crystal-to-Single-Crystal Phase Transition in a Cyanide Complex

International audience; The heterometallic hexanuclear cyanide-bridged complex {[Mn(bpym)(H(2)O)](2)[Fe(HB(pz)(3))(CN)(3)](4)} (1), its C(15)N and D(2)O enriched forms {[Mn(bpym)(H(2)O)](2)[Fe(HB(pz)(3))(C(15)N)(3)](4)} (2) and {[Mn(bpym)(D(2)O)](2)[Fe(HB(pz)(3))(CN)(3)](4)} (3), and the hexanuclear derivative complex {[Mn(bpym)(H(2)O)](2)[Fe(B(pz)(4))(CN)(3)](4)}*4H(2)O (4) [bpym = 2,2'-bipyrimidine, HB(pz)(3)(-) = hydrotris(1-pyrazolyl)borate, B(pz)(4)(-) = tetra(1-pyrazolyl)borate] have been synthesized. Their structures have been determined through single-crystal X-ray crystallography at different temperatures. Whereas 3 and 4 maintain a discrete hexanuclear motif during the entire temp…

Syntheses, crystal structures and magnetic properties of five new manganese(ii) complexes: Influence of the conformation of different alkyl/aryl substituted malonate ligands on the crystal packing

et al.

Single ion magnet behaviour in a two-dimensional network of dicyanamide-bridged cobalt(II) ions

A novel two-dimensional coordination polymer of the formula [Co(dca)2(atz)2]n (1) resulted from assembling trans-bis(2-amino-1,3,5-triazine)cobalt(II) motifs by dicyanamide spacers. Variable-temperature dc and ac magnetic susceptibility measurements of 1 show that the high-spin cobalt(II) ions act as single ion magnets (SIMs).

Magneto-structural correlations in dirhenium(iv) complexes possessing magnetic pathways with even or odd numbers of atoms

The employment of pyrazine (pyz), pyrimidine (pym) and s-triazine (triz) ligands in ReIV chemistry leads to the isolation of a family of complexes of general formula (NBu4)2[(ReX5)2(μ-L)] (L = pyz, X = Cl (1) or Br (2); L = pym, X = Br (3); L = triz, X = Br (4)). 1-4 are dinuclear compounds where two pentahalorhenium(iv) fragments are connected by bidentate pyz, pym and triz ligands. Variable-temperature magnetic measurements, in combination with detailed theoretical studies, uncover the underlying magneto-structural correlation whereby the nature of the exchange between the metal ions is dictated by the number of intervening atoms. That is, the spin-polarization mechanism present dictates …

Crystal structures and magnetic properties of the squarate-O1,On-bridged dinuclear copper(II) complexes [Cu2(phen)4(C4O4)](CF3SO3)2 · 3H2O (n=2) and [Cu2(bipy)4(C4O4)](CF3SO3)2 · 6H2O (n=3)

Abstract Two dinuclear copper(II) complexes of the formula [Cu2(phen)4(C4O4)](CF3SO3)2 · 3H2O (1) and [Cu2(bipy)4(C4O4)](CF3SO3)2 · 6H2O (2) [phen=1,10-phenanthroline, bipy=2,2′-bipyridine and C4O4 2−=dianion of 3,4-dihydroxy-3-cyclobuten-1,2-dione (squaric acid)] have been synthesized and characterized by single-crystal X-ray diffraction. Their structures consist of [Cu2(phen)4(C4O4)]2+ (1) and [Cu2(bipy)4(C4O4)]2+ (2) dinuclear copper(II) cations, uncoordinated CF3SO3 − anions and crystallization water molecules. The copper is in a distorted square pyramidal environment: one squarate-oxygen atom and three phen- (1) or bipy- (2) nitrogen atoms of two phen (1) or bipy (2) terminal ligands f…

Solid state polymerization causing transition to a ferromagnetic state. Crystal structures and magnetic properties of [Cu2(dpp)(H2O)(dmso)Cl4]·dmso and [Cu2(dpp)Cl4]n (dpp = 2,3-bis(2-pyridyl)pyrazine)

The preparation, crystal structures and variable-temperature magnetic susceptibility data for [Cu2(dpp)(H2O)(dmso)Cl4]·dmso (1a) and [Cu2(dpp)Cl4]n (2) (dpp = 2,3-bis(2-pyridyl)pyrazine, dmso = dimethyl sulfoxide) are reported. 1a consists of dinuclear dpp-bridged molecules with chlorine, water and dmso serving as terminal ligands. The two copper atoms are crystallographically independent, with distorted square pyramidal and trigonal bipyramidal coordination geometries, respectively. In a first approximation 2 may be described as a chain compound with out-of-plane mono-μ-chloro bridges (Cu–Cl–Cu–Cl). Only one of the crystallographically independent copper atoms participates in this chain fo…

Novel chiral three-dimensional iron(III) compound exhibiting magnetic ordering at T(c) = 40 K.

The preparation and crystal structure determination of the iron(III) compound of formula [(NH(4))(2)[Fe(2)O(ox)(2)Cl(2)].2H(2)O](n) (1) (ox = oxalate dianion) are reported here. Complex 1 crystallizes in the orthorhombic system, space group Fdd2, with a = 14.956(7) A, b = 23.671(9) A, c = 9.026(4) A, and Z = 8. The structure of complex 1 consists of the chiral anionic three-dimensional network [Fe(2)O(ox)(2)Cl(2)](2-) where the iron(III) ions are connected by single oxo and bisbidentate oxalato groups. The metal-metal separations through these bridging ligands are 3.384(2) and 5.496(2) A, respectively. Ammonium cations and crystallization water molecules are located in the helical pseudohex…

Magnetic properties and molecular structures of binuclear (2-pyrazinecarboxylate)-bridged complexes containing Re(iv) and M(ii) (M = Co, Ni)

Three novel Re(iv) compounds, the mononuclear complex Bu(4)N[ReBr(5)(Hpyzc)] (1) and the heterobimetallic complexes [ReBr(5)(mu-pyzc)M(dmphen)(2)].2CH(3)CN [M = Co (2), Ni (3)] (Hpyzc = 2-pyrazinecarboxylic acid, dmphen = 2,9-dimethyl-1,10-phenanthroline), have been synthesized and their crystal structures determined by single-crystal X-ray diffraction. The structure of 1 consists of [ReBr(5)(Hpyzc)](-) complex anions and tetrabutylammonium cations, Bu(4)N(+). The Re(iv) is surrounded by five bromide anions and a N-donor Hpyzc monodentate ligand, in a distorted octahedral environment. The structures of 2 and 3 consist of dinuclear units [ReBr(5)(mu-pyzc)M(dmphen)(2)], with the metal ions li…

The azido ligand: a useful tool in designing chain compounds exhibiting alternating ferro- and antiferro-magnetic interactions

A one-pot reaction of NiII 1, CoII 2, FeII 3 and MnII 4 with 2,2A-bipyridine (bipy) and azide in water leads to [M(bipy)(N3)2]n chains where the metal ion is alternatively bridged by double end-on (EO) and end-to-end (EE) azido bridges; theoretical analysis of the variable-temperature magnetic susceptibility data of 1 and 4 reveals the occurrence of intrachain alternating ferro- (through EO) and antiferro-magnetic (through EE) interactions. Julve Olcina, Miguel, Miguel.Julve@uv.es ; Lloret Pastor, Francisco, Francisco.Lloret@uv.es ; Clemente Juan, Juan Modesto, Juan.M.Clemente@uv.es

Ligand effects on the dimensionality of oxamato-bridged mixed-metal open-framework magnets

Increasing dimensionality [from 2D (1) to 3D (2)] and T(C) [from 10 (1) to 20 K (2)] in two new oxamato-bridged heterobimetallic Mn(II)(2)Cu(II)(3) open-frameworks result from the steric hindrance provided by the different alkyl substituents of the N-phenyloxamate bridging ligands.

Synthetically persistent, self assembled [V(IV)2V(V)4] polyoxovanadates: facile synthesis, structure and magnetic analysis.

Slow diffusion in a H-tube at room temperature of a methanolic solution of [VO(acac)(2)] (Hacac = acetylacetone) and 1,10-phenanthroline (phen) or 2,2'-bipyridine (bipy) into an aqueous solution of sodium pyrophosphate (Na(4)P(2)O(7)) resulted in the serendipitous formation of X-ray quality crystals of mixed-valent, hexameric oxovanadates of general formula [V(6)O(12)(OCH(3))(4)(L)(4)]·solv [L = 1,10-phenanthroline (phen) for 1· 2CH(3)OH · 4H(2)O (1a), and 2,2'-bipyridine (bipy) for 2· 4H(2)O (2a)]. These were characterized by single-crystal X-ray diffraction, IR, elemental and thermogravimetric analysis (TGA). A facile, rationalized synthetic route for the isolation of 1a and 2a could be e…

Two-Dimensional Coordination Polymers Constructed by [NiIILnIII] Nodes and [WIV(bpy)(CN)6]2– Spacers: A Network of [NiIIDyIII] Single Molecule Magnets

Three isomorphous two-dimensional (2D) coordination polymers of general formula {[Ni(II)(valpn)Ln(III)(NO3)(H2O)(μ-NC)4W(IV)(bipy)(CN)2]·xH2O·yCH3CN}n have been synthesized by reacting Ph4P[W(V)(CN)6(bipy)] with the heterodinuclear [Ni(II)Ln(III)(valpn)(O2NO)3] complexes [H2valpn = 1,3-propanediyl-bis(2-iminomethylene-6-methoxyphenol), bipy = 2,2'-bipyridine, and Ln = Gd (1), Dy (2), and Tb (3) with x = 2 (1), 3.9 (2), and 3.35 (3) and y = 2.50 (1), 2 (2), and 1.8 (3)]. Their crystal structures consist of [Ni(II)Ln(III)] 3d-4f nodes which are connected by [W(IV)(bipy)(CN)6](2-) diamagnetic linkers resulting from the reduction of W(V) to W(IV) during the reaction process. The Ni(II) and Ln(I…

Ferro- and Antiferromagnetic Interactions in Oxalato-Centered Inverse Hexanuclear and Chain Copper(II) Complexes with Pyrazole Derivatives.

Two novel copper(II) complexes of formulas {[Cu(4-Hmpz)4][Cu(4-Hmpz)2(µ3-ox-κ2O1,O2:κO2′:κO1′)(ClO4)2]}n (1) and {[Cu(3,4,5-Htmpz)4]2[Cu(3,4,5-Htmpz)2(µ3-ox-κ2O1,O2:κO2′:κO1′)(H2O)(ClO4)]2[Cu2(3,4,5-Htmpz)4(µ-ox-κ2O1,O2:κ2O2′,O1′)]}(ClO4)4·6H2O (2) have been obtained by using 4-methyl-1H-pyrazole (4-Hmpz) and 3,4,5-trimethyl-1H-pyrazole (3,4,5-Htmpz) as terminal ligands and oxalate (ox) as the polyatomic inverse coordination center. The crystal structure of 1 consists of perchlorate counteranions and cationic copper(II) chains with alternating bis(pyrazole)(µ3-κ2O1,O2:κO2′:κO1′-oxalato)copper(II) and tetrakis(pyrazole)copper(II) fragments. The crystal structure of 2 is made up of perchlorat…

Preparation, crystal structure and magnetic properties of di-2-pyridylamine (dpa) copper(II) complexes [Cu(dpa)(N3)2]n and [Cu2(dpa)2(NCO)4]

Abstract The preparation, crystal structures and magnetic properties of two copper(II) complexes with di-2-pyridylamine (dpa) as end-cap ligand and azide (1) and cyanate (2) as bridging groups, [Cu(dpa)(N3)2]n (1) and [Cu2(dpa)2(NCO)4] (2), are reported. Compound 1 consists of uniform chains of copper(II) ions bridged by single μ-1,1-azido groups whereas that of compound 2 is made up of centrosymmetric dicopper(II) units with double μ-1,1-N-cyanate bridges, the other two cyanate groups acting as terminal ligands. The copper atoms in 1 and 2 are five-coordinated with two nitrogen atoms of a bidentate dpa ligand (1 and 2), one nitrogen atom from a terminally bound azide (1)/cyanate (2) and tw…

Cyanido-bridged {FeIIILnIII} heterobimetallic chains assembled through the [FeIII{HB(pz)3}(CN)3]−complex as metalloligand: synthesis, crystal structure and magnetic properties

A new series of cyanido-bridged {FeIIILnIII} heterobimetallic chains of general formula {[(NC)FeIII{HB(pz)3}(μ-CN)2LnIII(bpdo)(NO3)2(H2O)]·CH3CN}n [HB(pz)3− = hydrotris(pyrazol-1-yl)borate, bpdo = 2,2′-bipyridine-N,N′-dioxide and Ln = Gd (1), Tb (2), Dy (3) and Ho (4)], were obtained by using the low-spin [Fe{HB(pz)3}(CN)3]− complex as a metalloligand towards the preformed [Ln(bdpo)(NO3)2(H2O)]+ species. Single-crystal X-ray diffraction shows that 1–4 are isostructural compounds that crystallize in the monoclinic P21/c space group. Their crystal structure consists of neutral 1D coordination polymers where the [Fe{HB(pz)3}(CN)3]− fragment adopts a bis-monodentate coordination mode, through t…

Rational Synthesis of Chiral Metal-Organic Frameworks from Preformed Rodlike Secondary Building Units.

The lack of rational design methodologies to obtain chiral rod-based MOFs is a current synthetic limitation that hampers further expansion of MOF chemistry. Here we report a metalloligand design strategy consisting of the use, for the first time, of preformed 1D rodlike SBUs (1) for the rational preparation of a chiral 3D MOF (2) exhibiting a rare eta net topology. The encoded chiral information on the enantiopure ligand is efficiently transmitted first to the preformed helical 1D building block and, in a second stage, to the resulting chiral 3D MOF. These results open new routes for the rational design of chiral rod-based MOFs, expanding the scope of these unique porous materials.

Growth of thin films of single-chain magnets on functionalized silicon surfaces

A one-pot strategy for the direct growth of continuous and regular thin films of a neutral oxamato-bridged heterobimetallic chain, synthesized from Co2+ nitrate and the tetramethylammonium salt of the anionic copper(II) complex (Me4N)2[Cu(2,6-Et2pa)2]·6H2O (1) (2,6-Etpa = N-2,6-diethylphenyloxamate) over Si(111) surfaces functionalized with carboxylic acid terminating groups has been developed. Variation of the growth conditions can provide important differences in the morphology of the obtained films when working in H2O at 20 °C. An anisotropic growth of 1-D fibers is observed under stoichiometric conditions (Co2+/1 = 1:1), while an isotropic growth of 3-D particles occurs for an excess of…

Synthesis, crystal structure and magnetic properties of a new [ZnII6DyIII6] dodecanuclear motif

Abstract A new dodecanuclear complex, [{(HL)(L)(dmf)ZnIIDyIII(dmf)(H2O)}6]·3dmf·4.2H2O has been assembled using a supramolecular compartmental ligand (H3L results from the condensation reaction of 3-formylsalicylic acid and hydroxylamine). The six DyIII ions describe an octahedron that is inscribed into the octahedron generated by the zinc(II) ions each DyIII ion from this motif behaving as a single ion magnet.

Spinpolarisierung und Ferromagnetismus in zweidimensionalen CoII-Schichtpolymeren: [Co(L)2(NCS)2] (L = Pyrimidin, Pyrazin)

Wie vorhergesagt antiferro- und ferromagnetisch sind die beiden Schichtpolymere [Co(NCS)2(pyz)2] 1 bzw. [Co(NCS)2(pym)2] 2 (Strukturausschnitt im Bild). Die Verbindungen sowie der einkernige Komplex [Co(NCS)2(pyd)4] 3, der zu Vergleichszwecken synthetisiert wurde, konnten aus Losungen von Co(NCS)2 und Pyrazin (pyz; 1), Pyrimidin (pym; 2) bzw. Pyridazin (pyd; 3) in Methanol erhalten, strukturell charakterisiert und ihre magnetischen Eigenschaften untersucht werden.

Spin crossover in a catenane supramolecular system.

The compound [Fe(tvp)(2)(NCS)(2)] . CH(3)OH, where tvp is 1,2-di-(4-pyridyl)-ethylene, has been synthesized and characterized by x-ray single-crystal diffraction. It consists of two perpendicular, two-dimensional networks organized in parallel stacks of sheets made up of edge-shared [Fe(II)](4) rhombuses. The fully interlocked networks define large square channels in the [001] direction. Variable-temperature magnetic susceptibility measurements and Mossbauer studies reveal that this compound shows low-spin to high-spin crossover behavior in the temperature range from 100 to 250 kelvin. The combined structural and magnetic characterization of this kind of compound is fundamental for the inte…

A novel supramolecular assembly in an iron(III) compound exhibiting magnetic ordering at 70 K

Ethyl-substituted ammonium cation allows the preparation of an unprecedented oxo- and oxalato-bridged supramolecular three-dimensional network. The compound exhibits magnetic ordering with Tc = 70 K due to a weak spin canting. Julve Olcina, Miguel, Miguel.Julve@uv.es ; Lloret Pastor, Francisco, Francisco.Lloret@uv.es

Field-Induced Slow Magnetic Relaxation in a Mononuclear Manganese(III)-Porphyrin Complex

We report on a novel manganese(III)-porphyrin complex with the formula [Mn(III) (TPP)(3,5-Me2 pyNO)2 ]ClO4 ⋅CH3 CN (2; 3,5-Me2 pyNO=3,5-dimethylpyridine N-oxide, H2 TPP=5,10,15,20-tetraphenylporphyrin), in which the Mn(III) ion is six-coordinate with two monodentate 3,5-Me2 pyNO molecules and a tetradentate TPP ligand to build a tetragonally elongated octahedral geometry. The environment in 2 is responsible for the large and negative axial zero-field splitting (D=-3.8 cm(-1) ), low rhombicity (E/|D|=0.04) of the high-spin Mn(III) ion, and, ultimately, for the observation of slow magnetic-relaxation effects (Ea =15.5 cm(-1) at H=1000 G) in this rare example of a manganese-based single-ion ma…

Solution chemistry of N,N'-ethylenebis(salicylideneimine) and its copper(II), nickel(II) and iron(III) complexes

Abstract Potentiometric determination of protonation-deprotonation equilibria of the N,N'-ethylenebis(salicylideneimine) (H2sal2en), the related N-(2-aminoethyl)salicylideneimine, (Hsalen), and their organic fragments, salicylaldehyde (Hsal) and ethylenediamine (en), has been used to study the equilibria involved in the formation of Schiff bases from Hsal, sal− and en and in their complex formation with copper(II), nickel(II) and iron(III) ions in dimethyl sulfoxide (dmso)-water (80:20 wt./wt.) mixture (25 °C and 0.1 mol dm−3 KClO4 ionic strength): en+Hsal⇔Hsalen; en+2Hsal⇔H2sal2en; en+ sal−⇔salen−; en+2sal−⇔sal2en2−; sal−+en+MN+⇔[M(salen)](n−1)+; 2sal−+en+Mn+⇔ [M(sal2en)](n−2)+. In these t…

Field-induced slow magnetic relaxation in pseudooctahedral cobalt(ii) complexes with positive axial and large rhombic anisotropy

The preparation, X-ray crystal structure, spectroscopic and variable-temperature dc and ac magnetic properties of two six-coordinate cobalt(ii) complexes of formula [Co(bim)4(tcm)2] (1) and [Co(bmim)4(tcm)2] (2) (bim = 1-benzylimidazole, bmim = 1-benzyl-2-methylbenzimidazole and tcm- = tricyanomethanide ion) are reported. 1 and 2 crystallize in the monoclinic P21/n and C2/c space groups with the asymmetric units composed of one tcm- ion and half the [Co(bim)4]2+ and [Co(bmim)4]2+ complex cations, respectively. Their cobalt atoms are in compressed (1)/rhombic (2) CoN6 octahedral environments, the axial positions being occupied by monodentate tricyanomethanide anions. The neutral molecules in…

Cyanido-Bridged {LnIIIWV} Heterobinuclear Complexes: Synthesis and Magneto-Structural Study

A new series of cyanido-bridged {LnIIIWV} heterobinuclear complexes of formula [LnIII(pyim)2(i-PrOH)(H2O)2(μ-CN)WV(CN)7]·2H2O [Ln = Gd (1), Tb (2), Dy (3), Ho (4), and Er (5); pyim = 2-(1H-imidazol-2-yl)-pyridine) and i-PrOH = isopropyl alcohol] were synthesized by one-pot reaction between (NH3Bu)3[W(CN)8] and [Ln(pyim)2]2+ complexes (generated in situ by mixing the corresponding LnIII ions and the pyim ligand). Compounds 1–5 are isomorphous and crystallize in the monoclinic system P21/n space group. Their crystal structure consists of binuclear units in which the octacyanotungstate(V) anion coordinates to the corresponding LnIII ion through a single cyanide ligand. The tungsten(V) and lant…

Theoretical Insights into the Ferromagnetic Coupling in Oxalato-Bridged Chromium(III)-Cobalt(II) and Chromium(III)-Manganese(II) Dinuclear Complexes with Aromatic Diimine Ligands

Two novel heterobimetallic complexes of formula [Cr(bpy)(ox)(2)Co(Me(2)phen)(H(2)O)(2)][Cr(bpy)(ox)(2)]·4H(2)O (1) and [Cr(phen)(ox)(2)Mn(phen)(H(2)O)(2)][Cr(phen)(ox)(2)]·H(2)O (2) (bpy = 2,2'-bipyridine, phen = 1,10-phenanthroline, and Me(2)phen = 2,9-dimethyl-1,10-phenanthroline) have been obtained through the "complex-as-ligand/complex-as-metal" strategy by using Ph(4)P[CrL(ox)(2)]·H(2)O (L = bpy and phen) and [ML'(H(2)O)(4)](NO(3))(2) (M = Co and Mn; L' = phen and Me(2)phen) as precursors. The X-ray crystal structures of 1 and 2 consist of bis(oxalato)chromate(III) mononuclear anions, [Cr(III)L(ox)(2)](-), and oxalato-bridged chromium(III)-cobalt(II) and chromium(III)-manganese(II) din…

Spin Crossover in Double Salts Containing Six- and Four-Coordinate Cobalt(II) Ions

The preparation and spectroscopic and structural characterization of three cobalt(II) complexes of formulas [Co(tppz)2](dca)2 (1), [Co(tppz)2][Co(NCS)4]·MeOH (2), and [Co(tppz)2][Co(NCO)4]·2H2O (3) [tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine and dca = dicyanamide] are reported here. Compounds 1–3 have in common the presence of the cationic [Co(tppz)2]2+ entity where each mer-tridentate tppz ligand coordinates to the cobalt(II) ion equatorially through two pyridyl donors and axially via the pyrazine, completing the six-coordination. The electroneutrality is achieved by the organic dca group (1) and the anionic tetrakis(thiocyanato-κN)cobaltate(II) (2) and tetrakis(cyanato-κN)cobaltate(II) (3…

A hybrid catalyst for decontamination of organic pollutants based on a bifunctional dicopper(II) complex anchored over niobium oxyhydroxide

Abstract This article describes the preparation and characterization of a hybrid oxidation catalyst for decontamination of organic pollutants which involves a bifunctional dicopper(II) complex and the niobium(V) oxyhydroxide as the active species, the later one being also a solid support. The pH range for the existence of the active species was determined by potentiometric and UV–vis spectroscopy at 25 °C and 0.15 M NaCl in a H 2 O/EtOH (70:30 v/v) solvent mixture containing copper(II) and the ligand N , N -2,2′-ethylenediphenylenebis(oxamic acid) (H 4 L). As far as the hybrid material is concerned, FTIR, FT-Raman, TEM and SEM images, surface area and TG/DTA analyses showed the occurrence o…

Copper(II)-dipicolinate-mediated clickable azide–alkyne cycloaddition in water as solvent

Copper(II)-dipicolinate complex [CuIIL(H2O)2] (1) (H2L = dipicolinic acid (H2dipic)) was synthesized via oxidation of copper(I) iodide and pyridine-2,6-dicarboxylic acid in water and acetonitrile in the presence of glycine. Complex 1 was characterized by FT-IR and elemental analysis and its structure confirmed by single crystal X-ray analysis. This complex is an efficient precatalyst that mediates azide-alkyne cycloaddition reactions in water at room temperature either in the absence or presence of a reducing agent. Compound 1-mediated azide-alkyne cycloaddition affords alkyl/aryl substituted 1,2,3-triazole heterocycles in a regioselective manner and excellent yields under very mild reactio…

Influence of the pyrazine substituent on the structure and magnetic properties of dicyanamide-bridged cobalt(ii) complexes.

Substituted pyrazines were successfully used to prepare two new coordination polymers of formulas {[Co(dca)2(NH2pyz)2]·H2O}n (1) and [Co3(dca)6(HOpyz)5(H2O)2]n (2) [dca = dicyanamide, NH2pyz = 2-aminopyrazine and HOpyz = 2-hydroxypyrazine] whose structures were determined by single-crystal X-ray crystallography. The structure of 1 consists of a two-dimensional rhombus grid of cobalt(II) ions where the dca ligand adopts the μ1,5 bridging mode with trans-positioned monodentate NH2pyz molecules completing the six-coordination around each metal ion. Compound 2 exhibits a stair-like two-dimensional structure where the intralayer connections are performed by the dca and HOpyz groups exhibiting μ1…

Cyanide-bridged iron(III)-cobalt(II) double zigzag ferromagnetic chains: two new molecular magnetic nanowires.

and opened the perspective of a potential useof 1D magnetic molecular nanowires for information storage.Even though 1D magnetism is a very active area of research,such dynamic behavior was never detected before since it isnot clear how to fulfill experimentally the requirements of aperfect 1D Ising-type chain. This finding prompted us to lookcarefully at 1D systems containing anisotropic elements,suchas cobalt(ii) and low-spin iron(iii) centers that we synthesizedrecently,

Tuning up the Tc in Mn(II)Cu(II) bimetallic planes and design of molecular-based magnets

Abstract A family of related compounds of general formula (PPh4)2Mn2[Cu((L)]3nH2O, where PPh4+ is the tetraphenylphosphonium cation and L stands for ortho-phenylenebis(oxamate) (opba, 1), ortho-phenylene (N′-methyloxamidate) (oxamate) (Meopba, 2) and ortho-phenylenebis (N′-methyloxamidate) (Me2opba, 3), have been synthesized. The X-ray absorption near-edge structure (XANES) and extended X-ray Within absorption fine structure (EXAFS) spectra at both Mn and Cu K-edges for all three compounds, as well as their powder X-ray patterns, are consistent with a layered structure built up of parallel Mn11Cu11 two-dimensional honeycomb networks separated by PPh4+ cations. Within the antonic metallic la…

Chromium(III) complexes with 2-(2′-pyridyl)imidazole: Synthesis, crystal structure and magnetic properties

Abstract The preparation, crystal structure and variable temperature-magnetic investigation of three 2-(2′-pyridyl)imidazole-containing chromium(III) complexes of formula PPh4[Cr(pyim)(C2O4)2]·H2O (1), AsPh4[Cr(pyim)(C2O4)2]·H2O (2) and [Cr2(pyim)2(C2O4)2(OH2)2]·2pyim · 6H2O (3) [pyim = 2-(2′-pyridyl)imidazole, C 2 O 4 2 - = dianion of oxalic acid , PPh 4 + = tetraphenylphosphonium cation and AsPh 4 + = tetraphenylarsonium cation ] are reported herein. The isomorphous compounds are made up of discrete [Cr(pyim)(C2O4)2]− anions, XPh 4 + cations [X = P (1) and As (2)] and uncoordinated water molecules. The chromium environment in 1 and 2 is distorted octahedral with Cr–N and Cr–O bond distanc…

Copper(II) complexes of 1,4,5,8,9,12-hexaazatriphenylene with oxalate, squarate, perchlorate as auxiliary ligands or counter ion

Abstract The crystal structures of [Cu(hat)(H2O)(ox)]·H2O (I), [Cu(hat)(H2O)3(sq)]·3H2O (II) and [Cu(hat)(H2O)2](ClO4)2·4H2O (III) have been determined from X-ray single crystal diffraction data (hat=1,4,5,8,9,12-hexaazatriphenylene, ox=oxalate, sq=squarate=dianion of 3,4-dihydroxy-cyclobut-3-ene-1,2-dione). Compound I crystallises in the triclinic system, space group P 1 with a=6.6626(10), b=9.2001(14), c=12.9954(19) A , α=103.301(15), β=91.414(21), γ=105.523(13)°, Z=2; compound II in the orthorhombic system, space group P212121 with a=6.9274(2), b=8.4327(3), c=34.0577(14) A , Z=4; and compound III in the monoclinic system, space group C2/c with a=22.6652(10), b=9.2220(10), c=16.1400(10) A…

On/Off Photoswitching in a Cyanide-Bridged {Fe2Co2} Magnetic Molecular Square

International audience; A repeatable bidirectional paramagnetic ↔ diamagnetic photomagnetic effect has been observed in the cyanide-bridged Fe-Co square complex {[Fe{B(pz)(4)}(CN)(3)](2)[Co(bik)(2)](2)}(ClO(4))(2)*3H(2)O [B(pz)(4) = tetrapyrazolylborate, bik = bis(1-methylimidazol-2-yl)ketone]. Magnetic measurements and low-temperature single-crystal X-ray diffraction experiments have shown that a complete electron transfer from the diamagnetic Fe(II)-Co(III) state to the paramagnetic Fe(III)-Co(II) metastable state is induced by 808 nm laser light irradiation, whereas the diamagnetic state is recovered in an almost quantitative yield under irradiation at 532 nm.

The crystal structure and magnetic properties of 3-pyridinecarboxylate-bridged Re(ii)M(ii) complexes (M = Cu, Ni, Co and Mn)

The novel Re(II) complex NBu4[Re(NO)Br4(Hnic)] (1) and the heterodinuclear compounds [Re(NO)Br4(μ-nic)Ni(dmphen)2]·½CH3CN (2), [Re(NO)Br4(μ-nic)Co(dmphen)2]·½MeOH (3), [Re(NO)Br4(μ-nic)Mn(dmphen)(H2O)2]·dmphen (4), [Re(NO)Br4(μ-nic)Cu(bipy)2] (5) [Re(NO)Br4(μ-nic)Cu(dmphen)2] (5') (NBu4(+) = tetra-n-butylammonium cation, Hnic = 3-pyridinecarboxylic acid, dmphen = 2,9-dimethyl-1,10-phenanthroline, bipy = 2,2'-bipyridine) have been prepared and the structures of 1-5 determined using single crystal X-ray diffraction. The structure of 1 consists of [Re(NO)Br4(Hnic)](-) anions and NBu4(+) cations. Each Re(II) is six-coordinate with four bromide ligands, a linear nitrosyl group and a nitrogen ato…

An Azide-Bridged Copper(II) Ferromagnetic Chain Compound Exhibiting Metamagnetic Behavior

The one-dimensional chain complex [Cu(2)(mgr;(2)-1,1-N(3))(2)(mgr;(2)-1,3-NO(3))(2)(mgr;(2)-1,3-Me(3)NCH(2)CO(2))(2)](n)() (1) contains three different bridge groups,mgr;(2)-1,1-azide (end-on),mgr;(2)-nitrate, andmgr;(2)-syn,syn-carboxylate, arranged so that the azide and carboxylate groups bridge equatorially and dictate the intrachain magnetic behavior between the copper magnetic orbitals. Variable-temperature magnetic susceptibility studies at low field, and magnetization studies at variable field, reveal dominant intrachain ferromagnetism (J = 26 cm(-)(1)) but also much weaker interchain ferromagnetism (THETAV; = 2.3 K) and antiferromagnetism (J(eff) = -0.18 cm(-)(1)). The structure has…

Unprecedented coexistence of cyano-bridged Mn4(III)Cr(III) and Mn2(III)Cr(III) heterobimetallic complexes in one single crystal.

The penta-[{MnIII(4-MeO-salen)(H2O)(micro-CN)}4CrIII(CN)2]+ and trinuclear [{MnIII(4-MeO-salen)(H2O)(micro-CN)}2CrIII(CN)4](-) units coexist in 1 with weak antiferromagnetic interactions which are overcome by a dc magnetic field of 2.5 T.

A novel octacyanido dicobalt(iii) building block for the construction of heterometallic compounds

The first bimetallic octacyanido complex of CoIII, (PPh4)2[Co2(μ-2,5-dpp)(CN)8] (1), was synthesized and used as a metalloligand with [Mn(MAC)(H2O)2]Cl2·4H2O to give a new {CoIIIMnII} heterometallic chain of formula [MnII(MAC)(μ-NC)2Co2III(μ-2,5-dpp)(CN)6]n·7nH2O (2) (PPh4+ = tetraphenylphosphonium cation; 2,5-dpp = 2,5-bis(2-pyridyl)pyrazine and MAC = 2,13-dimethyl-3,6,9,12,18-pentaazabicyclo-[12.3.1]octadeca-1(18),2,12,14,16-pentaene). Both compounds were characterized by single-crystal X-ray diffraction. Compound 1 contains a diamagnetic 2,5-dpp-bridged dicobalt(III) unit with four peripheral cyanide ligands at each cobalt center achieving a six-coordinate surrounding, the electroneutral…

Mononuclear Fe(III) and tetranuclear [Fe(III)Gd(III)]2 complexes with a Schiff-base ligand derived from the o-vanillin: Synthesis, crystal structures and magnetic properties

The mononuclear high-spin iron(III) complexes [Fe(3-MeOsalpn)Cl(H 2 O)] ( 1 ) and [Fe(3-MeOsalpn)(NCS)(H 2 O)]·0.5CH 3 CN ( 2 ) and the tetranuclear oxo-bridged compound [{Fe(3-MeOsalpn)Gd(NO 3 ) 3 } 2 (μ-O)]·CH 3 CN ( 3 ) [3-MeOsalpn 2−  =  N , N ′-propylenebis(3-methoxysalicylideneiminate)] have been prepared and magneto-structurally characterised. The iron(III) ion in 1 and 2 is six-coordinated in a somewhat distorted octahedral surrounding with the two phenolate-oxygens and two imine-nitrogens from the Schiff-base building the equatorial plane and a water ( 1 and 2 ) and a chloro ( 1 )/thiocyanate-nitrogen ( 2 ) in the axial positions. The neutral mononuclear units of 1 and 2 are assemb…

Synthesis, crystal structure and magnetic properties of the chiral iron(II) chain [Fe(bpym)(NCS)2]n (bpym = 2,2′-bipyrimidine)

Abstract The iron(II) compound of formula [Fe(bpym)(NCS)2]n (bpym = 2,2′-bipyrimidine) has been synthesized and its crystal structure determined by X-ray diffraction methods. It crystallizes in the tetragonal P41 (No. 76) and P43 space groups, a = 8.849(2), c=16.486(3) A , V=1290.9(5) A 3 , Z=4, D c =1.699 g cm −3 , M r =330.2, F(000)=664, λ( Mo K α)=0.71073 A , μ( Mo K α)=14.8 cm −1 and T=295 K. A total of 2449 reflections was collected over the range 3≤2ϑ≤55°; of these, 1657 were unique and 1321 were considered as observed (13σ(I)) and used in the structural analysis. The final R and Rw residuals were 0.027 and 0.026, respectively. The structure is made up of chiral (Δ and Λ enantiomers c…

Building-up host-guest helicate motifs and chains: a magneto-structural study of new field-induced cobalt-based single-ion magnets.

In this work, we present the synthetic pathway, a refined structural description, complete solid-state characterization and the magnetic properties of four new cobalt(II) compounds of formulas [Co(H2O)6][Co2(H2mpba)3]·2H2O·0.5dmso (1), [Co(H2O)6][Co2(H2mpba)3]·3H2O·0.5dpss (2), [Co2(H2mpba)2(H2O)4]n·4nH2O (3), and [Co2(H2mpba)2(CH3OH)2(H2O)2]n·0.5nH2O·2ndpss (4) [dpss = 2,2′-dipyridyldisulfide and H4mpba = 1,3-phenylenebis(oxamic) acid], where 2 and 4 were obtained from [Co(dpss)Cl2] (Pre-I) as the source of cobalt(II). All four compounds are air-stable and were prepared under ambient conditions. 1 and 2 were obtained from a slow diffusion method [cobalt(II) : H2mpba2− molar ratio used 1 : …

A mixed-valence Cu(I)–Cu(II) and metal–metal bond containing coordination polymer obtained from an in situ oxidation reaction route

Abstract A new mixed-valence copper coordination polymer with copper–copper metal bonds in a two-dimensional network was generated from an in situ oxidation reaction route under hydrothermal conditions. The synthesis of this coordination polymer demonstrated that the novel compounds that may not be accessible using the known methods could be synthesized via an oxidation reaction route. The reaction conditions are mild enough to keep the building blocks intact during the oxidation and self-assembly process under hydrothermal conditions.

Sustainable Construction of Heterocyclic 1,2,3-Triazoles by Strict Click [3+2] Cycloaddition Reactions Between Azides and Alkynes on Copper/Carbon in Water

1,4-Disubstituted-1,2,3-triazoles, considered as an important and useful class of heterocycles with potential applications in material science and biology, have been prepared in an efficient and selective manner by copper on carbon-catalyzed [3+2] cycloaddition reactions of azides and alkynes (CuAAC) in water under strict click chemistry conditions. Copper(I) catalysts heterogenized onto commercially activated carbon materials (Cu-CC) and on another carbon material produced from vegetable biomass using Argan nut shells (Cu-CANS) were found to be versatile catalytic sources for sustainable CuAAC. These copper on carbon supports were prepared and fully characterized by using two types of acti…

Cu(II) and Cu(I) complexes with 1,2-dithiosquarate as a ligand; from molecular compounds to supramolecular network structures

Abstract Four new complexes of copper(II) and/or copper(I) with 1,2-dtsq as a ligand have been synthesized and characterized by single crystal X-ray diffraction methods, [CuII(terpy)(1,2-dtsq)] (1), [CuII(dmen)(1,2-dtsq)]n (2), {[CuII(dmen)2][CuI(1,2-dtsq)]2}n·2nH2O(3) and {[CuII(men)2][CuI (1,2-dtsq)]2}n·nH2O (4) (1,2-dtsq = 1,2-dithiosquarate, dianion of 3,4-dimercapto-1-cyclobutene-1,2-dione; dmen = N,N-dimethylethylenediamine; men = N-methylethylenediamine, terpy = 2,2′:6,2″-terpyridine). Compound 1 consists of neutral [CuII(terpy)(1,2-dtsq)] mononuclear units which are held together by O⋯H–C and van der Waals interactions. Compound 2 is built of neutral [CuII(dmen)(1,2-dtsq)] entities …

Study of the complex formation between the [Cu(bpca)]+ secondary building unit and the aromatic N donors 2,3,5,6-tetra(2-pyridyl)pyrazine (tppz) and 1,3-bis(4-pyridyl)propane (bpp)

Two new complexes of the formula [{Cu(bpca)}2(μ-tppz)](NO3)2·5H2O (1) and [Cu(bpca)(H2O)(ClO4)(μ-bpp)Cu(bpca)(H2O)2]ClO4·H2O (2) [tppz = 2,3,5,6-tetra(2-pyridyl)pyrazine and bpp = 1,3-bis(4-pyridyl)propane] have been prepared by the reaction of the [Cu(bpca)]+ [Hbpca = bis(2-pyridylcarbonyl)imide] building block and the tppz and bpp N donors. An unusual coordination mode of the tppz ligand was observed in 1, which functions as a bis(bidentate) ligand to two copper(II) atoms each coordinated to a nitrogen atom of the pyrazine moiety and a pyridyl nitrogen atom. This compound presents a layered structure of alternating anionic (ca. 1.6 A) and cationic (ca. 10 A) slices, providing the opportun…

Molecular Engineering To Control the Magnetic Interaction between Single-Chain Magnets Assembled in a Two-Dimensional Network

International audience; Two two-dimensional (2D) systems having the formula [{Fe-III(dmbpy)(CN)(4)}(2)(CoL)-L-II](n) [L = pyetNO (1), tvpNO (2)] and consisting of single-chain magnets connected through organic ligands (L) have been prepared, and their magnetic properties have been investigated. The overall magnetic behavior depends on the capacity of the organic pillars to transmit long-range magnetic interactions. 1 is the first example of a 2D compound exhibiting double relaxation of the magnetization, whereas 2 behaves as a metamagnet.

A Chiral, Photoluminescent, and Spin-Canted {Cu(I)Re(IV)2}n Branched Chain.

A new heteroleptic 1D Cu(I)-Re(IV) coordination polymer of the formula {Cu(I)Re(IV)Cl4(μ-Cl)(μ-pyz)[Re(IV)Cl4(μ-bpym)]}n·nMeNO2 (1; pyz = pyrazine, bpym = 2,2'-bipyrimidine) has been prepared through the Cu(I)-mediated self-assembly of two different Re(IV) metalloligands, namely, [ReCl5(pyz)](-) and [ReCl4(bpym)]. 1 consists of chiral branched chains with an overall rack-type architecture displaying photoemission and magnetic ordering. These results constitute a first step toward making new multifunctional magnetic materials based on mixed 3d-5d molecular systems.

Synthesis, crystal structure and magnetic properties of a new cyanide-bridged iron(III)–nickel(II) ferromagnetic chain

Abstract The reaction of the iron(III) unit fac-[Fe{HB(pz)3}(CN)3]− [ HB ( pz ) 3 - = hydrotris ( 1 - pyrazolyl ) borate ] as the lithium salt (1) with the nickel(II) complex mer-[Ni(dpt)(H2O)3](ClO4)2 [dpt = dipropylenetriamine] in water affords the heterometallic compound of formula {[FeIII{HB(pz)3}(CN)3]2[NiII(dpt)]}n · 3nH2O (2). The structure of 2 has been determined by X-ray diffraction on single crystals and their magnetic properties have been investigated in the temperature range 1.9–300 K. Compound 2 is a zigzag chain compound with regular alternating bis-monodentate [Fe(1){HB(pz)3}(CN)3]− units and [Ni(dpt)]2+ cations, the six coordination around the nickel atom being achieved by …

[FeIILSCoIIILS]2⇔ [FeIIILSCoIIHS]2 photoinduced conversion in a cyanide-bridged heterobimetallic molecular square

The self-assembly of [Fe(III){B(pz)(4)}(CN)(3)](-) and [Co(II)(bik)(2)(S)(2)](2+) affords the diamagnetic cyanide-bridged [Fe(II)(LS)Co(III)(LS)](2) molecular square which is converted into the corresponding magnetic [Fe(III)(LS)Co(II)(HS)](2) species under light irradiation at relatively low temperatures.

Oxotris(oxalato)niobate(V) as counterion in cobalt(II) spin-crossover systems

Abstract This work is devoted to the investigation of the thermally induced spin-crossover behavior from a high-spin state (HS, S = 3/2) at higher temperatures to a low-spin phase (LS, S = 1/2) at lower temperatures of the six-coordinate cobalt(II) complex in the compound [Co(terpy)2]3[NbO(C2O4)3]2·3CH​3OH·4H2O (2). The crystal structure of 2 together with that of its counterion as tetraphenylarsonium(V) salt (AsPh4)3[NbO(C2O4)3]·9H2O (1) are also included. The spin-crossover process was followed by the thermal variation of the χMT product between 2.0 and 400 K under the warming mode, with the LS configuration being achieved at T ⩽ 200 K and the LS → HS interconversion being incomplete at 4…

Corrosion inhibition performance of a structurally well-defined 1,2,3-triazole derivative on mild steel-hydrochloric acid interface

Abstract In the present work, a new 1,4-disubstituted-1,2,3-triazole product, named 4-[1-(4-methoxy-phenyl)-1H-[1,2,3]triazol-4-ylmethyl]-morpholine (MPTM) was successfully synthesized under click chemistry regime. The structure of the new compound that has a rigid triazole moiety and a flexible morpholine ligand has been characterized using 1H NMR, 13C NMR, HRMS, and FTIR spectroscopy. Its inhibition performance for mild steel in acidic medium 1 M HCl has been studied by utilizing a combination of experimental, spectroscopic and computational methods. The electrochemical characterization was carried out by a gravimetric study, electrochemical impedance spectroscopy (EIS), and potentiodynam…

Selective Gas and Vapor Sorption and Magnetic Sensing by an Isoreticular Mixed-Metal–Organic Framework

A novel isoreticular oxamato-based manganese(II)-copper(II) open metal-organic framework H(2)O@iso1 featuring a pillared square/octagonal layer structure with alternating open and closed octagonal pores has been rationally prepared. The open-framework topology is responsible for a large selectivity in the separation of small gas (CO(2) over CH(4)) and vapor molecules (CH(3)OH over CH(3)CN and CH(3)CH(2)OH). H(2)O@iso1 displays a long-range three-dimensional ferromagnetic ordering with a drastic variation of the critical temperature as a function of the guest molecule [T(C)2.0 K (CO(2)@iso1 and CH(4)@iso1) and T(C) = 6.5 (CH(3)OH@iso1) and 21.0 K (H(2)O@iso1)].

Redox switching of the antiferromagnetic coupling in permethylated dicopper(ii) paracyclophanes

A unique magnetic electroswitching behavior has been observed in an oxamato-based permethylated dicopper(II) paracyclophane; upon reversible one-electron oxidation of the double tetramethyl-substituted p-phenylenediamidate bridging skeleton, the spin alignment of the two Cu(II) ions (S(Cu) = ½) changes from antiparallel (OFF) to parallel (ON) in the resulting dicopper(II) π-radical cation species.

Manganese(II) complexes with croconate and 2-(2-pyridyl)imidazole ligands: Syntheses, X-ray structures and magnetic properties

Abstract The mixed-ligand complexes of manganese(II) of formula [Mn(pyim)2(C5O5)] (1) and [Mn(pyim)(H2O)(C5O5)]n · 2.5nH2O (2) [pyim = 2-(2-pyridyl)imidazole and C 5 O 5 2 -  = croconate (dianion of 4,5-dihydroxy-4-cyclopentene-1,2,3-trione)] have been prepared and their structures determined by X-ray crystallographic methods. Compound 1 is a tris-chelated mononuclear complex where the manganese atom is six-coordinate: four nitrogen atoms from two pyim molecules and two oxygen atoms from a croconate group build a somewhat distorted octahedral surrounding around the metal atom. The resulting neutral mononuclear units are linked to each other through double bridges which are constituted by th…

Three one-dimensional systems with end-to-end dicyanamide bridges between copper(ii) centres: structural and magnetic properties

The preparation, crystal structures and magnetic properties of three different copper(II) chains of formula [Cu(pyim)(H2O)(dca)]n(NO3)n (1), [Cu(dpa)(dca)2]n (2) and [Cu(bpa)(dca)2]n (3) [pyim = 2-(2-pyridyl)imidazole, dca = dicyanamide anion, dpa = 2,2′-dipyridylamine and bpa = 1,2-bis(4-pyridyl)ethane] are reported. A chain structure with single, symmetrical, end-to-end dca bridges is found in compound 1. This bridging mode, with two short, equatorially coordinated Cu–N bonds has not been previously observed in the [Cu(dca)Xn] (X = coligand) family of compounds. The copper atom in 1 has a distorted square pyramidal geometry with a bidentate pyim ligand and two nitrile nitrogen atoms from …

Crystal structure and magnetic properties of the flexible self-assembled two-dimensional square network complex [Cu2(mal)2(H2O)2(4,4′-bpy)] (H2mal=malonic acid and 4,4′-bpy=4,4′-bipyridine)

Abstract The copper(II) complex [Cu 2 (mal) 2 (H 2 O) 2 (4,4′-bpy)] ( 1 ) (H 2 mal=malonic acid and 4,4′-bpy=4,4′-bipyridine) has been prepared and its structure determined by single crystal X-diffraction methods. Compound 1 has a two-dimensional square grid network structure. The square grids are stacked parallel but in a staggered manner on each other along the c -axis, with an interlayer separation of 3.850(1) A. Each layer contains a large cavity of 15.784(1)×15.784(1) A with each edge shared by one malonate group and one 4,4′-bpy ligand and a small planar square of 4.644(1)×4.644(1) A with Cu(II) ions and malonate groups at each corner and side, respectively. Each copper atom is in a d…

Combining Cyanometalates and Coordination Clusters: An Alternative Synthetic Route toward Original Molecular Materials

International audience; With the discovery of molecules or molecule-based compounds that can display blocked magnetization, magnetic ordering or switchable magnetic bistability, the research efforts devoted to molecular magnetic materials have considerably increased over the past two decades, fully exploiting the advantages of the bottom-up approach. 1-4 This research field focuses on promising properties for potential technological applications such as information storage, quantum computing and spintronics at the molecular scale, but it also provides fundamental insights into original quantum phenomena. 5,6 Coordination chemists have developed efficient synthetic tools for the preparation …

Syntheses, crystal structures and magnetic properties of mono- and polynuclear [bis(2-arylcarbonyl)amidate]copper(II) complexes

Abstract Five copper(II) complexes of formulas [Cu(bpcam)(CN)(H2O)] (1), [Cu(bpcam)(N3)(H2O)]2 (2), [Cu(bpcam)(NCS)(H2O)] (3), [Cu(bpcam)(dca)(H2O)]2 (4) and [Cu(bpca)(tcm)]n (5) [bpcam = bis(2-pyrimidylcarbonyl)amidate, bpca = bis(2-pyridylcarbonyl)amidate, dca = dicyanamide and tcm = tricyanomethanide] have been prepared and their structures determined by single crystal X-ray diffraction. Compounds 1 and 3 are mononuclear species where each copper atom is five coordinated with a tridentate bpcam and a terminally bound cyanide (1)/thiocyanate (3) ligands creating a basal plane with a water molecule in the axial position of a distorted square pyramid. Compound 2 is made of neutral di-μ-1,1-…

Dicopper(II) Metallacyclophanes as Multifunctional Magnetic Devices: A Joint Experimental and Computational Study

Metallosupramolecular complexes constitute an important advance in the emerging fields of molecular spintronics and quantum computation and a useful platform in the development of active components of spintronic circuits and quantum computers for applications in information processing and storage. The external control of chemical reactivity (electro- and photochemical) and physical properties (electronic and magnetic) in metallosupramolecular complexes is a current challenge in supramolecular coordination chemistry, which lies at the interface of several other supramolecular disciplines, including electro-, photo-, and magnetochemistry. The specific control of current flow or spin delocaliz…

Magnetism in Heterobimetallic and Heterotrimetallic Chains Based on the Use of [W V (bipy)(CN) 6 ] – as a Metalloligand

Magnetic Properties of a New Hexahalorhenate(IV) Compound and Structural Comparison with Its Hexahaloplatinate(IV) Analog

New alkoxo-bridged mixed-valence cobalt clusters: Synthesis, crystal structures and magnetic properties

Two new Co II /Co III complexes, [{Co II Co III (mea) 3 } 2 (bpe) 3 ](ClO 4 ) 4  · 1.5CH 3 OH · 1.5H 2 O ( 1 ) and [ Co 4 II Co 3 III ( dea ) 6 ( CH 3 COO ) 3 ] ( ClO 4 ) 0.75 ( CH 3 COO ) 1.25 · 0.5 H 2 O ( 2 ) [Hmea = monoethanolamine H 2 dea = diethanolamine and bpe = 1,2-bis(4-pyridyl)ethane], have been obtained by reacting cobalt(II) perchlorate ( 1 and 2 ), Hmea ( 1 )/H 2 dea ( 2 ), bpe ( 1 ) and sodium acetate ( 2 ). The crystal structures of 1 and 2 have been solved by single crystal X-ray diffraction. Crystal 1 contains “Chinese lantern”-like shaped cations, resulting by connecting two {Co II Co III (mea) 3 } moieties with three flexible bpe ligands. The coordination sphere of the …

High-temperature spin crossover in a mononuclear six-coordinate cobalt(II) complex.

The six-coordinate cobalt(II) complex of formula [Co(tppz)2](tcm)2 exhibits a thermally induced spin-crossover behavior from a high spin (S = 3/2) at higher temperatures to a low spin (S = 1/2) at lower temperatures, with the low-spin phase being achieved at T ≤ 200 K.

Synthesis and crystal structure of the low-spin iron(II) complex [Fe(bpz)3](ClO4)2·H2O (bpz=2,2′-bipyrazine)

Abstract The crystal structure of the title compound [Fe(bpz) 3 ](ClO 4 ) 2  · H 2 O (bpz=2,2 ′ -bipyrazine) has been determined by a single crystal X-ray diffraction study at 293(2) K. The complex is monoclinic, P 2 1 / c , a =17.263(3), b =9.983(2), c =17.921(4) A, β =107.94(3)°, V =2938.3(10) A 3 , Z =4, R =0.073 and R w =0.118. The structure is made up of tris-chelated [Fe(bpz) 3 ] 2+ cations, uncoordinated perchlorate anions and crystallization water molecules. The iron atom exhibits a FeN 6 distorted octahedral geometry with average Fe–N bond length and N–Fe–N bidentate angle of 1.962(5) A and 81.6(2)°. The value of the Fe–N bond distance and that of the room temperature magnetic mome…

Synthesis, crystal structure and magnetic properties of a cyanide-bridged heterometallic {CoIIMnIII} chain

The assembly reaction between the low-spin [CoII(dmphen)(CN)3]- metalloligand and the [MnIII(salen)(H2O)]+ complex cation yielded the one-dimensional compound {[MnIII(salen)(μ-NC)2CoII(dmphen)(CN)]·2H2O}n (1), which behaves as a ferrimagnetic chain, the intrachain magnetic coupling being J = -1.71(1) cm-1.

Solution and solid state studies with the bis-oxalato building block [Cr(pyim)(C2O4)2]− [pyim = 2-(2′-pyridyl)imidazole]

The preparation, X-ray structure, and variable temperature magnetic study of the new compound {Ba(H2O)3/2[Cr(pyim)(C2O4)2]2}n·9/2nH2O (1) [pyim = 2-(2′-pyridyl)imidazole and C2O42− = dianion of oxalic acid], together with the potentiometric and spectrophotometric studies of the protonation/deprotonation equilibria of the pyim ligand and the ternary complex [Cr(pyim)(C2O4)2]−, are reported herein. The crystal structure of 1 consists of neutral chains, with diamond-shaped units sharing barium(II), with the two other corners occupied by chromium(III). The two metal centers are connected through bis(bidentate) oxalate. Very weak antiferromagnetic interactions between the chromium(III) ions occu…

Synthesis, characterization and X-ray structure of glycosyl-1,2-isoxazoles and glycosyl-1,2-isoxazolines prepared via 1,3-dipolar cycloaddition

Abstract A convenient preparative method of a series of glycosyl-1,2-isoxazoles ( 6–11 ) and glycosyl-1,2-isoxazolines ( 15–20 ) by a simple and efficient 1,3-dipolar cycloaddition of a series of aryl nitrile oxide, generated in situ from aryl oximes ( 4–5 ), with a variety of O -propargyl glycosyles ( 1 – 3 ) or O -allyl glycosyles ( 12–14 ) respectively, is reported. The carbohydrate-containing 1,2-isoxazoles and 1,2-isoxazolines compounds were isolated in excellent yields (81–91%) and they were fully characterized by 1 H, 13 C NMR and mass spectrometry. The relative stereochemistry of the glycosyl-1,2-isoxazole 10 was confirmed by single crystal X-ray analysis. The molecular structure of…

A cyanide and hydroxo-bridged nanocage: a new generation of coordination clusters.

International audience; Combining serendipitously-formed hydroxo-clusters, [CoII3(OH)(piv)4(L)]+ (where L = MeCN or Hpiv), with assembling cyanide building block, [FeIII(Tp)(CN)3]−, has led to an unprecedented architecture where polymetallic cobalt clusters and blocked tris-cyanide iron complexes define the apexes of a unique magnetic cubic nanocage.

Spin Polarization and Ferromagnetism in Two-Dimensional Sheetlike Cobalt(II) Polymers: [Co(L)2(NCS)2] (L=Pyrimidine or Pyrazine)

Potentiometric study of the formation of hydroxo complexes of [Cu(terpy)]2+. Synthesis and crystal structure of [Cu(terpy) (H2O)](CF3SO3)2

Two complexes of formula [Cu(terpy)(H2O)](CF3SO3)2 (1) and [Cu(terpy)(OH)]BPh4 (2) (terpy=2,2′∶6′,2″-terpyridine and BPh4=tetraphenylborate anion) have been synthesized and characterized by spectroscopic techniques. The x-ray crystal structure of (1) has been determined by x-ray diffraction. The structure is made up of [Cu(terpy)(H2O)]2+ mononuclear cations plus semi-coordinated CF3SO3 − anions. The coordination geometry around the copper atom is approximately elongated tetragonal octahedral. The oxygen atom of water and the three nitrogen atoms of terpy occupy the equatorial sites whereas the apical ones are filled by trifluoromethanesulphonate oxygen atoms. The formation of hydroxo comple…

Dicopper(II) metallacyclophanes with photoswitchable oligoacene spacers: a joint experimental and computational study on molecular magnetic photoswitches

Dinuclear copper(II) complexes of the metallacyclophane-type, (nBu4N)4[Cu2(2,6-anba)2] (1) and (nBu4N)4[Cu2(1,5-naba)2]·4H2O (2) with photoactive 2,6-anthracene-(2,6-anba) and 1,5-naphthalenebis(oxamate) (1,5-naba) bridging ligands, are reported. They undergo a thermally reversible, solid-state photomagnetic (ON/OFF) switching between the moderately strong antiferromagnetically coupled dicopper(II) species and the corresponding magnetically uncoupled [4+4] photocycloaddition product. Density functional calculations give further insights on the intramolecular (“pseudo-bimolecular”) photocycloaddition reaction of the two facing 2,6-anthracene or 1,5-naphthalene spacers in this novel family of…

Synthesis, crystal structure and magnetic characterization of a series of CuII-LnIII heterometallic [Ln = La, Ce, Pr, Nd and Sm) metal-organic compounds with an unusual single crystal to single crystal phase transition

The synthesis and structural characterization of five Cu(II)-Ln(III) heteronuclear metal-organic frameworks of formula {[Ln4Cu 4(H2O)26(bta)5]·mH 2O}n and {[Ln4Cu4(H 2O)24(bta)5]·pH2O} n [Ln = LaIII (1A/1B), CeIII (2A/2B), Pr III (3A/3B), NdIII (4A/4B) and SmIII (5A/5B) with m/p = 20 (1A)/16 (1B), 18 (2A)/16 (2B), 14 (3A)/16 (3B), 22 (4A)/16 (4B) and 21 (5A)/14 (5B); H4bta =1,2,4,5-benzenetetracarboxylic acid (1-5)] have been performed. These compounds present a single-crystal to single-crystal phase transition from expanded A phases toward the B shrinking networks, which is triggered only in the presence of a dry environment. This phase transition is accompanied by a compression of the cry…

Hydrogen-bonded 2-(2-pyridyl)imidazole (pyim) manganese(II) complexes as building blocks for molecular assembling: Syntheses and structural characterization of cis-[Mn(pyim)2X2] compounds (X=, NCO− and NCS−)

Abstract The preparation and crystal structures of three new manganese(II) complexes with 2-(2-pyridyl)imidazole (pyim) and pseudohalides as ligands, cis-[Mn(pyim)2(N3)2] (1), cis-[Mn(pyim)2(NCO)2] (2) and cis-[Mn(pyim)2(NCS)2] (3), are reported. The structural building block in each structure is a mononuclear, neutral complex unit. The metal ion in each case adopts a distorted octahedral coordination geometry with the two pseudohalide ligands in cis positions. The main differences between the molecular structures of the three compounds are associated with the orientation of the anionic ligands. Hydrogen bonds between imidazole N–H and the metal-coordinated nitrogen atom of the pseudohalide…

Synthesis, characterization and crystal structure of 2-dicyanomethylene-1,3-bis(ferrocenylmethyl)-1,3-diazolidine

By reaction of N,N′-ethylenebis(ferrocenylmethylamine)1 with tetracyanoethylene in dichloromethane the yellow compound 2-dicyanomethylene-1,3-bis(ferrocenylmethyl)-1,3-diazolidine 2 can be isolated. The single-crystal structure of 2 has been determined. It crystallizes in the non-centrosymmetric trigonal space group P3221, a= 12.255(2), c= 13.831(7)A, Z= 3. Refinement of the atomic parameters by least-squares techniques gave a final R factor of 0.038 (R′= 0.034) for 1782 observed reflections having I > 2.5δ(I). Anomalous values of the bond distances and the vinyl carbon chemical shift in the 13C NMR spectrum of 2 are explained on the basis of a polarization due to a combination of the elect…

Synthesis, crystal structure and magnetic properties of [Cu(bpym)(mal)(H2O)]·6H2O and [Cu2(bpym)(mal)2(H2O)2]·4H2O (bpym=2,2′-bipyrimidine, H2mal=malonic acid)

Abstract Two new mixed-ligand complexes of formula [Cu(bpym)(mal)(H2O)]·6H2O (1) and [Cu2(bpym)(mal)2(H2O)2]·4H2O (2) (bpym=2,2′-bipyrimidine and H2mal=malonic acid) have been synthesised and characterised by X-ray diffraction methods. The crystal structure of 1 consists of mononuclear [Cu(bpym)(mal)(H2O)] units in which the copper atom shows a slightly distorted square-pyramidal environment with two bpym-nitrogen and two malonate-oxygen atoms forming the equatorial plane and a water molecule in the axial position. The structure of 2 is built by centrosymmetric bpym-bridged dinuclear [Cu2(bpym)(mal)2(H2O)2] units, in which the geometry of each Cu(II) ion is similar to that found in 1. Malon…

Synthesis, crystal structure and magnetic properties of the cyclic tetranuclear compound [Cu4(pz)4(hppa)2(H2O)4] [pz = pyrazolate; hppa = R,S-2-hydroxo-2-phenyl-2-(1-pyrazolyl)acetate]

Abstract The synthesis, X-ray structure and magnetic properties of the neutral tetranuclear copper(II) complex of formula [Cu4(pz)4(hppa)2(H2O)4] (1) [Hpz = pyrazole and hppa = R,S-2-hydroxo-2-phenyl-2-(1-pyrazolyl)acetate] are reported. Remarkably, the structure of 1 reveals the presence of the S- and R-forms of the new hppa ligand which is formed in situ in the complex reaction between copper(II), pyrazole and phenylmalonate in water:methanol solvent mixture under ambient conditions. The two crystallographically independent copper(II) ions [Cu(1)/Cu(2)] are five-coordinate in square pyramidal surroundings. Three nitrogen atoms, from two pz groups and one hppa ligand and one oxygen atom of…

Synthese, Struktur und magnetische Eigenschaften eines achtkernigen Nickel(II)-Komplexes mit einer zentralenhexahedro-Ni8-Einheit

Self-Assembly of the Hexabromorhenate(IV) Anion with Protonated Benzotriazoles: X-ray Structure and Magnetic Properties

Two novel ReIV compounds of formulas [HBTA]2[ReIVBr6] (1) and [HMEBTA]2[ReIVBr6] (2) [BTA = 1H-benzotriazole and MEBTA = 1-(methoxymethyl)-1H-benzotriazole] have been synthesized and magneto-structurally characterized. 1 and 2 crystallize in the triclinic system with space group P1̅. In both compounds, the rhenium ion is six-coordinate, bonded to six bromo ligands in a regular octahedral geometry. Short ReIV–Br···Br–ReIV contacts, π–π stacking, and H-bonding interactions occur in the crystal lattice of both 1 and 2, generating novel supramolecular structures based on the ReIV. The different dispositions of the cations and the intermolecular Br···Br contacts in 1 and 2 play an important stru…

Oxotris(oxalate)niobate(V): An oxalate delivery agent in the design of building blocks

This work concerns the oxalate delivery process that occurs when using (NH4)3[NbO(C2O4)3]·6H2O as a suitable oxalate source in the synthesis of two compounds, [Cu(dmphen)(C2O4)(H2O)] (1) and [{Cu(dmphen)(CH3OH)}2(μ-C2O4)](ClO4)2 (2) (dmphen = 2,9-dimethyl-1,10-phenanthroline). {[Fe{HB(pz)3}(CN)2(μ-CN)]2[{Cu(dmphen)}2(μ-C2O4)]}∙xCH3OH (3) (2.0 ≤ x ≤ 2.4) was obtained by reacting 2 and PPh4[Fe{HB(pz)3}(CN)3]∙H2O [ = tetraphenylphosphonium and = tris(pyrazolyl)borate]. Crystal structures of 1–3 have been determined by single-crystal X-ray diffraction experiments: 1 is a mononuclear trigonal bipyramidal copper(II) species, 2 is a centrosymmetric oxalato-bridged dicopper(II) complex, and 3 consi…

Solid-state dinuclear-to-trinuclear conversion in an oxalato-bridged chromium(III)-cobalt(II) complex as a new route toward single-molecule magnets.

A novel bis(oxalato)chromium(III) salt of a ferromagnetically coupled, oxalato-bridged dinuclear chromium(III)-cobalt(II) complex of formula [CrL(ox)(2)CoL'(H(2)O)(2)][CrL(ox)(2)]·4H(2)O (1) has been self-assembled in solution using different aromatic α,α'-diimines as blocking ligands, such as 2,2'-bipyridine (L = bpy) and 2,9-dimethyl-1,10-phenanthroline (L' = Me(2)phen). Thermal dehydration of 1 leads to an intriguing solid-state reaction between the S = 3/2 Cr(III) anions and the S = 3 Cr(III)Co(II) cations to give a ferromagnetically coupled, oxalato-bridged trinuclear chromium(III)-cobalt(II) complex of formula {[CrL(ox)(2)](2)CoL'} (2). Complex 2 possesses a moderately anisotropic S =…

Solvent effects on the dimensionality of oxamato-bridged manganese(II) compounds

Two new oxamate-containing manganese(II) complexes, [{Mn(H2edpba)(H2O)2}2]n (1) and [Mn(H2edpba)(dmso)2]∙dmso∙CH3COCH3∙H2O (2) (H4edpba = N,N′-ethylenediphenylenebis(oxamic acid) and dmso = dimethylsulfoxide), have been synthesized and the structures of 1 and 2 were characterized by single crystal X-ray diffraction. The structure of 1 consists of neutral honeycomb networks in which each manganese(II) is six-coordinate by one H2edpba2− ligand and two carboxylate–oxygens from two other H2edpba2− ligands building the equatorial plane. Each manganese is connected to its nearest neighbor through two carboxylate(monoprotonated oxamate) bridges in an anti-syn conformation. A dmso solution of singl…

In situ generation of Ph3PO in cyanido-bridged heterometallic {FeIIILnIII}2 molecular squares (Ln = Eu, Sm)

Two new examples of cyanido-bridged {FeIIILnIII}2 molecular squares, with pyim and PPh3O as capping ligands at the LnIII sites, exhibit weak antiferromagnetic interactions [Ln = Eu (1), Sm (2), pyim = 2-(1H-imidazol-2-yl)pyridine, PPh3PO = triphenylphosphine oxide].

Electroswitching of the single-molecule magnet behaviour in an octahedral spin crossover cobalt(ii) complex with a redox-active pyridinediimine ligand

Thermal-assisted spin crossover and field-induced slow magnetic relaxation coexist in the solid state for the mononuclear cobalt(II) complex with the non-innocent 2,6-bis(N-4-methoxyphenylformimidoyl)pyridine ligand. One-electron oxidation of the paramagnetic low-spin CoII ion (SCo = 1/2) to the diamagnetic low-spin CoIII ion (SCo = 0) leads to the electroswitching of the slow magnetic relaxation in acetonitrile solution.

An {Fe60} tetrahedral cage: building nanoscopic molecular assemblies through cyanometallate and alkoxo linkers

International audience; A nanoscopic {Fe60} coordination cage (approximately 3 nm) was prepared by the self assembly of a partially blocked tricyanidoferrate(III) complex and tris(alkoxo)-based iron(III) coordination motifs. This cage is a rare example of a mixed cyanido/alkoxo-bridged high nuclearity complex and it exemplifies the great potential of this new synthetic route to generate uncommon molecular architectures using cyanometallates as metalloligands versus alkoxo-based polynuclear entities.

Oxamidato complexes. Part 4. Electrochemical study of the copper(III)/copper(II) couple in monomeric N,N?-bis(substituent)oxamidatocopper(II) complexes

The electrochemical behaviour of a series of monomeric N,N′-bis(substituent)oxamidato copper(II) complexes of formula Na2[Cu(3,5,3′,5′-X4obbz)]·4H2O [X = Cl (1), Br (2), I (3) and obbz = oxamidobis(benzoato)], Na2-[Cu(obbz)]·4H2O (4), Na2[Cu(5,5′-Me2obbz)]·4H2O (5), Na2[Cu(4,5,4,5′-(MeO)4obbz)]·4H2O(6),Na2[Cu(obp)]· 3.5H2O (7) (obp = oxamidobis(propionato)) and Na2[Cu(pba)]·6H2O (8), [pba = propylenebis(oxamate)] has been investigated by cyclic voltammetry, rotating disk electrode and coulometry in water and dimethylsulphoxide (dmso) solutions. NaNO3 (0.1 M) and n-Bu4NPF6 (0.1 M) were used as supporting electrolytes in H2O and dmso respectively, all solutions being thermostatted at 25 °C. I…

[MIII(bpym)(CN)4]−: a suitable building block to design ferrimagnetic cyano-bridged heterobimetallic chains (M = Fe, Cr; bpym = 2,2′-bypyrimidine)

Two cyano-bridged M(III)Mn(III) [M = Fe () and Cr ()] ferrimagnetic chains are reported; exhibits metamagnetism with two critical fields of 1250 G and 2.0 T which correspond to the overcoming by the applied dc field of the inter- and intrachain magnetic interactions, respectively.

The Cation as a Tool to Get Spin-Canted Three-Dimensional Iron(III) Networks

Alkyl-substituted ammonium cations (X) allow the preparation of a series of spin-canted oxo- and oxalato-bridged three-dimensional iron(III) networks, exhibiting magnetic ordering at T(c) values ranging from 40 to 56 K. The value of T(c) varies with the cation despite the lack of significant structural modifications.

A new ferromagnetically coupled μ-alkoxo–μ-acetato copper(II) trinuclear complex: [Cu3(H2tea)(Htea)(CH3COO)2](ClO4) (H3tea=triethanolamine)

Abstract A μ-alkoxo–μ-acetato trinuclear copper(II) complex, [Cu3(H2tea)(Htea)(CH3COO)2](ClO4) 1, has been synthesized by reacting copper(II) perchlorate, triethanolamine and sodium acetate. The unit cell contains two centrosymmetric, crystallographically independent trinuclear Cu(II) complexes and two ClO 4 - ions. The crystallographically independent trinuclear Cu(II) complexes differ mainly in some of their geometry parameters. The coordination environment of the central copper atom is square-planar, in one trinuclear entity, and elongated octahedral in the other one (in this last case, the coordination number of the central copper atom increases through the semicoordination of an oxygen…

Influence of the coligand in the magnetic properties of a series of copper(ii)–phenylmalonate complexes

This work presents a series of layered systems based on phenylmalonate-containing copper(II) complexes and different coligands. Eight compounds [Cu(L)(Phmal)]n where L = pyrimidine (pym, 1) pyrazine (pyz, 2), 3-cyanopyridine (3-CNpy, 3), 4-cyanopyridine (4-CNpy, 4), 3-fluoropyridine (3-Fpy, 5), 3-chloropyridine (3-Clpy, 6), 3-bromopyridine (3-Brpy, 7) and 3-iodopyridine (3-Ipy, 8), have been synthesized and magneto-structurally characterized. The coligands selected not only modify the coordination environment of the metal ion, blocking or extending the polymerization, but also interact with the phenyl ring of the phenylmalonate ligand and dramatically affect the crystal packing through weak…

Molecular magnetism, quo vadis? A historical perspective from a coordination chemist viewpoint☆

Abstract Molecular magnetism has travelled a long way from the pioneering studies on electron exchange and double exchange or spin crossover and valence tautomerism in small oligonuclear complexes, from mono- to di- and tetranuclear species, to the current investigations about magnetic anisotropy and spin dynamics or quantum coherence of simple mono- or large polynuclear complexes, behaving as switchable bistable molecular nanomagnets for potential applications in information data storage and processing. In this review, we focus on the origin and development of the research in the field of molecular magnetism from a coordination chemistry viewpoint, which dates back to the establishment of …

Synthesis, spectroscopic and structural characterization of [Cu(phen)(C5O5)(H2O)]·H2O, [Ni(terpy)(C5O5)(H2O)]·H2O and [Ni(terpy)2](NO3)2·0.5H2O

Abstract The new mononuclear complexes [Cu(phen)(C5O5)(H2O)]·H2O (1), [Ni(terpy)(C5O5)(H2O)]·H2O (2) and [Ni(terpy)2](NO3)2·0.5H2O (3) [phen=1,10-phenanthroline, C 5 O 5 2 − =dianion of the 4,5-dihydroxycyclopent-4-ene-1,2,3-trione and terpy=2,2′:6′,2″-terpyridine] have been synthesized and characterized by single-crystal X-ray diffraction. The copper atom of 1 has a distorted square pyramidal environment with two phen-nitrogen and two croconate-oxygen atoms building the equatorial plane and a water molecule in the apical position. The nickel atom of 2 exhibits a distorted NiN3O3 octahedral coordination, which may be described either as tetragonally compressed or as skewed trapezoidal bipyr…

An original 3D coordination polymer constructed from trinuclear nodes and tetracarboxylato spacers

A novel 3D coordination polymer, ∞3[{Cu3(felden)}4(btec)3]·17H2O, has been assembled using cationic trigonal nodes, [CuII3(felden)]3+, generated by a tricompartmental ligand, H3felden, which results from the Schiff condensation reaction between 2,4,6-triformylphloroglucinol and N,N-dimethylethylenediamine. The tetraanion of the 1,2,4,5-benzenetetracaboxylic acid (H4btec) was employed as a spacer. The structure of 1 shows large icosahedral cavities and channels and the magnetic interaction between the copper(II) ions within the triangles is weak and antiferromagnetic.

Study of the interaction of [Cu(bipy)]2+ with oxalate and squarate in aqueous solution

A study of the formation of complexes between [Cu(bipy)]2+ and ox2− and sq2− in aqueous solution, (bipy being 2,2′-bipyridine and ox2− and sq2− the dianions of ethanedioic acid and 3,4-dihydroxy-3-cyclobutene-1,2-dione, respectively), has been carried out with the aim of comparing the coordinating properties of these related ligands. The constants of the equilibria (i) and (ii) $$[Cu(bipy)]^{2 + } + ox^{2 - } \rightleftharpoons [Cu(bipy)ox]$$ (i) $$[Cu(bipy)]^{2 + } + sq^{2 - } \rightleftharpoons [Cu(bipy)sq]$$ (ii) have been determined by potentiometry and spectrophotometry at 25.0°C and 0.1 M NaNO3:logβ=5.78(2) and 2.16(2) for the oxalato- and squarato-complex, respectively. Such differen…

Cubane-Type CuII4 and MnII2MnIII2 Complexes Based on Pyridoxine: A Versatile Ligand for Metal Assembling

By using Vitamin B6 in its monodeprotonated pyridoxine form (PN-H) [PN = 3-hydroxy-4,5-bis(hydroxymethyl)-2-methylpyridine], two tetranuclear compounds of formula [Mn4(PN-H)4(CH3CO2)3Cl2]Cl·2CH3OH·2H2O (1) and [Cu4(PN-H)4Cl2(H2O)2]Cl2 (2) have been synthesized and magneto-structurally characterized. 1 crystallizes in the triclinic system with space group P1 whereas 2 crystallizes in the orthorhombic system with Fdd2 as space group. They exhibit Mn(II)2Mn(III)2 (1) and Cu(II)4 (2) cubane cores containing four monodeprotonated pyridoxine groups simultaneously acting as chelating and bridging ligands (1 and 2), three bridging acetate ligands in the syn-syn conformation (1), and two terminally …

Tuning the Spin Ground State in Heterononanuclear Nickel(II)−Copper(II) Cylinders with a Triangular Metallacyclophane Core

3 páginas, 2 figuras, 1 gráfico.-- et al.

Ferromagnetic Coupling Through the End-to-End Thiocyanate Bridge in Cobalt(II) and Nickel(II) Chains

The preparation, spectroscopic characterization, and X-ray crystal structure of two novel one-dimensional compounds of formula [MII(tppz)(NCS)(μ-1,3-NCS)]n [tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine and M = Co(1) and Ni (2)] are reported. 1 and 2 are isomorphous compounds, and they crystallize in the P21/n space group. Their structures are made up of zigzag chains of cobalt(II) (1) and nickel(II) ions (2) bridged by single end-to-end thiocyanate groups with a tridentate tppz molecule and a terminally bound thiocyanate-N ligand achieving distorted MN5S octahedral surroundings around each metal center. The main source of the distortion of the ideal octahedron is due to the geometrical constr…

A tribute to Professor Juan Faus Payá

International audience; Pas de résumé

Solvent-driven dimensionality control in molecular systems containing CuII, 2,2′-bipyridine and an oxamato-based ligand

A discrete dicopper(II) system, [Cu(bipy)(H2mpba)]2·2H2O (1), and its isomeric chain, [Cu(bipy)(H2mpba)]·dmso (2) [bipy = 2,2′-bipyridine and H4mpba = N,N′-1,3-phenylenebis(oxamic acid)], were obtained by modifying the ratio of the H2O–dmso solvent mixture, and their interconversion was also monitored by changing the solvents during the synthesis. The solvents play an essential role in the formation and crystallization of these complexes, presenting different dimensionalities and connectivities. The double deprotonated H2mpba2− adopts the bidentate/monodentate (1) and bis-bidentate (2) bridging modes toward the (2,2′-bipyridyl)copper(II) units affording a dinuclear compound (1) and a linear…

Self-Assembled One- and Two-Dimensional Networks Based on NH2Me2[ReX5(DMF)] (X = Cl and Br) Species: Polymorphism and Supramolecular Isomerism in Re(IV) Compounds

Three mononuclear rhenium(IV) compounds of general formula NH 2 Me 2 [ReX 5 (DMF)] [NH 2 Me 2 + = dimethylammonium cation, DMF = N,N-dimethylformamide, and X = Cl (1 and 2) and Br (3)] have been prepared and characterized. In all three cases, the rhenium atom is six-coordinated by five chloro (1 and 2) or bromo (3) atoms and one oxygen atom from a DMF molecule (1―3) building a somewhat distorted octahedral surrounding. Short Re IV ―X · · · X―Re IV contacts and H-bonds occur in the crystal lattice generating novel supramolecular Re(IV) architectures. 1 and 2 are polymorphs and supramolecular isomers that exhibit supramolecular ladder-like ( 1 ) and rectangular two-dimensional grids (2), the …

Cover Picture: Cyanide-Bridged Iron(III)–Cobalt(II) Double Zigzag Ferromagnetic Chains: Two New Molecular Magnetic Nanowires (Angew. Chem. Int. Ed. 13/2003)

Hydrogen-bond tuning of ferromagnetic interactions: synthesis, structure and magnetic properties of polynuclear copper(ii) complexes incorporating p-block oxo-anions

The reaction of copper(II) hydroxide with 2,2'-bipyridine (bipy) (1 : 1) in alkaline aqueous solution (pH 14) at room temperature affords the alternating carbonate/hydroxo-bridged copper(II) polymeric chain compound {[Cu3(bipy)3(mu-OH)2(mu-CO3)2].11H2O}n, 1, as determined by single-crystal X-ray diffraction. The structure of 1 is built up from two similar centro-symmetric dinuclear [(bipy)Cu(mu-OH)]2 cores which link together via bridging carbonate groups to mononuclear [(bipy)Cu] fragments to form the chain. Interdigitation of adjacent chains through pi-pi interactions, which involve each bipy ligand, forms sheets that are separated by the water molecules of crystallisation. Variable-tempe…

Unexpected formation of a dodecanuclear {CoII6CuII6} nanowheel under ambient conditions: magneto-structural correlations.

We report the unique heterobimetallic dodecanuclear oxamate-based {CoII6CuII6} nanowheel obtained using an environmentally friendly synthetic protocol. The effective Hamiltonian methodology employed herein allows the rationalisation of magnetic isotropic or anisotropic metal clusters, being a significant advance for future studies of exciting properties only observed at low and ultralow temperatures.

Dicopper(II) Metallacyclophanes with N,N'-2,6-Pyridinebis(oxamate): Solution Study, Synthesis, Crystal Structures, and Magnetic Properties.

The complexing ability of copper(II) in solution by the ligand N,N'-2,6-pyridinebis(oxamic acid) (H4mpyba, H4L) was determined through potentiometric and UV-vis spectroscopy at 25 °C and 0.15 M NaCl. The logarithms of the equilibrium constants for its copper(II) complexes according to the eqs 2H2L + 2Cu ⇆ [Cu2(H2L)2], 2H2L + 2Cu ⇆ [Cu2(H2L) (HL)] + H, 2H2L + 2Cu ⇆ [Cu2(HL)2] + 2H, 2H2L + 2Cu ⇆ [Cu2(HL)(L)] + 3H, and 2H2L + 2Cu ⇆ [Cu2L2] + 4H were 12.02(7), 8.04(5), 1.26(6), -7.51(6), and -16.36(6), respectively. The knowledge of the solution behavior has supported the synthesis of three new compounds bearing the common building block Cu2L2(4-). Their formulas are (Me4N)4[Cu2(mpyba)2(H2O)2]·…

Antiferromagnetic Interactions in Copper(II) µ-Oxalato Dinuclear Complexes: The Role of the Counterion

We report the preparation, crystal structure determination, magnetic properties and DFT calculations of five oxalato-bridged dicopper(II) complexes of formula [Cu-2(bpy)(2-)(H2O)(2)(C2O4)](CF3SO3)(2) (1), [Cu-2(bpy)(2)(C2O4)](PF6)(2) (2), [Cu-2(bpy)(2)(C2O4)](ClO4)(2) (3), [Cu-2(bpy)(2)Cl-2(C2O4)]center dot H2O (4) and [Cu-2(bpy)(2)(NO2)(2)(C2O4)] (5) (bpy = 2,2'-bipyridine and C2O42-= oxalate). Compounds 1, 2, 4 and 5 crystallize in the monoclinic system and 3 crystallizes in the triclinic system. The oxalate ligands in 1-5 adopt the bis-bidentate coordination mode and the two bpy molecules act as terminal ligands. The coordination of the counterions and the surroundings of the copper(II) …

Metallosupramolecular approach toward multifunctional magnetic devices for molecular spintronics

Abstract The work presented in this review constitutes a successful extension of our group's research on the chemistry and physics of dinuclear copper(II) metallacyclophanes with aromatic polyoxalamide ligands. The design and synthesis of metallacyclic complexes that contain multiple electro- and photoactive (either metal- or ligand-based) spin carriers and the study of their spectroscopic and magnetic properties as well as their redox and photochemical activity are of large interest in the multidisciplinary field of metallosupramolecular chemistry. In doing this, a ligand design approach has been followed which is based on the copper(II)-mediated self-assembly of bis(oxamato) bridging liga…

Single-ion magnet behaviour in mononuclear and two-dimensional dicyanamide-containing cobalt(ii) complexes.

Three cobalt(II) complexes of formulae [Co(dca)2(bim)4] (1), [Co(dca)2(bim)2]n (2) and [Co(dca)2(bmim)2]n (3) [dca = dicyanamide, bim = 1-benzylimidazole and bmim = 1-benzyl-2-methylimidazole] were prepared and structurally analyzed by single-crystal X-ray crystallography. Compound 1 is a mononuclear species where the cobalt(II) ion is six-coordinate with four bim molecules in the equatorial positions [Co–Nbim = 2.1546(15) and 2.1489(15) A] and two trans-positioned dca ligands [Co–Ndca = 2.1575(18) A] in the axial sites of a somewhat distorted octahedral surrounding. The structures of 2 and 3 consist of two-dimensional grids of cobalt(II) ions where each metal atom is linked to the other fo…

Slow relaxation of the magnetization in a {CoIIIMnIII} heterometallic brick-wall network

Abstract The use of the cyanide-bearing dicobalt(III) complex (PPh4)2[Co2III(μ−2,5-dpp)(CN)8] as a metalloligand towards [Mn(salen)(H2O)]ClO4 afforded the heterobimetallic two-dimensional compound of formula [{MnIII(salen)}2{(μ-NC)4Co2III(μ−2,5-dpp)(CN)4}]n (1) [PPh4+ = teraphenylphosphonium cation, 2,5-dpp = 2,5-bis(2-pyridyl)pyrazine and H2salen = N,N’-ethylenebis(salicylideneimine)] whose structure has been determined by single crystal X-ray diffraction. Compound 1 exhibits a neutral brick-wall structure, where each [Co2III(μ−2,5-dpp)(CN)8]2− unit adopts a tetrakis-monodentate bridging mode towards four {MnIII(salen)}+ fragments through four of its eight cyanide ligands. Each cobalt(III)…

Inside Cover: Oligo-m-phenyleneoxalamide Copper(II) Mesocates as Electro-Switchable Ferromagnetic Metal-Organic Wires (Chem. Eur. J. 43/2010)

Study of the interaction between [Cu(bipy)]2+ and oxalate in dimethyl sulfoxide. Crystal structure of [Cu2(bipy)2(H2O)2ox]SO4·[Cu(bipy)ox]

Abstract A study of complex formation between [Cu(bipy)]2+ and ox2− (bipy and ox2− being 2,2′-bipyridyl and the dianion of oxalic acid), has been carried out by potentiometry in dimethyl sulfoxide solution. The constants of the equilibria and are log β110 = 11.165(1) and log β210 = 13.185(5) at 25 °C and 0.1 mol dm−3 tetra-n- butylammonium perchlorate. The high values of these constants are consistent with the symmetrical bidentate and bis-bidentate modes of oxalate in [Cu(bipy)ox] and [Cu2(bipy)2ox]2+ units, respectively, as shown by X-ray diffraction studies. Well-formed single crystals of [Cu2(bipy)2(H2O)2ox]SO4· [Cu(bipy)ox] were grown from aqueous solutions and characterized by X-ray d…

Low-dimensional copper(II) complexes with the trinucleating ligand 2,4,6-tris(di-2-pyridylamine)-1,3,5-triazine: synthesis, crystal structures, and magnetic properties.

The preparation and structural characterization of three new copper(II) complexes of formula [Cu(3)(dipyatriz)(2)(H(2)O)(3)](ClO(4))(6) x 2 H(2)O (1), {[Cu(4)(dipyatriz)(2)(H(2)O)(2)(NO(3))(2)(ox)(2)](NO(3))(2) x 2 H(2)O}(n) (2), and [Cu(6)(dipyatriz)(2)(H(2)O)(9)(NO(3))(3)(ox)(3)](NO(3))(3) x 4 H(2)O (3) [dipyatriz = 2,4,6-tris(di-2-pyridylamine)-1,3,5-triazine and ox = oxalate] are reported. The structure of 1 consists of trinuclear units [Cu(3)(dipyatriz)(2)(H(2)O)(3)](6+) and uncoordinated perchlorate anions. The two dipyatriz molecules in 1 act as tris-bidentate ligands with the triazine cores being in a quasi eclipsed conformation. Each copper atom in 1 exhibits a distorted square pyr…

X-Ray structure of [ReCl4(μ-ox)Cu(pyim)2]: a new heterobimetallic ReIVCuIIferrimagnetic chain

A new heterobimetallic Re(IV)Cu(II) compound has been prepared and its crystal structure determined by single-crystal X-ray diffraction; magnetic susceptibility measurements show that this compound behaves as a ferrimagnetic chain with significant antiferromagnetic interactions between Re(IV) and Cu(II) metal ions.

Synthesis, structural analysis, and thermal and spectroscopic studies of methylmalonate-containing zinc(II) complexes

The synthesis, crystal structure, thermal analysis and spectroscopic studies of five zinc(II) complexes of formulae [Zn(Memal)(H2O)]n (1) and [Zn2(L)(Memal)2(H2O)2]n (2-5) [H2Memal = methylmalonic acid, and L = 4,4′-bipyridine (4,4′-bpy) (2), 1,2-bis(4-pyridyl)ethylene (bpe) (3), 1,2-bis(4-pyridyl)ethane (bpa) (4) and 4,4′-azobispyridine (azpy) (5)] are presented here. The crystal structure of 1 is a three-dimensional arrangement of zinc(II) cations interconnected by methylmalonate groups adopting the μ3-κ2O:κO’:κO”:κO”’ coordination mode to afford a rare (10,3)-d utp-network. The structures of the compounds 2-5 are also three-dimensional and they consist of corrugated square layers of meth…

Field-Induced Slow Magnetic Relaxation in a Six-Coordinate Mononuclear Cobalt(II) Complex with a Positive Anisotropy

International audience; The novel mononuclear Co(II) complex cis-[Co-II(dmphen)(2)(NCS)(2)]center dot 0.25EtOH (1) (dmphen = 2,9-dimethyl-1,10-phenanthroline) features a highly rhombically distorted octahedral environment that is responsible for the strong positive axial and rhombic magnetic anisotropy of the high-spin Co-II ion (D = +98 cm(-1) and E = +8.4 cm(-1)). Slow magnetic relaxation effects were observed for 1 in the presence of a dc magnetic field, constituting the first example of field-induced single-molecule magnet behavior in a mononuclear six-coordinate Co(II) complex with a transverse anisotropy energy barrier.

Synthesis, crystal structure and magnetic properties of [Cu2(bpym)(N3)4] (bpym=2,2′-bipyrimidine)

Abstract The compound of formula [Cu 2 (bpym)(N 3 ) 4 ] (bpym=2,2′-bipyrimidine) has been synthesized and its crystal structure determined by X-ray diffraction methods. It crystallizes in the monoclinic space group P 2 1 / n with cell constants: a =10.071(2), b =6.376(1), c =11.617(2) A and β=95.93(1)°; V =742.0(2) A 3 , D (calc., Z =2)=2.029 g cm −3 , M r =453.4, F (000)=448, λ (Mo Kα)=0.71073 A, μ (Mo Kα)=29.1 cm −1 and T =298 K. A total of 2027 reflections was collected over the range 3⩽2θ⩽55°; of these, 1723 were unique and 1427 were considered as observed ( I >3σ( I )) and used in the structural analysis. The final R and R w residuals were 0.0275 and 0.0328, respectively. The structure…

Synthesis, Crystal Structures, and Magnetic Properties of Two Novel Cyanido-Bridged Heterotrimetallic {CuIIMnIICrIII} Complexes

The self-assembly process between the heteroleptic [CrIII(phen)(CN)4]− and [CrIII(ampy)(CN)4]− metalloligands and the heterobimetallic {CuII(valpn)MnII}2+ tecton afforded two heterotrimetallic complexes of formula [{CuII(valpn)MnII(μ-NC)2CrIII(phen)(CN)2}2{(μ-NC)CrIII(phen)(CN)3}2]·2CH3CN (1) and {[CuII(valpn)MnII(μ-NC)2CrIII(ampy)(CN)2]2·2CH3CN}n (2) [phen = 1,10-phenanthroline, ampy = 2-aminomethylpyridine, and H2valpn = 1,3-propanedyilbis(2-iminomethylene-6-methoxyphenol)]. The crystal structure of 1 consists of neutral CuII2MnII2CrIII4 octanuclear units, where two [Cr(phen)(CN)4]− anions act as bis-monodentate ligands through cyanide groups toward two manganese(II) ions from two [CuII(v…

Syntheses, crystal structures and magnetic properties of dinuclear copper(II) complexes with pyrazino[2,3-f  ][4,7]phenanthroline (pap) as bridging ligand

Three dinuclear copper(II) complexes with pyrazino[2,3-f][4,7]phenanthroline (pap) as bridging ligand have been prepared; [Cu2(pap)(C2O4)2]·5H2O 1, [Cu2(pap)(H2O)7(SO4)]SO4·3H2O 2 and [Cu2(pap)(H2O)3(NO3)3]NO33. These are the first metal complexes of pap which have been characterized by X-ray crystallography and magnetic susceptibility measurements. In 1 the dinuclear complex is intercepted by a mirror plane; the bridging pap and the terminal oxalate ligands are bidentate in the equatorial plane of copper. In addition copper has weak axial interactions to oxygen atoms of oxalate in two neighbouring molecules. In 2 the two crystallograpically independent copper atoms are both six-co-ordinate…

Slow Dynamics of the Magnetization in One-Dimensional Coordination Polymers: Single-Chain Magnets

18 pages; International audience; Slow relaxation of the magnetization (i.e., "magnet-like" behavior) in materials composed of magnetically isolated chains was observed for the first time in 2001. This type of behavior was predicted in the 1960s by Glauber in a chain of ferromagnetically coupled Ising spins (the so-called Glauber dynamics). In 2002, this new class of nanomagnets was named single-chain magnets (SCMs) by analogy to single-molecule magnets that are isolated molecules displaying related superparamagnetic properties. A long-range order occurs only at T = 0 K in any pure one-dimensional (1D) system, and thus such systems remain in their paramagnetic state at any finite temperatur…

Chains and channels in polynuclear copper(II) complexes with 2,3-bis(2-pyridyl)pyrazine (dpp) as bridging ligand; syntheses, crystal structures and magnetic properties

Abstract The preparation and crystal structures for three Cu(II) polynuclear, chain complexes with 2,3-bis(2-pyridyl)pyrazine (dpp) as bridging ligand are reported, [Cu(dpp)(H2O)2]n(NO3)2n·2n/3H2O (1), [Cu(dpp)(H2O)2]n(CF3SO3)2n (2), and [Cu(dpp)(H2O)2]n(BF4)2n·2nH2O (3). For the latter compound the crystal structure at four different temperatures have been studied. Variable-temperature magnetic susceptibility data and ESR measurements of 1–3 and of the related copper(II) chain [Cu(dpp)(H2O)2]n(ClO4)2n·2nH2O (4) (whose structure was previously reported) have been performed. Compounds 1 and 2 crystallize in the same trigonal space group, R 3 c; 3 is orthorhombic, space group Pbca. Complexes …

Ferromagnetic coupling through spin polarization in the hexanuclear [MnII(3)CuII(3)] complex.

A novel Cu(II)-Mn(II) hexanuclear complex of formula [[MnCuL](3)(tma)](ClO(4))(3).8H(2)O [H(2)L = macrocyclic Robson proligand; H(3)tma = trimesic acid] has been obtained by connecting three heterobinuclear [Cu(II)Mn(II)L](2+) cationic species through the trimesate anion. The complex exhibits a C(3) rotational symmetry, imposed by the geometry of the bridging ligand. The interaction within each Mn(II)-Cu(II) pair is antiferromagnetic (J = -16.7 cm(-1)). A weak ferromagnetic coupling among the three S = 2 resulting spins through the tricarboxylato bridge leads to a S = 6 ground spin state, for which the spin polarization mechanism is responsible.

Bis and tris(oxalato)ferrate(iii) complexes as precursors of polynuclear compounds

The preparation and crystal structure of two oxalato-bridged NaI–FeIII compounds, [Na3Fe(ox)3(H2O)4]·H2O (1) and [FeII(phen)3][NaFe(ox)3(H2O)3]·4H2O (5), two mononuclear FeIII complexes AsPh4[Fe(bipy)(ox)2]·H2O (3) and AsPh4[Fe(phen)(ox)2]·H2O (4) and an oxalato-bridged FeIII compound [AsPh4]4[Fe2(ox)5]·5H2O (2) (ox = oxalate dianion, bipy = 2,2′-bipyridine, phen = 1,10-phenantroline and AsPh4+ = tetraphenylarsonium cation) are reported here. The structure of 1 consists of infinite anionic [NaFe(ox)3]2− layers linked trough centrosymmetric [Na4(H2O)8]4+ tetranuclear units yielding a three-dimensional motif. Crystallization water molecules ensure the cohesion of the crystal lattice in 1. The…

Versatile supramolecular self-assembly : Part II. Network formation and magnetic behaviour of copper(ii) malonate anions in ammonium derivatives

Five new metal–organic compounds of formula An[Cu(mal)2(H2O)m] (A being an amine cation and H2mal = malonic acid) have been structurally and magnetically characterized. The crystal structure of these compounds consists of an alternation of malonate-containing copper(II) anionic and amine cationic layers. Depending on the amine cation, the bis(malonate)cuprate(II) units can be connected to other units through carboxylate bridges resulting in anionic networks which exhibit different topologies: monomers (2 and 5), layers (3 and 4) and three-dimensional structures (1). Hydrogen bonding plays an important role in the self-assembling of metal–organic compounds and how the size of the amine catio…

Self-assembly of the tetrachlorido(oxalato)rhenate( iv ) anion with protonated organic cations: X-ray structures and magnetic properties

Two novel ReIV compounds of formulae [H2bpy][ReIVCl4(ox)] (1) and [H3biim]2[ReIVCl4(ox)] (2) [H2bpy2+ = 4,4′-bipyridinium dication, H3biim+ = 2,2′-biimidazolium monocation, and ox2− = oxalate dianion] have been synthesised and magneto-structurally characterised. 1 crystallises in the monoclinic system with space group C2/c, and 2 crystallises in the triclinic system with space group P[1 with combining macron]. The ReIV ion in 1 and 2 is six-coordinate, bonded to four chloride ions and two oxalate-oxygen atoms in a distorted octahedral geometry. Short intermolecular ReIV–Cl⋯Cl–ReIV contacts, Cl⋯π type interactions and hydrogen bonds are present in the crystal lattice of both compounds, gener…

The flexibility of molecular components as a suitable tool in designing extended magnetic systems

In this work we show how the design of n-dimensional magnetic compounds (nD with n = 1–3) can strongly benefit from the use crystal engineering techniques, which can give rive to structures of different shapes with different properties. We focus on the networks built by assembling the malonato-bridged tetranuclear copper(II) units Cu4(mal)4 (mal2− is the dianion of propanedioic acid, H2mal) through the potentially bridging 2,4′-bipyridine (2,4′-bpy), 4,4′-bipyridine (4,4′-bpy) and pyrazine (pyz). The magneto-structural study of the complexes of formula [Cu4(mal)4(2,4′-bpy)4(H2O)4]·8H2O (1), [Cu4(mal)4(H2O)4(4,4′-bpy)2] (2) (this compound was the subject of a previous report but it is includ…

Versatile supramolecular self-assembly. Part I. Network formation and magnetic behaviour of the alkaline salts of the bis(malonate)cuprate(ii) anion

Five malonate-containing copper(II) compounds of formula {[A(H2O)n]2 [Cu(mal)2(H2O)m]} [A = Li (1), Na (2), K (3), Rb (4) and Cs (5); H2mal = malonic acid] have been synthetized and characterized by X-ray diffraction. The structure of these compounds consists of bis(malonate)cuprate(II) anions and alkaline cations that are held together by means of carboxylate bridges and water molecules leading to 3D networks. A study of the self-assembling of the bis(malonate)cuprate(II) and the alkaline cations is carried out, the size of the alkaline metal ion playing an important role in the control of the resulting malonate-bridged copper(II) structure. A regular alternation of layers of anionic malon…

Ascorbic acid decomposition into oxalate ions: a simple synthetic route towards oxalato-bridged heterometallic 3d-4f clusters.

Two types of oxalato-bridged heterometallic 3d–4f dodeca- and hexanuclear compounds have been obtained by connecting six bi- and, respectively, trinuclear moieties through oxalato bridges arising from the slow decomposition of the L-ascorbic acid.

Crystal Structures and Magnetic Properties of Novel [LnIIICuII4] (Ln = Gd, Dy, Ho) Pentanuclear Complexes. Topology and Ferromagnetic Interaction in the LnIII−CuII Pair

The first pentanuclear complexes of formula {Dy[Cu(apox)](2)[Cu(apox)(H(2)O)](2)}[ClO(4)](3).7H(2)O (1), {Ho[Cu(apox)][Cu(apox)(H(2)O)](3)}[PF(6)](3).4.5H(2)O (2), {Gd[Cu(apox)](2)[Cu(apox)(H(2)O)](2)}[ClO(4)](3).7H(2)O (3) and {Gd[Cu(apox)][Cu(apox) (H(2)O)](3)}[PF(6)](3).4.5H(2)O (4) (H(2)apox = N,N'-bis(3-aminopropyl)oxamide) have been synthesized. The crystal structures of complexes 1 and 2 have been determined by X-ray diffraction methods. Complexes 3 and 4 are isostructural with 1 and 2, respectively. Crystallographic data are as follows: 1 and 3, monoclinic, space group C2/c and Z = 4, with a = 14.646(6) Å, b = 29.496(7) Å, c = 16.002(7) Å, and beta = 111.76(2) degrees for 1 and a = …

C3-symmetric trinuclear copper(ii) species as tectons in crystal engineering

Three new complexes have been obtained using C3-symmetric trinuclear complexes as tectons; [Cu3(felden)(NCS)3(dmf)3] (1), [Cu3(felden)(mand)3]·(C2H5)2O (2), and [Cu3(felden)(dca)3(C2H5OH)]·2H2O (3) (H3felden is the Schiff base resulting from the condensation of 2,4,6-triformylphloroglucinol with N,N-dimethylethylenediamine, mand− is the anion of the R-mandelic acid and dca− is the dicyanamide anion). Compounds 1 and 2 are discrete trinuclear species, while compound 3 is a 2D coordination polymer, constructed from trinuclear nodes and dicyanamido spacers. The variable-temperature magnetic properties of 1–3 have been investigated and they reveal the occurrence of weak antiferromagnetic intera…

Preparation, crystal structures and magnetic properties of three thiocyanato-bridged copper(II) complexes with 2,2′-biimidazole or 2-(2′-pyridyl)imidazole as terminal ligands

The synthesis, crystal structures and variable temperature magnetic investigation of three new thiocyanato-bridged copper(II) complexes with 2,2′-biimidazole (H2bim) or 2-(2′-pyridyl)imidazole) (pyim) as coligands, {[Cu(H2bim)2][Cu(H2bim)(NCS)2(SCN)0.6667(NO3)0.3333]2} · 2H2O (1), [Cu(H2bim)(NCS)2]n (2) and [Cu(pyim)(NCS)2]n (3) are reported. Complex 1 contains centrosymmetric trinuclear species where central [Cu(2)(H2biim)2]2+ cations and peripheral [Cu(1)(H2biim)(NCS)2(SCN)]− anions are linked through single end-to-end thiocyanato bridges. Complexes 2 and 3 are made up of neutral zigzag chains of copper(II) ions linked by single (2) and double (3) end-to-end thiocyanato bridges. A bidenta…

Metamagnetic behaviour in a new Cu(ii)Re(iv) chain based on the hexachlororhenate(iv) anion

A new chloro-bridged heterobimetallic Cu(ii)Re(iv) chain of formula {Cu(pyim)(Him)2ReCl6}n·MeCN (·MeCN) has been prepared and magnetostructurally characterised. Compound is the first example of the [Re(IV)Cl6](2-) anion acting as a metalloligand towards a paramagnetic metal ion.

Cover Feature: Design of Magnetic Coordination Polymers Built from Polyoxalamide Ligands: A Thirty Year Story (Eur. J. Inorg. Chem. 3‐4/2018)

Novel cobalt(II) coordination polymers based on 1,2,4,5-benzenetetracarboxylic acid and extended bis-monodentate ligands

Four new high-spin cobalt(II) complexes of formulae [Co2(bta)(4,4′-bpy)2(H2O)2]n (1), {Hbpe[Co(Hbta)(bpe)(H2O)2]}n (2), {[Co(H2bta)(azpy)(H2O)2]·azpy}n (3) and {[Co2(bta)(bpa)2(H2O)4]·8H2O}n (4) with H4bta = 1,2,4,5-benzenetetracarboxylic acid, 4,4′-bpy = 4,4′-bipyridine, bpe = trans-1,2-bis(4-pyridyl)ethene, azpy = 4,4′-azobispyridine and bpa = trans-1,2-bis(4-pyridyl)ethane, have been prepared and characterized by single crystal X-ray diffraction. Compounds 1–4 exhibit two-dimensional networks where the fully (1 and 4) or partially (2 and 3) deprotonated tetracarboxylic ligand connects two (2 and 3) or four (1 and 4) cobalt(II) ions through two trans-carboxylate (1–3) or all the carboxyla…

Oxamato-based coordination polymers: recent advances in multifunctional magnetic materials

The design and synthesis of novel examples of multifunctional magnetic materials based on the so-called coordination polymers (CPs) have become very attractive for chemists and physicists due to their potential applications in nanoscience and nanotechnology. However, their preparation is still an experimental challenge, which requires a deep knowledge of coordination chemistry and large skills in organic chemistry. The recent advances in this field using a molecular-programmed approach based on rational self-assembly methods which fully exploit the versatility of the coordination chemistry of the barely explored and evergreen family of N-substituted aromatic oligo(oxamato) ligands are prese…

Syntheses, Characterization, and Magnetic Studies of Copper(II) Complexes with the Ligand N,N,N′,N′-Tetrakis(2-pyridylmethyl)-1,3-benzenediamine (1,3-tpbd) and its Phenol Derivative 2,6-Bis[bis(2-pyridylmethyl)amino]-p-cresol] (2,6-Htpcd)

The copper(II) complexes [Cu4(1,3-tpbd)2(H2O)4(NO3)4]n(NO3)4n·13nH2O (1), [Cu4(1,3-tpbd)2(AsO4)(ClO4)3(H2O)](ClO4)2·2H2O·0.5CH3OH (2), [Cu4(1,3-tpbd)2(PO4)(ClO4)3(H2O)](ClO4)2·2H2O·0.5CH3OH (3), [C...

Ferrocene containing chelating ligands 3. Synthesis, spectroscopic characterization, electrochemical behaviour and interaction with metal ions of new ligands obtained by condensation of ferrocenecarboxaldehyde with 2-amino-benzoic acid derivatives. Crystal structures of 2-ferrocenylmethylamino-5-methyl-benzoic acid and 2-bis(ferrocenylmethyl)ammonium-5-methyl-benzoic acid perchlorate

Abstract Ferrocenecarboxaldehyde reacts with 2-amino-benzoic acid, 2-amino-5-methyl-benzoic acid or 3-amino-2-naphthoic acid to give the corresponding Schiff-base derivatives 2-ferrocenylmethylidenimino-benzoic acid (1), 2-ferrocenylmethylidenimino-5-methyl-benzoic acid (2) and 3-ferrocenylmethylidenimino-2-naphthoic acid (3). 1, 2 and 3 are stable in the solid state but easily hydrolyze in solution. This hydrolysis has been studied kinetically in a methanol-water medium. In order to increase the stability in solution to use these compounds as ligands, the imino group from 1, 2 and 3 was reduced by NaBH4 to give the amino derivatives 2-ferrocenylmethylamino-benzoic acid (4), 2-ferrocenylmet…

Design of 3d–4f molecular squares through the [Fe{(HB(pz)3)}(CN)3]− metalloligand

A new series of {FeIII2LnIII2} heterobimetallic squares of general formula [FeIII{HB(pz)3}(CN)(μ-CN)2Ln(pyim)x(NO3)2(H2O)y]2·zH2O [Ln = La (1), Gd (2), Tb (3) and Dy (4); {HB(pz)3}− = hydrotris(pyrazolyl)borate and pyim = 2-(1H-imidazol-2-yl)pyridine; x = 2, y = 0 (1), x = y = 1 (2–4) and z = 10 (1), 6 (2), 2.76 (3), 4 (4)] were synthesized by reacting the low-spin [FeIII{HB(pz)3}(CN)3]− complex anion with the preformed [LnIII(pyim)x(NO3)2(H2O)y]+ complex cation [formed in situ by mixing the lanthanide(III) salt and the pyim ligand]. Single-crystal X-ray diffraction shows that 1–4 crystallize in the P triclinic space group, 2–4 being isomorphous. In all cases, the structure comprises neutra…

Magneto-structural studies on heterobimetallic malonate-bridged M(II)Re(IV) complexes (M = Mn, Co, Ni and Cu).

The mononuclear Re(IV) compound of formula (PPh(4))(2)[ReBr(4)(mal)] (1) was used as a ligand to obtain the heterobimetallic species [ReBr(4)(μ-mal)Co(dmphen)(2)]· MeCN (2), [ReBr(4)(μ-mal)Ni(dmphen)(2)] (3), [ReBr(4)(μ-mal)Mn(dmphen)(2)] (4a), [ReBr(4)(μ-mal)Mn(dmphen)(H(2)O)(2)]·dmphen·MeCN·H(2)O (4b), [ReBr(4)(μ-mal)Cu(phen)(2)]·1/4H(2)O (5) and [ReBr(4)(μ-mal)Cu(bipy)(2)] (6) (mal = malonate dianion, dmphen = 2,9-dimethyl-1,10-phenanthroline, phen = 1,10-phenanthroline and bipy = 2,2'-bipyridine). The structures of 2 and 5 (single-crystal X-ray diffraction) are made up of neutral [ReBr(4)(μ-mal)M(AA)] dinuclear units [AA = dmphen with M = Co (2) and AA = phen with M = Cu (5)] where the …

2,2′-Bipyrimidine- and 2,3-bis(2-pyridyl)pyrazine-containing manganese(II) compounds: Structural and magnetic properties

The preparation, crystal structures and magnetic properties of four different manganese(II) compounds of formula [Mn(bipym)Cl2]n·2nH2O (1), [Mn2(dpp)2(H2O)2Cl4]·2H2O (2), [Mn(dpp)(H2O)2]n(ClO4)2n·1.5nH2O (3) and [Mn(dpp)(dca)2]n (4) [bipym = 2,2′-bipyrimidine, dpp = 2,3-bis(2-pyridyl)pyrazine and dca = dicyanamide anion] are reported. Compounds 1 and 3 are uniform chains of six-coordinated manganese(II) ions bridged by bis(bidentate) bipym (1) and dpp (3) ligands with two chloride groups (1) and two water molecules (3) in cis position. The electroneutrality in 3 is achieved by uncoordinated perchlorate anions. The manganese atom in 1 and 3 exhibits a distorted octahedral environment mainly …

Self-assembly, binding ability and magnetic properties of dicopper(ii) pyrazolenophanes

A novel series of dinuclear copper(II) pyrazolenophanes of the formula [Cu2(μ-4-Mepz)2(μ-ClO4)(ClO4)(bpm)2] (1), [Cu2(μ-pz)2(μ-H2O)(ClO4)(4,7-Me2phen)2]ClO4·H2O·CH3CN (2), [Cu2(μ-pz)2(μ-H2O)(ClO4)3/2(H2O)1/2(phen)2]2[Cu2(μ-pz)2(μ-ClO4)(ClO4)2(phen)2]·8H2O (3), and [Cu2(μ-pz)2(CH3CN)2(3,4,7,8-Me4phen)2](ClO4)2 (4) (Hpz = pyrazole, H-4-Mepz = 4-methylpyrazole, bpm = 2,2'-bipyrimidine, phen = 1,10-phenanthroline, 4,7-Me2phen = 4,7-dimethyl-1,10-phenanthroline, and 3,4,7,8-Me4phen = 3,4,7,8-tetramethyl-1,10-phenanthroline) have been synthesized and magneto-structurally investigated. The crystal structures of 1–4 contain bis(pyrazolate)(perchlorate)- (1 and 3), bis(pyrazolate)(aqua)- (2 and 3), …

Intramolecular versus intermolecular exchange pathways in the binuclear complex [Cu2(H2tea)2(4,4′-bipy)](ClO4)2·3H2O (H3tea=triethanolamine and 4,4′-bipy=4,4′-bipyridine)

Abstract The binuclear copper(II) complex of formula [Cu2(H2tea)2(4,4′-bipy)](ClO4)2·3H2O (1) (H3tea=triethanolamine and 4,4′-bipy=4,4′-bipyridine) has been isolated and characterized by X-ray diffraction. Its structure consists of dinuclear [Cu2(H2tea)2(4,4′-bipy)]2+ cations, uncoordinated perchlorate anions and crystallization water molecules. Each copper atom exhibits a trigonal-bipyramidal environment with the three triethanolamine-oxygen atoms building the equatorial plane, and the triethanolamine-nitrogen and one of the 4,4′-bipy nitrogen atoms defining the three-fold axis. The 4,4′-bipy molecule acts as a bismonodentate bridging ligand, the copper–copper separation across it being 11…

Magnetic coupling in discrete cyano-bridged Mn(III)-Fe(III) motifs: synthesis, crystal structure, magnetic properties and theoretical study.

The preparation, crystal structures and magnetic properties of the heterobimetallic complexes of formula [Mn(III)(n-MeOsalen)(H(2)O)(mu-CN)Fe(III)(bpym)(CN)(3)]·mH(2)O with n = m = 3 (1) and n = 4 and m = 2 (2) [n-MeOsalen(2-) = N,N'-ethylenebis(n-methoxysalicylideneiminate) dianion and bpym = 2,2'-bipyrimidine] are reported. 1 and 2 are dinuclear neutral species where the cyano-bearing low-spin unit [Fe(III)(bpym)(CN)(4)](-) acts as a monodentate ligand towards the [Mn(III)(SB)(solv)(x)](+) entity (SB = tetradentate Schiff-base) through one of its four cyano groups. Adjacent heterobimetallic units are interlinked through hydrogen bonds involving the coordinated water molecule of one dinucl…

Photoluminescent and Slow Magnetic Relaxation Studies on Lanthanide(III)-2,5-pyrazinedicarboxylate Frameworks

In the series described in this work, the hydrothermal synthesis led to oxidation of the 5-methyl-pyrazinecarboxylate anion to the 2,5-pyrazinedicarboxylate dianion (2,5-pzdc) allowing the preparation of three-dimensional (3D) lanthanide(III) organic frameworks of formula {[Ln2(2,5-pzdc)3(H2O)4]·6H2O}n [Ln = Ce (1), Pr (2), Nd (3), and Eu (4)] and {[Er2(2,5-pzdc)3(H2O)4]·5H2O}n (5). Single-crystal X-ray diffraction on 1–5 reveals that they crystallize in the triclinic system, P1 space group with the series 1–4 being isostructural. The crystal structure of the five compounds are 3D with the lanthanide(III) ions linked through 2,5-pzdc2– dianions acting as two- and fourfold connectors, buildi…

Cu(ii)-alginate-based superporous hydrogel catalyst for click chemistry azide-alkyne cycloaddition type reactions in water.

A novel sustainable hydrogel catalyst based on the reaction of sodium alginate naturally extracted from brown algae Laminaria digitata residue with copper(II) was prepared as spherical beads, namely Cu(II)-alginate hydrogel (Cu(II)-AHG). The morphology and structural characteristics of these beads were elucidated by different techniques such as SEM, EDX, BET, FTIR and TGA analysis. Cu(II)-AHG and its dried form, namely Cu(II)-alginate (Cu(II)-AD), are relatively uniform with an average pore ranging from 200 nm to more than 20 μm. These superporous structure beads were employed for the copper catalyzed [3 + 2] cycloaddition reaction of aryl azides and terminal aryl alkynes (CuAAC) via click …

Multielectron transfer in a dicopper(II) anthraquinophane.

The new dinuclear copper(II) metallacyclophane with the non-innocent N,N'-1,4-bis(oxamate)-9,10-anthraquinone bridging ligand possesses a dual multielectron redox behavior featuring stepwise one-electron oxidation of the antiferromagnetically coupled Cu(II) ions and two-electron reduction of the anthraquinone spacers in a π-stacked anti conformation.

Crystal structures and magnetic properties of uniform and alternating azido-bridged (2,2′-bipyridyl)copper(II) chains

Abstract Single crystals of four copper(II) complexes of formula [Cu(bipy)(N3)2]n (1,2), [Cu(bipy)2(N3)(ClO4)] (3) and [Cubipy)2(N3)]ClO4 (4) (bipy=2,2′-bipyridine) were obtained from aqueous solutions containing (2,2′-bipyridyl) copper(II) perchlorate and sodium azide, and their crystal structures were determined by X-ray diffraction methods. The structures of compounds 1 and 4 were already known, but the better accuracy of our structural determination of complex 1 led us to reconsider it here. The structures of compounds 1 and 2 are made up of neutral chains of copper(II) ions bridged by two azide groups exhibiting asymmetrical end-on (1) and alternating asymmetrical end-on and end-to-end…

Spin canting in Re(IV) complexes: magnetic properties of [ReX4(bpym)] ( X = Cl and Br; bpym = 2,2′-bipyrimidine)

The mononuclear complexes [ReCl4(bpym)] (1) and [ReBr4(bpym)] (2) (bpym = 2,2′-bipyrimidine) are weak ferromagnets. Magnetic ordering occurs below 7.0 (1) and 20.0 K (2) and good hysteresis loops are observed for the two compounds at 2.0 K. A spin-canting phenomenon, i.e., a non-strict linearity of the individual spins aligned in an anti-parallel way by intermolecular antiferromagnetic coupling occurring in many Re(IV) complexes, accounts for these magnetic features which are unusual in molecular solids such as 1 and 2.

[Cr(dmbipy)(ox)2]−: a new bis-oxalato building block for metal assembling. Crystal structures and magnetic properties of XPh4[Cr(dmbipy)(ox)2]·5H2O (X = P and As), {Ba(H2O)2[Cr(dmbipy)(ox)2]2}n·17/2nH2O and {Ag(H2O)[Cr(dmbipy)(ox)2]}n·3nH2O

The synthesis, X-ray structure and variable-temperature magnetic study of new compounds of formula PPh4[Cr(dmbipy)(ox)2]·5H2O (1), AsPh4[Cr(dmbipy)(ox)2]·5H2O (2), {Ba(H2O)2[Cr(dmbipy)(ox)2]2}n·17/2nH2O (3) and {Ag(H2O)[Cr(dmbipy)(ox)2]}n·3nH2O (4) (PPh4+ = tetraphenylphosphonium cation; AsPh4+ = tetraphenylarsonium cation; dmbipy = 4,4′-dimethyl-2,2′-bipyridine; ox2− = oxalate dianion) are reported herein. The isomorphous compounds 1 and 2 are made up of discrete [Cr(dmbipy)(ox)2]− anions, XPh4+ cations [X = P (1) and As (2)] and uncoordinated water molecules. The chromium environment in 1 and 2 is distorted octahedral with Cr–O and Cr–N bond distances varying in the ranges 1.950(2)–1.9782…

Design of single cyanide-bridged tetranuclear bimetallic rectangles exhibiting ferromagnetic coupling

Abstract The cyanide-bridged tetranuclear bimetallic rectangles ( XPh 4 ) 4 [ Fe 2 III Cu 2 II ( μ - CN ) 4 ( CN ) 8 ( L ) 2 ] · n H 2 O [X = P (1) and As (2); L = bpcam (1) and bpca (2); n = 4 (1) and 0 (2)] have been prepared and their crystal structures were characterized by single crystal X-ray diffraction; 1 exhibits intramolecular ferromagnetic interactions (J1 = +3.7 cm−1 and J2 = +7.0 cm−1, H = - J 1 [ S Fe ( 1 ) · S Cu ( 1 ) + S Fe ( 1 a ) · S Cu ( 1 a ) ] − J 2 [ S Fe ( 1 ) · S Cu ( 1 a ) + S Fe ( 1 a ) · S Cu ( 1 ) ] + D [ S Fe ( 1 ) z 2 + S Fe ( 1 a ) z 2 ] ) leading to a low-lying S = 2 spin state.

Synthesis, crystal structure and magnetic properties of the first single azido-bridged copper(II) chain [Cu(bpym)(N3)2]n (bpym = 2,2′-bipyrimidine)

Abstract Single crystals of the copper(II) chain of formula [Cu(bpym) (N32]n (bpym = 2,2′-bipyrimidine) were prepared and characterized by X-ray diffraction methods. The structure consists of neutral chains of copper (II) ions bridged by a single azide group exhibiting the asymmetric end-to-end coordination mode. A terminally bound azide ligand and a didentate bpym group complete the square pyramidal geometry of the metal atom. The intrachain copper-copper separation is 5.063(1)A. The magnetic behaviour was investigated in the temperature range 2.0–290 K. The susceptibility curve exhibits a maximum at .9 K showing the occurrence of a weak intrachain antiferromagnetic coupling. Analysis of t…

A new chiral dimanganese(iii) complex: synthesis, crystal structure, spectroscopic, magnetic, and catalytic properties

Two enantiomeric complexes of formula [MnIII2(μ-OCH3)2(R-valBINAM)2]·1.75DMF (1) and [MnIII2(μ-OCH3)2(S-valBINAM)2]·2DMF (2) [valBINAM = 1,1′-binaphthalene-2,2′-bis(3-methoxysalicylideneiminate)] have been synthesized using as a ligand the chiral Schiff bases resulting from the condensation reactions between o-vanillin and the chiral 1,1′-binaphthyl-2,2′-diamine. The structures of 1 and 2 which have been solved by single crystal X-ray diffraction consist of neutral dimers, the manganese(III) ions being bridged by two methoxido anions, arising from the solvent, and by two valBINAM2− ligands. Their circular dichroism spectra at room temperature emphasize the occurrence of the exciton coupling…

Slow relaxation of the magnetization in Oximato-bridged heterobimetallic Copper(II)-Manganese(III) chains

The use of the oximato-containing copper(II) complexes, [Cu(Hdeg)2] (H2deg = diethylglyoxime), [Cu(Hmeg)2] (H2meg = methylethylglyoxime) and [Cu(Hdmg)2] (H2dmg = dimethylglyoxime), as ligands toward manganese(II) acetate in methanol afforded the heterobimetallic compounds of formula [MnCu(deg)2(CH3COO)(H2O)2] (1), [MnCu(meg)2(CH3COO)(H2O)2] (2) and [MnCu(dmg)2(CH3COO)(H2O)2] (3) where the starting manganese(II) ion was oxidized to manganese(III) by air. In the lack of single crystals suitable for X-ray diffraction analysis, X-ray absorption techniques (EXAFS and XANES) at 40 K were used for the structural characterization of 1-3. The analysis of the X-ray absorption data reveals that 1-3 ar…

Influence of Copper(II) and Nickel(II) Ions in the Topology of Systems Based on a Flexible Bis-Oxamate and Bipyridine Building Blocks

Single crystals of the mononuclear bis-oxamate nickel(II) complex [Ni(bipy)(H2edpba)]·dmso (1) are obtained by reacting [Ni(bipy)Cl2]·H2O and the flexible K2(H2edpba) ligand [bipy = 2,2′-bipyridine; H4edpba = N,N′-2,2′-ethylenediphenylenebis(oxamic acid)]. The reaction of 1 with copper(II) ions resulted in two products in which the replacement of the nickel(II) ion by copper(II) took place: the chain compound [Cu(bipy)(H2edpba)]n·3nH2O·ndmso [dmso = dimethyl sulfoxide] (2) and the analogous chain compound without dmso crystallization molecules [Cu(bipy)(H2edpba)]n·1.5nH2O (3a) in its polycrystalline form. The reaction of [Cu(bipy)Cl2] and K2(H2edpba) yielded single crystals of [Cu(bipy)(H2e…

Design of Magnetic Coordination Polymers Built from Polyoxalamide Ligands: A Thirty Year Story

International audience; The aim of this review is to pay tribute to the legacy of O. Kahn. Kahn's credo was to synthesize magnetic compounds with predictable structure and magnetic properties. This is illustrated herein with results obtained by Kahn's group during his Orsay period thirty years ago, but also on the basis of our recent results on the synthesis of coordination polymers with oxamate ligands. The first part of this review is devoted to a short description of the necessary knowledge in physics and theoretical chemistry that Kahn and his group have used to select oxamate ligands, the complex‐as‐ligand strategy and the synthesis of heterobimetallic systems. Then, we describe the st…

A Theoretical Study of the Relationship between the Electrophilicity ω Index and Hammett Constant σp in [3+2] Cycloaddition Reactions of Aryl Azide/Alkyne Derivatives

The relationship between the electrophilicity ω index and the Hammett constant σp has been studied for the [2+3] cycloaddition reactions of a series of para-substituted phenyl azides towards para-substituted phenyl alkynes. The electrophilicity ω index—a reactivity density functional theory (DFT) descriptor evaluated at the ground state of the molecules—shows a good linear relationship with the Hammett substituent constants σp. The theoretical scale of reactivity correctly explains the electrophilic activation/deactivation effects promoted by electron-withdrawing and electron-releasing substituents in both azide and alkyne components.

Structural analysis and magnetic properties of the copper(II) dicyanamide complexes [Cu2(dmphen)2(dca)4], [Cu(dmphen)(dca)(NO3)] and [Cu(4,4′-dmbpy)(H2O)(dca)2] (dca=dicyanamide; dmphen=2,9-dimethyl-1,10-phenanthroline; 4,4′-dmbpy=4,4′-dimethyl-2,2′-bipyridine)

Abstract The preparation, crystal structures and magnetic properties of three copper(II) compounds of formulae [Cu2(dmphen)2(dca)4] (1), [Cu(dmphen)(dca)(NO3)]n (2) and [Cu(4,4′-dmbpy)(H2O)(dca)2] (3) (dmphen=2,9-dimethyl-1,10-phenanthroline, dca=dicyanamide and 4,4′-dmbpy=4,4′-dimethyl-2,2′-bipyridine) are reported. The structure of 1 consists of discrete copper(II) dinuclear units with double end-to-end dca bridges whereas that of 2 is made up of neutral uniform copper(II) chains with a single symmetrical end-to-end dca bridge. Each copper atom in 1 and 2 is in a distorted square pyramidal environment: two (1) or one (2) nitrile-nitrogen atoms from bridging dca groups, one of the nitrogen…

2,2'-BIPYRIMIDINEOXALATOCOPPER(II) COMPLEXES - FROM THE MONONUCLEAR COMPLEX TO THE 2D SHEET-LIKE POLYMER

Synthesis, crystal structure and magnetic properties of H2tppz[ReCl6] and [Cu(bpzm)2(μ-Cl)ReCl3(μ-ox)Cu(bpzm)2(μ-ox)ReCl3(μ-Cl)]n.

Two new Re(iv) compounds of formulae H2tppz[ReCl6] (1) and [Cu(bpzm)2(μ-Cl)ReCl3(μ-ox)Cu(bpzm)2(μ-ox)ReCl3(μ-Cl)]n (2) [tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine and bpzm = bis(pyrazolyl-1-yl)methane] have been prepared and their crystal structures determined by X-ray diffraction on single crystals. Compound 1 is a mononuclear species whose structure consists of octahedral hexachlororhenate(iv) anions and diprotonated H2tppz(2+) cations which are arranged in the unit cell as alternating anionic and cationic layers, held together by electrostatic forces. The structure of 2 is made up of alternating [Cu(1)(bpzm)2](2+) and [(ox)ReCl3(μ-Cl)Cu(2)(bpzm)2(μ-Cl)ReCl3(ox)](2-) entities interlinked …

Synthesis, Crystal Structures, and Magnetic Properties of a New Family of Heterometallic Cyanide-Bridged FeIII2MII2 (M = Mn, Ni, and Co) Square Complexes

New heterobimetallic tetranuclear complexes of formula [Fe(III){B(pz)(4)}(CN)(2)(μ-CN)Mn(II)(bpy)(2)](2)(ClO(4))(2)·CH(3)CN (1), [Fe(III){HB(pz)(3)}(CN)(2)(μ-CN)Ni(II)(dmphen)(2)](2)(ClO(4))(2)·2CH(3)OH (2a), [Fe(III){B(pz)(4)}(CN)(2)(μ-CN)Ni(II)(dmphen)(2)](2)(ClO(4))(2)·2CH(3)OH (2b), [Fe(III){HB(pz)(3)}(CN)(2)(μ-CN)Co(II)(dmphen)(2)](2)(ClO(4))(2)·2CH(3)OH (3a), and [Fe(III){B(pz)(4)}(CN)(2)(μ-CN)Co(II)(dmphen)(2)](2)(ClO(4))(2)·2CH(3)OH (3b), [HB(pz)(3)(-) = hydrotris(1-pyrazolyl)borate, B(Pz)(4)(-) = tetrakis(1-pyrazolyl)borate, dmphen = 2,9-dimethyl-1,10-phenanthroline, bpy = 2,2'-bipyridine] have been synthesized and structurally and magnetically characterized. Complexes 1-3b have be…

2,2’Bipyrimidine: A Useful Tool in Designing Polynuclear Complexes of Controlled Nuclearity

The versatility of a simple ligand such as 2,2’-bipyrimidine (bpym) which can adopt chelating and bis(chelating) coordination modes facilitates the preparation of both mononuclear and polynuclear complexes whose nuclearity can be controlled by playing with the metal to bpym molar ratio, the nature of the counterion and the presence of additional ligands. In this work, we summarize our results dealing with the preparation and the structural and magnetic characterization of complexes between first-row transition metal ions and bpym. Examples of orbital reversal and tunable exchange in bpym-containing copper(II) complexes are presented and discussed. The influence of the number of unpaired ele…

Synthesis, crystal structure and magnetic properties of the malonato-bridged bimetallic chain [Mn(II)Cu(II)(mal)2(H2O)4]·2H2O

Abstract The first malonato-bridged bimetallic chain of formula [MnCu(mal)2(H2O)4]·2H2O (1) (H2mal=malonic acid) was prepared and its structure determined by X-ray diffraction methods. Each copper atom in 1 is in a square planar environment formed by four malonate-oxygens from two malonate ligands. The manganese atom is six-coordinated with four water molecules and two cis-coordinated malonate-oxygens from two malonate groups building a distorted octahedral surrounding. The malonate group acts simultaneously as bidentate and monodentate ligand towards copper and manganese atoms respectively, leading to a bimetallic chain. Two structurally different carboxylato-bridges exhibiting an anti–syn…

Solid‐State Anion–Guest Encapsulation by Metallosupramolecular Capsules Made from Two Tetranuclear Copper(II) Complexes (Eur. J. Inorg. Chem. 29/2007)

The cover picture shows unique examples of homo- and heterochiral, dimeric metal capsules resulting from the self-assembly of two helical, bowl-shaped tetranuclear copper(II) complexes that encapsulate different anions in the solid state, like pearls in an oyster (shown as the background). This kind of self-assembled, coordination-bonded motifs are a major topic in metallosupramolecular chemistry because of their binding capabilities and associated host–guest chemistry. However, their magnetic properties are largely unexplored, and here we provide one of the rare magnetic studies on these host–guest systems. For more details on the combined structural and magnetic investigations of this cla…

A new eight-coordinate complex of manganese(II): synthesis, crystal structure, spectroscopy and magnetic properties of [Mn(Hoxam)2(H2O)4] (H2oxam=oxamic acid)

Abstract The crystal structure of an eight-coordinate manganese(II) compound containing oxamato and water molecules as ligands [Mn(Hoxam)2(H2O)4], were H2oxam=oxamic acid, has been determined by X-ray diffraction on single-crystals. The coordinated oxygen atoms are located at the vertices (corners) of a distorted bicapped trigonal antiprism. Hydrogen bonding is responsible for an extended 3D-network. The magnetic susceptibility data of the compound have been investigated. χMT follows the Curie law, at very low temperatures χMT decreases smoothly due to weak intermolecular interactions and/or due to a small zero field splitting of the sextuplet spin state of the Mn(II).

[Fe(bipy)(CN)4]- as a Versatile Building Block for the Design of Heterometallic Systems:  Synthesis, Crystal Structure, and Magnetic Properties of PPh4[FeIII(bipy)(CN)4]·H2O, [{FeIII(bipy)(CN)4}2MII(H2O)4]·4H2O, and [{FeIII(bipy)(CN)4}2ZnII]·2H2O [bipy = 2,2‘-Bipyridine; M = Mn and Zn]

The new cyano complexes of formulas PPh4[FeIII(bipy)(CN)4]·H2O (1), [{FeIII(bipy)(CN)4}2MII(H2O)4]·4H2O with M = Mn (2) and Zn (3), and [{FeIII(bipy)(CN)4}2ZnII]·2H2O (4) [bipy = 2,2‘-bipyridine and PPh4 = tetraphenylphosphonium cation] have been synthesized and structurally characterized. The structure of complex 1 is made up of mononuclear [Fe(bipy)(CN)4]- anions, tetraphenyphosphonium cations, and water molecules of crystallization. The iron(III) is hexacoordinated with two nitrogen atoms of a chelating bipy and four carbon atoms of four terminal cyanide groups, building a distorted octahedron around the metal atom. The structure of complexes 2 and 3 consists of neutral centrosymmetric […

Cadmium(ii) coordination polymers based on substituted malonic acid: synthesis, characterization and photoluminescence properties

Four novel complexes of cadmium(II) with alkyl/aryl-substituted malonate ligands of formulae {[Cd(Memal)(H2O)]6·0.5H2O}n (1), [Cd(Etmal)(H2O)]n (2), [Cd(Butmal)(H2O)]n (3) and [Cd(Bzmal)(H2O)]n (4), (Memal = methylmalonate, Etmal = ethylmalonate, Butmal = butylmalonate and Bzmal = benzylmalonate) have been prepared and characterized by single crystal X-ray analysis. Their luminescence, UV-Vis absorption properties and thermal behaviour were also investigated. Complex 1 is a three-dimensional compound where each metal centre is connected to four other ones leading to a sodalite network with the point symbol {42·64}. Each cadmium(II) ion in 1 is seven-coordinate with a water molecule and six …

Homo- and heterometallic complexes constructed from hexafluoroacetylacetonato and Schiff-base complexes as building-blocks

Three new homo- and heterotrimetallic complexes have been synthesized and crystallographically characterized: [Cu2(saldmpn)2(μ-OCH3)2Cu2(hfac)2] (1), [Ni2(valaepy)2(hfac)2] (2), [Cu(saldmpn)Co(hfac)2] (3) [H2saldmpn is the Schiff-base resulting from condensation of salicylaldehyde with 2,2-dimethyl-1,3-diaminopropane and Hvalaepy results from the reaction of o-vanillin with 2-(2-aminoethyl)pyridine)]. The structure of 1 consists of a neutral tetranuclear species that can be viewed as resulting from mutual coordination of one {(hfac)Cu(μ-OCH3)2(Cu(hfac)} and two {Cu(saldmpn)} building blocks. Compound 2 is a binuclear complex that results from two {Ni(hfac)(valaepy} fragments, the nickel(II)…

Structural versatility of the malonate ligand as a tool for crystal engineering in the design of molecular magnets

The synthesis of ferro- and ferri-magnetic systems with a tunable Tc and three-dimensional (3-D) ordering from molecular precursors implying transition metal ions is one of the active branches of molecular inorganic chemistry. The nature of the interactions between the transition metal ions (or transition metal ions and radicals) is not so easy to grasp by synthetic chemists working in this field since it may be either electrostatic (orbital) or magnetic (mainly dipolar). Therefore, the systems fulfilling the necessary requirements to present the expected magnetic properties are not so easy to design on paper and realize in the beaker. In this work we show how the design of one-, two- and t…

A pH-triggered bistable copper(II) metallacycle as a reversible emulsion switch for biphasic processes.

A unique bistable copper-metallacyclic complex is used as an elegant molecular switch for the reversible formation of emulsions by simple pH variation. This switch may have several exciting applications in biphasic processes such as catalysis and separation science technologies.

Slow Relaxation of the Magnetization in a {Co <sup>III</sup>Mn <sup>III</sup>} Heterometallic Brick-Wall Network

The use of the cyanide-bearing dicobalt(III) complex (PPh 4 ) 2 [Co 2 III (m-2,5-dpp)(CN) 8 ] as a metalloligand towards [Mn(salen)(H 2 O)]ClO 4 afforded the heterobimetallic two-dimensional compound of formula [{Mn III (salen)} 2 {(m-NC) 4 Co 2 III (m-2,5-dpp)(CN) 4 }] n (1) [PPh 4 + = teraphenylphosphonium cation, 2,5-dpp = 2,5-bis(2-pyridyl)pyrazine and H 2 salen = N,N’ -ethylenebis(salicylideneimine)] whose structure has been determined by single crystal X-ray diffraction. Compound 1 exhibits a neutral brick-wall structure, where each [Co 2 III (m-2,5-dpp)(CN) 8 ] 2- unit adopts a tetrakis-monodentate bridging mode towards four {Mn III (salen)} + fragments through four of its eight cyan…

Sustainable carbon–carbon bond formation catalyzed by new oxamate-containing palladium(II) complexes in ionic liquids

Abstract New and versatile bis(oxamato)palladate(II) complexes of formula ( n -Bu 4 N) 2 [Pd(2-Mepma) 2 ]·4H 2 O ( 1a ) and ( n -Bu 4 N) 2 [Pd(4-Mepma) 2 ]·2H 2 O·MeCN ( 1b ) ( n -Bu 4 N +  = tetra- n -buthylammonium, 2-Mepma =  N -2-methylphenyloxamate and 4-Mepma =  N -4-methylphenyloxamate) have been synthesized and characterized by spectroscopic methods and single crystal X-ray diffraction. Each palladium(II) ion in 1a and 1b is four-coordinate with two oxygen and two nitrogen atoms from two fully deprotonated oxamate ligands building a centrosymmetric square planar surrounding. Their catalytic role has been investigated for both Heck and Suzuki coupling reactions using a series of aryl…

Syntheses, Crystal Structures, and Magnetic Properties of the Oxalato-Bridged Mixed-Valence Complexes [FeII(bpm)3]2[FeIII2(ox)5]·8H2O and FeII(bpm)3Na(H2O)2Fe(ox)3·4H2O (bpm = 2,2‘-Bipyrimidine)

The preparation and crystal structures of two oxalato-bridged FeII-FeIII mixed-valence compounds, [FeII(bpm)3]2[FeIII2(ox)5].8H2O (1) and FeII(bpm)3Na(H2O)2FeIII(ox)(3).4H2O (2) (bpm = 2,2'-bipyrimidine; ox = oxalate dianion) are reported here. Complex 1 crystallizes in the triclinic system, space group P1, with a = 10.998(2) A, b = 13.073(3) A, c = 13.308(3) A, alpha = 101.95(2) degrees, beta = 109.20(2) degrees, gamma = 99.89(2) degrees, and Z = 1. Complex 2 crystallizes in the monoclinic system, space group P2(1)/c, with a = 12.609(2) A, b = 19.670(5) A, c = 15.843(3) A, beta = 99.46(1) degrees, and Z = 4. The structure of complex 1 consists of centrosymmetric oxalato-bridged dinuclear h…

Structural insight into the reaction mechanism of Pd-catalyzed nitrile hydration: Trapping the [Pd(H2O)4]2+ cation through a supramolecular complex

Abstract Four new bis(oxamato)palladate(II) complexes of formula (n-Bu4N)2[Pd(2,4,6-Me3pma)2]·2CH3CN (1), (n-Bu4N)2[Pd(2,4,6-Me3pma)2]·2CH3CONH2 (2) and (n-Bu4N)4[Pd(H2O)4][Pd(4-Xpma)2]3·2CH3CONH2 with X = Br (3) and Cl (4) (2,4,6-Me3pma = N-2,4,6-trimethylphenyloxamate, 4-Brpma = N-4-bromophenyloxamate, N-4-chlorophenyloxamate and n-Bu4N+ = tetra-n-butylammonium) have been obtained and characterized by single crystal X-ray diffraction. All of them contain bis(oxamato)palladate(II) anions and bulky n-Bu4N+ cations, but compounds 3 and 4 have also the out of the ordinary [Pd(H2O)4]2+ inorganic cation. Acetonitrile and appealing acetamide are present as lattice molecules in compounds (1) and …

Synthesis, crystal structure and magnetic properties of novel heterobimetallic malonate-bridged MIIReIV complexes (M = Mn, Fe, Co and Ni).

Five novel ReIV-MII bimetallic complexes of formula [ReCl4(mu-mal)M(dmphen)2].MeCN [M = Co (1), Fe (2) and Ni (3)], [ReCl4(mu-mal)Ni(dmphen)(MeCN)2(H2O)].(MeCN)0.5(H2O)0.5 (4), and [ReCl4(mu-mal)Mn(dmphen)(H2O)2].dmphen.MeCN.H2O (5) (mal = malonate dianion, dmphen = 2,9-dimethyl-1,10-phenanthroline) have been synthesized, and the structures of 1, 2, 4, and 5 determined by single-crystal X-ray diffraction. The structures of 1 and 2 consist of neutral [ReCl4(mu-mal)M(dmphen)2] dinuclear units where the metal ions are linked through a malonate ligand which adopts simultaneously the bidentate (at ReIV) and monodentate (at MII) coordination modes. The bridging carboxylate-malonate group in them …

Rhenium(IV) cyanate complexes: Synthesis, crystal structures and magnetic properties of NBu4[ReBr4(OCN)(DMF)] and (NBu4)2[ReBr(OCN)2(NCO)3]

Abstract Two new rhenium(IV) mononuclear compounds of formula NBu4[ReBr4(OCN)(DMF)] (1) and (NBu4)2[ReBr(OCN)2(NCO)3] (2) (NBu4 = tetrabutylammonium cation, OCN = O-bonded cyanate anion, NCO = N-bonded cyanate anion and DMF = N,N-dimethylformamide) have been synthesized and their crystal structures determined by single-crystal X-ray diffraction. 1 crystallizes in the monoclinic system with the space group P21/n, whereas 2 crystallizes in the triclinic one with P 1 ¯ as space group. In both complexes the rhenium atom is six-coordinated, in 1 by four Br atoms in the equatorial plane, and two trans-oxygen atoms, one of a DMF molecule and another one from a cyanato group, while in 2 by one brom…

Synthesis and crystal structure of the low-spin iron(II) complex [Fe(bpym)3](ClO4)2·1/4H2O (bpym=2,2′-bipyrimidine)

Abstract Single crystals of the mononuclear iron(II) complex of formula [Fe(bpym)3](ClO4)2·1/4H2O (bpym=2,2′-bipyrimidine) have been prepared and characterized crystallographically. The complex is monoclinic, P21/c, a=13.688(5), b=19.391(6), c=11.554(5) A, β=102.22(3)°, V=2997(2) A3, Z=4, R=0.063 and Rw=0.068. The structure analysis reveals a distorted octahedral geometry around the iron atom. The average Fe–N bond length and N–Fe–N bidentate angle are 1.970(5) A and 81.0(1)°, respectively. The value of the Fe–N distance and that of the room temperature magnetic moment are in agreement with its singlet 1A1 ground state.

Magneto-structural diversity of Co(ii) compounds with 1-benzylimidazole induced by linear pseudohalide coligands

We report the preparation, spectroscopic characterisation, crystal structure determination and cryomagnetic investigation of three cobalt(II) complexes of formula trans-[Co(bim)4(NCS)2] (1), [Co(bim)2(NCO)2] (2) and [Co(bim)2(N3)2]n (3) (bim = 1-benzylimidazole). The structure of 1 is made up of neutral [Co(bim)4(NCS)2] mononuclear units, where the cobalt(II) ion is six-coordinate with four monodentate bim ligands in equatorial positions and two N-thiocyanato groups in the axial sites building a slightly compressed octahedron. In contrast to 1, each cobalt(II) ion in 2 is four-coordinate with two imidazole-nitrogen atoms from two bim molecules and two N-cyanato ligands describing a slightly…

Strukturelle und magnetische Charakterisierung eines neuen, siebenkernigen Hydroxo-verbrückten Kupfer(II)-Clusters mit einem Zentralgerüst aus zwei eckenverknüpften Würfeln

TTF charge transfer salts containing cyanometallate anions [M(phen)(CN)4]− (M=Cr or Fe; phen=1,10-phenanthroline)

Abstract Two new charge transfer salts of TTF with the counter anions [M(phen)(CN) 4 ] − (phen = 1,10-phenanthroline, M = Cr ( I ) and Fe ( II )) are described. The structures consist of alternating stacks of dimerised TTF + cations and [M(phen)(CN) 4 ] − anions and they are linked together by many short S⋯S contacts and hydrogen bonds. Within the organic stack, two dimerised TTF + cations are arranged in a slipped face-to-face mode with short intra-dimer and long inter-dimer S⋯S distances. Strong antiferromagnetic exchange was found in the TTF + dimers. Conductivity measurements show that compound I is a semiconductor.

Synthesis, Crystal Structure and Magnetic Properties of Three {Cr III Mn II } Heterodimetallic Complexes Based on Heteroleptic Cyanido‐Bearing Cr III Building Blocks

The use of the heteroleptic [CrIII(AA)(CN)4]- complex as a ligand towards the preformed [MnII(tptz)]2+ and [MnII(pyim)2]2+ species afforded the heterometallic compounds: [MnII(tptz)(H2O)(NO3)(-NC)CrIII(ampy)(CN)3]CH3CN (1), [MnII(tptz)(H2O)(NO3)(-NC)CrIII(phen)(CN)3]H2O (2) and {[MnII(pyim)2][(-NC)Cr(phen)(CN)3]2}3H2O (3) [AA = 2-aminomethylpyridine (ampy) and 1,10-phenanthroline (phen), tptz = 2,4,6-tris(2-pyridyl)-1,3,5-triazine and pyim = 2-(1H-imidazol-2-yl)pyridine]. 1 and 2 are neutral heterodinuclear complexes where a [CrIII(AA)(CN)4]- building block acts as a monodentate ligand through one cyanide group towards a seven coordinate MnII ion. Compound 3 is a neutral heterotrinuclear co…

[Criii(L)(CN)4]−: a new building block in designing cyanide-bridged 4,2-ribbon-like chains {[Criii(L)(CN)4]2Mn(H2O)2}·nH2O [L = 2-aminomethylpyridine (n = 6) and 1,10-phenanthroline (n = 4)]

The preparation, X-ray crystallography and magnetic study of compounds PPh4[Cr(ampy)(CN)4]·H2O (1), PPh4[Cr(phen)(CN)4]·H2O·CH3OH (2), {[Cr(ampy)(CN)4]2Mn(H2O)2}·6H2O (3) and {[Cr(phen)(CN)4]2Mn(H2O)2}·4H2O (4), with PPh4+ = tetraphenylphosphonium cation, ampy = 2-aminomethylpyridine and phen = 1,10-phenanthroline, are reported here. 1 and 2 are mononuclear complexes whereas 3 and 4 are 4,2-ribbon-like bimetallic chains. The magnetic properties of 1–4 were investigated in the temperature range 1.9–300 K. A quasi Curie law behaviour for a magnetically isolated spin quartet is observed for 1 and 2. Compounds 3 and 4 are ferrimagnetic CrIII2MnII chains, which exhibit a metamagnetic behaviour, …

Synthesis, spectroscopic characterization and electrochemical behaviour of nickel(II) complexes with C-meso-5,5,7,12,12,14-hexamethylcyclotetradecane (Me6[14]aneN4). Crystal structure of {Ni(Me6[14]aneN4)|I2

A series of complexes of formula {Ni(Me6[14]aneN4)X2| (Me6[14]aneN4) = C-meso-5,5,7,12,12,14-hexamethyl-1,4,-8,11-tetraazacyclotetradecane and X = N3(1), NCO (2), NCS (3), AcO (4) or I (5) has been synthesized. The crystal structure of (5) has been determined by X-ray diffraction methods. The nickel atom is surrounded by a square-planar array of nitrogen atoms, giving a low-spin complex. The macrocyclic ligand shows the most stable conformation, the six-membered rings exhibiting the chair form while the gauche conformation is adopted by the five-membered rings. Spectroscopic and magnetic data for (1)–(4) are consistent with octahedral coordination around the nickel atom, which is achieved b…

Two-Dimensional Coordination Polymers Constructed Using, Simultaneously, Linear and Angular Spacers and Cobalt(II) Nodes. New Examples of Networks of Single-Ion Magnets

Two novel bidimensional coordination polymers, [Co(azbbpy)(4,4'-bipy)0.5(DMF)(NCS)2]·MeOH (1) and [Co(azbbpy)(bpe)0.5(DMF)(NCS)2]·0.25H2O (2), resulted from the assembling of cobalt(II) ions by 1,3-bis(4-pyridyl)azulene, using either 4,4'-bipyridyl or 1,2-bis(4-pyridyl)ethylene as neutral spacers. The cobalt(II) nodes in 1 and 2 act as single-ion magnets (SIMs).

Towards multifunctional magnetic systems through molecular-programmed self assembly of Re(IV) metalloligands

Abstract The molecular-programmed approach based on the use as ligands of tailor-made metalloligands containing stable six-coordinate rhenium(IV) as paramagnetic centres is presented in this review article. A relatively large amount of spin density is covalent-delocalized away from the rhenium to the peripheral atoms of the ligands in the case of the Re(IV) metalloligands, as shown by polarized neutron diffraction experiments and density functional theory calculations. This feature accounts for the significant through space-magnetic interactions that occur in most of its mononuclear species and more interestingly it also explains the strengthening of the magnetic interactions in the heterom…

An Overview on the Performance of 1,2,3-Triazole Derivatives as Corrosion Inhibitors for Metal Surfaces

This review accounts for the most recent and significant research results from the literature on the design and synthesis of 1,2,3-triazole compounds and their usefulness as molecular well-defined corrosion inhibitors for steels, copper, iron, aluminum, and their alloys in several aggressive media. Of particular interest are the 1,4-disubstituted 1,2,3-triazole derivatives prepared in a regioselective manner under copper-catalyzed azide-alkyne cycloaddition (CuAAC) click reactions. They are easily and straightforwardly prepared compounds, non-toxic, environmentally friendly, and stable products to the hydrolysis under acidic conditions. Moreover, they have shown a good efficiency as corrosi…

New anionic cobalt complexes using highly hindered bis-amides with varying donor abilities as ligands.

Four potential tetradentate ligands of formulae 1,2-bis-(3,5-di-tert-butyl-2-hydroxybenzamido)ethane (H(4)L(1), 1), 1,2-bis-(3,5-di-tert-butyl-2-hydroxybenzamido)propane (H(4)L(2), 2), 1,2-bis-(3,5-di-tert-butyl-2-hydroxybenzamido)benzene (H(4)L(3), 3) and 1,8-bis-(3,5-di-tert-butyl-2-hydroxybenzamido)naphthalene (H(4)L(4), 4) have been prepared and the crystal structures of three of them (1, 3 and 4) determined by single crystal X-ray diffraction. The investigation of their complexing ability toward Co(II) afforded the compounds of formulae [Co(III)(L(3))Na(I)(H(2)O)(2)] (5), [Co(III)(L(n))Li(I)(H(2)O)2] with n = 1 (6), 2 (7) and 3 (8) and [Co(II)(L(4))Li(I)(2)] (9). Complexes 5-8 are squa…

Ordered mesoporous silicas as host for the incorporation and aggregation of octanuclear nickel(ii) single-molecule magnets: a bottom-up approach to new magnetic nanocomposite materials

Silica-based mesoporous materials have been employed as the support host for a suitably designed small octanuclear nickel(II) guest complex with a moderately anisotropic S = 4 ground spin state (D = −0.23 cm−1), which behaves as a single-molecule magnet at low temperature (TB = 3.0 K). Both unimodal MCM-41 and bimodal UVM-7 porous silica provide appropriate template conditions for the incorporation and aggregation of the Ni8 complex precursor into larger complex aggregates, showing slow relaxation of the magnetization at higher blocking temperatures than the crystalline material. By playing with the initial complex vs. silica concentration, two series of samples with varying complex loading…

Syntheses, crystal structures and magnetic properties of di- and trinuclear croconato-bridged copper(ii) complexes

The new croconato-bridged copper(II) compounds [Cu2(terpy)2(H2O)2(C5O5)](NO3)2·H2O (1) and [Cu3(phen)5(C5O5)2](CF3SO3)2 (2) (C5O52− = croconate, dianion of 4,5-dihydroxycyclopent-4-ene-1,2,3-trione; terpy = 2,2′:6′,2″-terpyridine; phen = 1,10-phenanthroline) have been prepared, and their crystal structures and variable temperature magnetic susceptibilities determined. The structure of complex 1 consists of croconato-bridged dinuclear [Cu2(terpy)2(H2O)2(C5O5)]2+ complex ions, nitrate counter ions and water of hydration. The croconato ligand exhibits an asymmetrical bis-bidentate coordination mode through four of its five oxygen atoms. The two crystallographically independent copper atoms hav…

Synthesis, Crystal Structure, and Magnetic Properties of an Octanuclear Nickel(II) Complex with ahexahedro-Ni8 Core

Structural, photophysical and magnetic properties of transition metal complexes based on the dipicolylamino-chloro-1,2,4,5-tetrazine ligand

International audience; The ligand 3-chloro-6-dipicolylamino-1,2,4,5-tetrazine (Cl-TTZ-dipica) 1, prepared by the direct reaction between 3,6-dichloro-1,2,4,5-tetrazine and di(2-picolyl)-amine, afforded a series of four neutral transition metal complexes formulated as [Cl-TTZ-dipica-MCl2]2, with M = Zn(II), Cd(II), Mn(II) and Co(II), when reacted with the corresponding metal chlorides. The dinuclear structure of the isostructural complexes was disclosed by single crystal X-ray analysis, clearly indicating the formation of [MII–(μ-Cl)2MII] motifs and the involvement of the amino nitrogen atom in semi-coordination with the metal centers, thus leading to distorted octahedral coordination geome…

Long-distance magnetic coupling in dinuclear copper(II) complexes with oligo-para-phenylenediamine bridging ligands

Abstract Two novel dinuclear copper(II) complexes of formulae [Cu2(tren)2(bpda)](ClO4)4 (2) and [Cu2(tren)2(tpda)](ClO4)4 (3) containing the tripodal tris(2-aminoethyl)amine (tren) terminal ligand and the 4,4′-biphenylenediamine (bpda) and 4,4″-p-terphenylenediamine (tpda) bridging ligands have been synthesized and structurally, spectroscopically, and magnetically characterized. Their experimentally available electronic spectroscopic and magnetic properties have been reasonably reproduced by DFT and TDDFT calculations. Single crystal X-ray diffraction analysis of 2 shows the presence of dicopper(II) cations where the bpda bridging ligand adopts a bismonodentate coordination mode toward two …

Two-Dimensional 3d–4f Heterometallic Coordination Polymers: Syntheses, Crystal Structures, and Magnetic Properties of Six New Co(II)–Ln(III) Compounds

Six new heterometallic cobalt(II)-lanthanide(III) complexes of formulas [Ln(bta)(H2O)2]2[Co(H2O) 6]·10H2O [Ln = Nd(III) (1) and Eu(III) (2)] and [Ln2Co(bta)2(H2O)8] n·6nH2O [Ln = Eu(III) (3), Sm(III) (4), Gd(III) (5), and Tb(III) (6)] (H4bta = 1,2,4,5-benzenetretracaboxylic acid) have been synthesized and characterized via single-crystal X-ray diffraction. 1 and 2 are isostructural compounds with a structure composed of anionic layers of [Ln(bta)(H2O)2]n n- sandwiching mononuclear [Co(H2O)6]2+ cations plus crystallization water molecules, which are interlinked by electrostatic forces and hydrogen bonds, leading to a supramolecular three-dimensional network. 3-6 are also isostructural compou…

Syntheses, crystal structures and magnetic properties of new oxalato-, croconato- and squarato-containing copper(ii) complexesElectronic supplementary information (ESI) available: Stereoview of the structure of compound 2 (Fig. S1) and X-ray data as described in the text. See http://www.rsc.org/suppdata/nj/b3/b301212n/

The preparation and magnetic investigation of five mononuclear copper(II) complexes of formula [Cu(pyim)(C2O4)(H2O)]·2H2O (1), [Cu(pyim)(C4O4)(H2O)2]·2H2O (2), Cu(pyim)(C5O5)·2.5H2O (3), [Cu(H2bim)(C2O4)(H2O)]·H2O (4) and [Cu(bpz)(C5O5)(H2O)] (5) [pyim=2-(2-pyridyl)imidazole, H2bim=2,2′-biimidazole, bpz=2,2′-bipyrazine, C2O42−=dianion of oxalic acid, C4O42−=dianion of squaric acid and C5O52−=dianion of croconic acid] are reported. The crystal structures of 1, 2, 4 and 5 have been determined. The copper atom has a distorted square pyramidal geometry in this family of complexes: two nitrogen atoms from the bidentate nitrogen donor [pyim (1 and 2), H2bim (4) and bpz (5)] and two oxygen atoms e…

Crystal structures and magnetic properties of two- and three-dimensional malonato-bridged manganese(ii) complexes

Two new manganese(II) compounds of formula [Mn(mal)(H2O)(2,4′-bpy)]n (1) and [Mn2(mal)2(H2O)2(4,4′-bpy)]n (2) (2,4′-bpy = 2,4′-bipyridine, 4,4′-bpy = 4,4′-bipyridine and H2mal = malonic acid) have been prepared and structurally characterized by X-ray crystallography. Their structures are made up of two- (1) and three-dimensional (2) arrangements of manganese atoms linked by carboxylate-malonate groups in the anti–syn bridging mode (1 and 2) and bis(monodentate) 4,4′-bpy (2). The 2,4′-bpy group in 1 acts as a monodentate ligand. Each manganese atom in 1 and 2 is six-coordinated with four carboxylate-oxygens in the equatorial plane and a nitrogen atom and a water molecule in the axial positio…

Alternating Ferro- and Antiferromagnetic Interactions in a Chainlike CuII Coordination Polymer

Heterobimetallicd—f Metal Complexes as Potential Single-Source Precursors for MOCVD: Structure and Thermodynamic Study of the Sublimation of [Ni(salen)Ln(hfa)3], Ln = Y, Gd

Heterobimetallic [Ni(salen)Ln(hfa)3] species [H2salen and Hhfa being N,N′-ethylenebis(salicylideneimine) and hexa-fluoroacetylacetone respectively], where Ni(salen) acts as a neutral chelating ligand towards LnIII, form a series of isostructural compounds for Ln = YIII and any lanthanideIII cation from La to Yb. They are also isostructural with some of the [Cu(salen)Ln(hfa)3] compounds. They sublime without decomposition under vacuum which makes them potential single-source precursors in MOCVD. Sublimation, thermal behaviour, pressure and composition of the vapour phase versus temperature have been studied for the yttrium derivative, by means of thermal analyses, and mass spectrometry using…

Dicopper(II) pyrazolenophanes: Ligand effects on their structures and magnetic properties

Abstract The use of simple pyrazolate anions and related polychelating acyclic or macrocyclic pyrazolate derivatives as bridging ligands, and occasionally additional blocking ligands, has led to the stereospecific Cu II -mediated self-assembly of both homo- and heteroleptic di-μ-pyrazolatodicopper(II) complexes of the metallacyclophane type, so-called dicopper(II) pyrazolenophanes. Besides their unique molecular conformation features and binding abilities toward both neutral molecules and charged anionic species, which have illustrated the putative role of weak intramolecular π–π stacking, hydrogen bonding, and coordinative interactions in the self-assembling process, dicopper(II) pyrazolen…

Ligand design for multidimensional magnetic materials: a metallosupramolecular perspective.

The aim and scope of this review is to show the general validity of the ‘complex-as-ligand’ approach for the rational design of metallosupramolecular assemblies of increasing structural and magnetic complexity. This is illustrated herein on the basis of our recent studies on oxamato complexes with transition metal ions looking for the limits of the research avenue opened by Kahn's pioneering research twenty years ago. The use as building blocks of mono-, di- and trinuclear metal complexes with a novel family of aromatic polyoxamato ligands allowed us to move further in the coordination chemistry-based approach to high-nuclearity coordination compounds and high-dimensionality coordination po…

Copper(II) complexes with 2,5-bis(2-pyridyl)pyrazine and 1,1,3,3-tetracyano-2-ethoxypropenide anion: Syntheses, crystal structures and magnetic properties

International audience; The copper(II) complexes of formula [Cu2(2,5-dpp)(H2O)4(CF3SO3)4] · 2H2O (1) and [Cu2(2,5-dpp)(H2O)2(tcnoet)4]n (2) [2,5-dpp = 2,5-bis(2-pyridyl)pyrazine and tcnoet− = 1,1,3,3-tetracyano-2-ethoxypropenide anion] have been prepared and their structures determined by X-ray crystallographic methods. Compound 1 is a dinuclear complex where the 2,5-dpp molecule acts as a bis-bidentate bridge between the two copper centers, the electroneutrality being achieved by four terminally bound triflate anions. Each copper(II) ion presents an elongated octahedral CuN2O4 environment with two nitrogen atoms from 2,5-dpp and two water molecules in the basal plane and two triflate-oxyge…

Synthesis, crystal structure and magnetic properties of a new cyanide-bridged mixed-valence copper(I)/copper(II) clathrate

A unique cyanide-bridge mixed-valence CuI/CuII clathrate of formula [CuI2(CN)3][{CuII(tren)}2(μ-CN)](CF3SO3)2 [tren = tris(2-aminoethyl)amine] containing cyanide-bridged [{CuII(tren)}2(μ-CN)]3 + binuclear cations stacked between anionic honeycomb layered copper(I) cyanide networks, was synthesized and structurally characterized by single crystal X-ray diffraction. Variable-temperature magnetic susceptibility studies showed that the cyanide bridge mediates a strong antiferromagnetic interaction between the copper(II) centers (J = − 160 cm− 1, the spin Hamiltonian being defined as H = − JSA⋅SB).

Charge transfer salts containing a paramagnetic cyano-complex and iodine substituted organic donor involving –I(donor)···N(anion)-interactions

Abstract The preparation, crystal structures, EHT band calculation and optical properties of two new charge transfer salts, namely (DIET)2[Fe(bpca)(CN)3] (1) and (DIEDO)2[Fe(bpca)(CN)3] (2), where bpca = bis(2-pyridylcarbonyl)amide anion, DIET = diiodoethylenedithotetrathiavalene and DIEDO = diiodoethylenedioxotetrathiavalene are reported. The magnetic properties of 2 and those of the low-spin iron(III) precursor of formula (PPh4)[Fe(bpca)(CN)3]·H2O (3) were also investigated in the temperature range 1.9–205 K. Crystal data; (1): monoclinic P21, a = 8.8238(2)A, b = 13.2891(3) A, c = 18.5042(5) A, β = 91.115(1)°, Z = 2, R = 0.0710 for 7021 independent reflections with I > 2 σ(I) and (2): Mon…

Exploring the biological, catalytic, and magnetic properties of transition metal coordination complexes incorporating pyrophosphate

Abstract Polyphosphate anions are ubiquitous in nature, none more so than the diphosphate tetra-anion P2O74−, commonly referred to as pyrophosphate (PPi). The past decade has seen a rise in the number of pyrophosphate coordination complexes synthesized and characterized, and the areas of research interest expanded to include magnetic, medicinal, nutraceutical, catalytic and bioinorganic. The aim of the present review is to collect and organize the multidisciplinary information of the inorganic pyrophosphate system paying special attention to the following points: (i) the structural diversity of the PPi-containing metal complexes from discrete species to coordination polymers, which is due t…

Cd(II) and Cu(II) coordination polymers constructed from the expanded 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene ligand: conventional and ultrasound-assisted synthesis, crystal structure, luminescence and magnetic properties

Shaabani, Behrouz/0000-0001-5576-4604; Kubicki, Maciej/0000-0001-7202-9169; Grzeskiewicz, Anita M./0000-0003-0377-2260 WOS: 000447971700041 A 3D open inorganic/organic framework, {[Cd(mu-L)(mu(3)-SO4)(H2O)]center dot H2O}(n) (1) [L = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene] was synthesized by the reaction of CdSO4 center dot 8H(2)O with L. The treatment of Cu(NO3)(2)center dot 3H(2)O with the same N,N'-donor ligand in two different solvent mixtures, methanol/ dichloromethane (2) and methanol/ chloroform (3), afforded two new ladder-like coordination polymers of formula {[Cu(mu-L)(mu-NO3)(NO3)]center dot solv}(n) [solv = CH2Cl2 (2) and CHCl3 (3)]. The non-interpenetrated ladder motifs 2 a…

Influence of the alkaline earth cations on the topology of MII/CuII mixed-metal-organic frameworks (M = Ca, Sr and Ba)

The use of the mononuclear copper(ii) complex, [Cu II(Me 2pma) 2] 2- (Me 2pma = N-2,6-dimethylphenyloxamate), as a bis(bidentate) metalloligand toward solvated alkaline earth metal cations affords a new series of oxamato-bridged heterobimetallic two-dimensional compounds with mixed square-octagonal [Ca II 2Cu II 3] or square [M II 2Cu II 3] (M = Sr and Ba) layered structures of (4·82) and (44·62) net topologies, respectively. © 2012 The Royal Society of Chemistry.

Syntheses, crystal structures and magnetic properties of copper(ii) dicyanamide complexes; dinuclear, chain and ladder compounds

The preparation, crystal structures and magnetic properties of three heteroleptic copper(II) complexes with dicyanamide (dca) bridges, [Cu(bpca)(H2O)(dca)]2 (1) (bpca = bis(2-pyridylcarbonyl)amidate), [Cu(bpy)(dca)2]n (2) (bpy = 2,2′-bipyridine), [Cu2(bpm)(dca)4]n (3) (bpm = 2,2′-bipyrimidine) are reported. In addition, magnetic susceptibility measurements of the sheetlike polymer [Cu(phen)(dca)2] (4) (phen = 1,10-phenanthroline), structurally characterized previously, have been performed. In complex 1 pairs of mononuclear structural building blocks, [Cu(bpca)(dca)(H2O)], are loosely connected through a 1,3-dca bridge in which nitrile is equatorially bound and the amide is semi-coordinated …

[W(bipy)(CN)6]−: A Suitable Metalloligand in the Design of Heterotrimetallic Complexes. The First CuIILnIIIWV Trinuclear Complexes

The first 3d-4f-5d heterotrimetallic complexes using [W(V)(bipy)(CN)(6)](-) as a metalloligand were synthesized (bipy = 2,2'-bipyridine). The structural and magnetic properties of three [Cu(II)Ln(III)W(V)] complexes (Ln = Gd, Ho, Tb) are discussed.

Bis(N-substituted oxamate)palladate(ii) complexes as effective catalysts for sustainable Heck carbon–carbon coupling reactions in n-Bu4NBr as the solvent

Five bis(oxamato)palladate(II) complexes of the formulae (n-Bu4N)2[Pd(4-Fpma)2] (1), (n-Bu4N)2[Pd(4-Clpma)2] (2), (n-Bu4N)2[Pd(4-Brpma)2] (3), (n-Bu4N)2[Pd(4-Brpma)2]·H2O (3a), (n-Bu4N)2[Pd(4-MeOpma)2] (4) and (n-Bu4N)2[Pd(4-Isopma)2] (5) (n-Bu4N+ = tetra-n-butylammonium, 4-Fpma = N-4-fluorophenyloxamate, 4-Clpma = N-4-chlorophenyloxamate, 4-Brpma = N-4-bromophenyloxamate, 4-MeOpma = N-4-methoxyphenyloxamate and 4-isopma = N-4-isopropylphenyloxamate) have been easily prepared and characterized by spectroscopic methods and the crystal structures of two of them (3a and 4) have been determined by single crystal X-ray diffraction. Each palladium(II) ion in 3a and 4 is four-coordinate with two o…

Self-assembly and magnetic properties of a double-propeller octanuclear copper(II) complex with a meso-helicate-type metallacryptand core.

An octanuclear copper(II) complex possessing a dimer-of-tetramers structure self-assembles from a binuclear oxamatocopper(II) metallacryptand of the meso-helicate type; its magnetic behaviour is consistent with its unique double-propeller molecular topology. Pardo Marín, Emilio José, Emilio.Pardo@uv.es ; Julve Olcina, Miguel, Miguel.Julve@uv.es ; Lloret Pastor, Francisco, Francisco.Lloret@uv.es ; Ruiz Garcia, Rafael, Rafael.Ruiz@uv.es

[Cr(AA)(C2O4)2]− and [Cu(bpca)]+ as building blocks in designing new oxalato-bridged CrIIICuII compounds [AA=2,2′-bipyridine and 1,10-phenanthroline; bpca=bis(2-pyridylcarbonyl)amide anion]

Abstract The monouclear complex PPh4[Cr(bipy)(ox)2]·H2O (1) and the heterodinuclear compounds [Cu(bpca)(H2O)Cr(bipy)(ox)2]·2.5H2O (2) and [Cu(bpca)(H2O)Cr(phen)(ox)2]·2H2O (3) [PPh4+=tetraphenylphosphonium cation, bpca=bis(2-pyridylcarbonyl)amide anion, ox=oxalate dianion, bipy=2,2′-bipyridine and phen=1,10-phenanthroline] have been synthesized and characterized by single-crystal X-ray diffraction. Discrete [Cr(bipy)(ox)2]− mononuclear anions and tetraphenylphosphonium cations are present in 1 whereas the structures of 2 and 3 are made up neutral oxalato-bridged bimetallic CrIIICuII units. The chromium environment is distorted octahedral in the three complexes: two nitrogen atoms from a bi…

One-dimensional coordination polymers constructed from di- and trinuclear {3d–4f} tectons. A new useful spacer in crystal engineering: 1,3-bis(4-pyridyl)azulene

Four new heterometallic 3d–4f complexes have been obtained using bi- and trinuclear building blocks: 1∞[Ni(L1)Gd(NO3)3(azbbpy)]·CH3CN (1), [Zn(L1)Eu(NO3)3(azbbpy)]·H2O (2), 1∞[(CuL2)2Gd(NO3)2(dca)] 3 and 1∞[(NiL2)2Dy(H2O)4(oxy-bbz)]NO3·3H2O (4), [H2L1 = 1,3-propanediyl-bis(2-iminomethylene-6-methoxyphenol), H2L2 = 2,6-di(acetoacetyl)pyridine, azbbpy = 1,3-bis(4-pyridyl)azulene, dca− = dicyanamide anion, and oxy-bbz = the dianion of the 4,4′-oxy-bis(benzoic) acid]. 1 and 2 represent the first complexes containing 1,3-bis(4-pyridyl)azulene as a ligand. 1, 3, and 4 are one-dimensional coordination polymers constructed from heterometallic nodes connected by the exo-dentate ligands. Helical chai…

Syntheses, crystal structures and magnetic properties of chromato-, sulfato-, and oxalato-bridged dinuclear copper(II) complexes

Abstract Four dinuclear copper(II) complexes of formula [Cu2(bpca)2(H2O)3(CrO4)]·H2O (1), [Cu2(bpca)2(H2O)3(SO4)]·H2O (2), [Cu2(bpca)2(H2O)2(C2O4)]·2H2O (3), and [Cu2(bpca)2(C2O4)] (4) [bpca=bis(2-pyridylcarbonyl)amide anion] have been synthesized and their magnetic behavior has been investigated as a function of temperature. The structures of 1–3 have been determined by single-crystal X-ray diffraction, whereas the structure of 4 was already known. The structures of this family of complexes are made up of neutral chromateO1,O1′ (1), sulfateO1,O1′ (2) and oxalateO1,O2:O1′,O2′-bridged (3 and 4) dinuclear copper(II) units. The two copper atoms within the dinuclear unit of the isomorphous c…

Synthesis, crystal structure and magnetic properties of two-dimensional malonato-bridged cobalt(ii) and nickel(ii) compounds

Two isostructural malonato-bridged complexes of formula {[M(H2O)2][M(mal)2(H2O)2]}n [M = Co(II) (1), Ni(II) (2); H2mal = malonic acid] have been synthesised and characterized by X-ray diffraction. Their structure consists of corrugated layers of trans-diaquabismalonatemetalate(II) and trans-diaquametal(II) units bridged by carboxylate–malonate groups in the anti–syn conformation. Two crystallographycally independent metal atoms occur in 1 and 2. The malonate anion acts simultaneously as a bidentate and bis-monodentate ligand. Variable-temperature (1.9–295 K) magnetic susceptibility measurements indicate the occurrence of weak antiferro- (1) and ferromagnetic (2) interactions between the cob…

Trinuclear Nickel(II) and Cobalt(II) Complexes Constructed from Mannich–Schiff‐Base Ligands: Synthesis, Crystal Structures, and Magnetic Properties

Anion-Directed Self-Assembly of Unusual Discrete and One-Dimensional Copper(II) Complexes of 3,6-Bis(2′-pyridyl)pyridazine

The preparation and crystal structures of six new copper(II) compounds of formula [Cu(dppn)2(ClO4)]ClO4 (1), [Cu2(dppn)(OH)(ClO4)3(H2O)3]·H2O (2), [Cu2(dppn)2(H2O)2](ClO4)4 (3), [Cu2(dppn)2(ClO4)4] (4), {[Cu2(dppn)(N3)4]·H2O/[Cu2(dppn)(N3)4(H2O)]}n (5) and {[Cu2(dppn)(OH)(dca)3]·H2O}n (6) [dppn = 3,6-bis(2′-pyridyl)pyridazine and dca = dicyanamide] are reported. 1 is a mononuclear complex where two bidentate dppn molecules and a monodentate perchlorate build an intermediate square pyramidal/trigonal bipyramidal (sp/tbp) five-coordinate environment around the copper(II) ion, the overall positive charge being balanced by a free perchlorate anion. 2–4 are dinuclear complexes with either one (2…

A rare isostructural series of 3d–4f cyanido-bridged heterometallic squares obtained by assembling [FeIII{HB(pz)3}(CN)3]− and LnIII ions: synthesis, X-ray structure and cryomagnetic study

A new series of cyanido-bridged {FeIIILnIII}2 neutral molecular squares of general formula [Fe{HB(pz)3}(CN)(μ-CN)2Ln(NO3)2(pyim)(Ph3PO)]2·2CH3CN [Ln = Ce (1), Pr (2), Nd (3), Gd (4), Tb (5), Dy (6) and Er (7); {HB(pz)3}− = hydrotris(pyrazolyl)borate, pyim = 2-(1H-imidazol-2-yl)pyridine and Ph3PO = triphenylphosphine oxide] were obtained by reacting the low-spin [Fe{HB(pz)3}(CN)3]− species with the preformed [LnIII(pyim)(NO3)2(pyim)(Ph3PO)]+ complex anions (generated in situ by mixing the nitrate salt of each Ln(III) ion with pyim and Ph3PO molecules). Single-crystal X-ray diffraction studies show that 1–7 are isostructural compounds that crystallize in the triclinic P space group. Their cry…

Effects of electron donating/withdrawing groups in the 5-substituted-2-hydroxybenzaldehyde on the synthesis of neutral cubanes with a NiII4O4core: synthesis, crystal structures and magnetic properties

Two tetranuclear cubane-like nickel(II) complexes of formula [Ni4(CH3O)4(L1)4(CH3OH)4] (1) and [Ni4(CH3O)4(L2)4(CH3OH)4] (2) (HL1 = 2-hydroxybenzaldehyde and HL2 = 2-hydroxy-5-methylbenzaldehyde) have been prepared by the reaction of NiCl2·6H2O with methanolic solutions of HL1 and HL2 in the presence of triethylamine at room temperature. Complexes 1 and 2 have been characterized by elemental analyses, IR spectra and single-crystal X-ray diffraction. The X-ray crystal structure analysis revealed that 1 and 2 have a cubane-type structural topology with four Ni(II) ions and four methoxo-oxygen atoms regularly alternating at the corners. Each metal ion in 1 and 2 is six-coordinate in a distorte…

Holmium(III) Single-Ion Magnet for Cryomagnetic Refrigeration Based on an MRI Contrast Agent Derivative

The coexistence of field-induced blockage of the magnetization and significant magnetocaloric effects in the low-temperature region occurs in a mononuclear holmium(III) diethylenetriamine-N,N,N′,N″,N″-pentaacetate complex, whose gadolinium(III) analogue is a commercial MRI contrast agent. Both properties make it a suitable candidate for cryogenic magnetic refrigeration, thus enlarging the variety of applications of this simple class of multifunctional molecular nanomagnets.

A Metallacryptand-Based Manganese(II)–Cobalt(II) Ferrimagnet with a Three-Dimensional Honeycomb Open-Framework Architecture

Copper(II)-assisted hydrolysis of 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine (tpymt): syntheses, crystal structures and magnetic properties of [Cu(bpcam)(H2O)2]ClO4·3H2O, [Cu(bpcam)(H2O)2][Cu(bpcam)(H2O)(SO4)]·2H2O and [Cu2(bpcam)2(H2O)2(SO4)]·H2O [bpcam=bis(2-pyrimidylcarbonyl)amidate]

Abstract The reaction of the 2,4,6-tris(2-pyrimidyl)-1,3,5-triazine (tpymt) ligand with copper(II) perchlorate or sulfate in aqueous solution affords complexes [Cu(bpcam)(H2O)2]ClO4 · 3H2O (1), [Cu(bpcam)(H2O)2][Cu(bpcam)(H2O)(SO4)] · 2H2O (2) and [Cu2(bpcam)2(H2O)2(SO4)] · H2O (3) [bpcam = bis(2-pyrimidylcarbonyl)amidate], whose structures have been determined by single-crystal X-ray diffraction studies. Copper(II) promotes the hydrolysis of tpymt in mild conditions yielding the bpcam group which is present in the structures of 1–3 as a tridentate ligand. The structure of 1 consists of mononuclear [Cu(bpcam)(H2O)2]+ cations, uncoordinated perchlorate anions and water of crystallization. Th…

Magneto‐Structural Study of an Oxamato‐Bridged Pd II Co II Chain: X‐ray Crystallographic Evidence of a Single‐Crystal‐to‐Single‐Crystal Phase Transition

Two new mononuclear oxamato-containing palladium(II) complexes of formula K2[Pd(opba)]·2H2O (1) and (PPh4)2[Pd(opba)]·2H2O (2) and the heterodimetallic palladium(II)–cobalt(II) chain {[Co(H2O)2Pd(opba)]·dmso}n (3) [opba = 1,2-phenylenebis(oxamate), PPh4+ = tetraphenylphosphonium cation and dmso = dimethyl sulfoxide] have been prepared, and the structures of two of them (compounds 2 and 3) were determined by X-ray diffraction analysis of single crystals. The structure of 2 consists of discrete anions of [Pd(opba)2]2– and PPh4+ cations. Each PdII ion in 2 is surrounded by two oxamate nitrogen atoms and two carboxylate oxygen atoms in a square-planar surrounding. Compound 3 is a neutral chain …

Copper(I)‐chitin biopolymer based: An efficient and recyclable catalyst for click azide–alkyne cycloaddition reactions in water

Magneto-structural versatility of copper(II)-3-phenylpropionate coordination polymers with N-donor coligands.

A novel series of copper(II) coordination polymers [Cu2(O2CC8H9)4(pyz)]n (1), [Cu2(O2CC8H9)4(dps)]n (2), {[Cu(O2CC8H9)2(dps)(H2O)]·H2O}n (3), {[NaCu(O2CC8H9)2(bpm)(NO3)]·H2O}n (4), and [Cu4(O2CC8H9)6(OH)2(bpp)2]n (5) [O2CC8H9− = 3-phenylpropionate anion, pyz = pyrazine, dps = di(4-pyridyl)sulfide, bpm = 2,2′-bipyrimidine, and bpp = 1,3-bis(4-pyridyl)propane] have been synthesized and magneto-structurally investigated. Compounds 1 and 2 belong to a large group of copper(II) carboxylates where bis-monodentate pyz (1) and dps (2) ligands connect the paddle-wheel [CuII2(μ-O2CC8H9)4] units leading to alternating copper(II) chains. The structure of 3 consists of uniform chains of trans-[CuII(O2CC…

Three-dimensional bimetallic octacyanidometalates $[M^{IV}{(\mu-CN)_{4}Mn^{II}(H_{2}O)_2}_2 \cdot 4H_{2}O]_{n}$ (M=Nb,Mo,W) : synthesis, single-crystal X-ray diffraction and magnetism

Abstract We report the synthesis, the single-crystal X-ray crystallographic structures and the magnetic properties of three new isostructural cyanido-bridged networks: [M IV {(μ-CN) 4 Mn II (H 2 O) 2 } 2 ·4H 2 O] n [M IV  = Nb IV ( 1 ), Mo IV ( 2 ), W IV ( 3 )]. For compound 1 , the magnetic properties reveal a ferrimagnetic phase below 50 K. In contrast, compounds 2 and 3 show a paramagnetic behaviour with no magnetic ordering down to 2 K. The only electronic difference between the two kinds of compounds is the presence of two paired electrons on Mo IV ( 2 ) and W IV ( 3 ) (d 2 electronic configuration, S  = 0) with no possible exchange interactions with Mn II ions (d 5 electronic configur…

Hexachlororhenate(IV) salts of organic radical cations

Abstract The ionic salts ( p -rad) 2 [ReCl 6 ] ( 1 ) and ( m -rad) 2 [ReCl 6 ] ( 2 ) ( p / m -rad = 2-(4/3- N -methylpyridinium)-4,4,5,5-tetramethyl-4,5-dihydro-1 H -imidazol-1-oxyl-3- N -oxide) have been prepared and their crystal structures determined by single-crystal X-ray diffraction. The nitronyl nitroxide cations in compound 1 show a layered disposition, whereas the [ReCl 6 ] 2− units are placed between these layers. The nitronyl nitroxide cations in compound 2 adopt an hexagonal array but they do not result in layers. Bulk magnetic properties of 1 and 2 have been investigated in the temperature range 2–300 K. Both compounds show weak but significant intermolecular antiferromagnetic …

A Study of the Lack of Slow Magnetic Relaxation in Mononuclear Trigonal Bipyramidal Cobalt(II) Complexes

Solvothermal synthesis, crystal structure and magnetic properties of homometallic Co(II) and Cu(II) chains with double di(4-pyridyl)sulfide as bridges

Abstract Two new coordination polymers {[Co(μ-4,4′-dps)2(H2O)2](NO3)2·2(4,4′-dps)·4H2O}n (1) and {[Cu(μ-4,4′-dps)2(H2O)2](NO3)2·2H2O}n (2) [4,4′-dps = di(4-pyridyl)sulfide] have been synthesized by solvothermal reactions between the nitrate salts of cobalt(II) (1) and copper(II) (2) and the 4,4′-dps molecule. Compounds 1 and 2 have been characterized by elemental analysis, thermal analysis (TG/DTA), vibrational spectroscopy, single crystal X-ray diffraction analysis and variable-temperature magnetic measurements. Compounds 1 and 2 are cationic chain compounds of formula {[M(μ-4,4′-dps)2(H2O)2]n2n+ [M = Co(II) (1) and Cu(II) (2)] with double 4,4′-dps bridges, uncoordinated nitrate anions, an…

Cyanide-bridged Fe(III)–Co(II) bis double zigzag chains with a slow relaxation of the magnetisation

Reaction of [FeIII(bipy)(CN)4]¯ with fully solvated MII cations [M = Co (1) and Mn (2)] produces the isostructural bis double zigzag chains [[FeIII(bipy)(CN)4]2MII(H2O)]·MeCN·1/2H2O; 1 exhibits intrachain ferromagnetic and interchain antiferromagnetic couplings, slow magnetic relaxation and hysteresis effects. Luminita Marilena, Toma, Luminita.Toma@uv.es ; Lescouezec, Alain Francois Rodri, Alain.Lescouezec@uv.es ; Lloret Pastor, Francisco, Francisco.Lloret@uv.es ; Julve Olcina, Miguel, Miguel.Julve@uv.es

The construction of open GdIII metal–organic frameworks based on methanetriacetic acid: New objects with an old ligand

11 páginas, 11 figuras, 2 esquemas.-- et al.

Theoretical design of magnetic wires from acene and nanocorone derivatives

Theoretical calculations on a series of molecular models based on amino derivatives of linear and cycled acenes acting as organic linkers between two copper(ii) ions have shown a wire-like magnetic behaviour, so that the intermetallic magnetic communication does not vanish when the linker becomes larger due to its polyradical nature. Hence, these models can be considered as molecular magnetic wires, which can be used as active components for molecular spintronics, where the information transport is based on spin carriers instead of the more conventional charge transport. The nature of the spin ground state along these two series of models is governed by the topology of the organic linker, i…

CCDC 995944: Experimental Crystal Structure Determination

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CCDC 995946: Experimental Crystal Structure Determination

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CCDC 1049852: Experimental Crystal Structure Determination

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CCDC 1914220: Experimental Crystal Structure Determination

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CCDC 1024052: Experimental Crystal Structure Determination

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CCDC 2070862: Experimental Crystal Structure Determination

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CCDC 1582396: Experimental Crystal Structure Determination

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CCDC 1002975: Experimental Crystal Structure Determination

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CCDC 1580448: Experimental Crystal Structure Determination

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CCDC 1867353: Experimental Crystal Structure Determination

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CCDC 1016163: Experimental Crystal Structure Determination

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CCDC 1469224: Experimental Crystal Structure Determination

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CCDC 1402358: Experimental Crystal Structure Determination

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CCDC 1818142: Experimental Crystal Structure Determination

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CCDC 1049851: Experimental Crystal Structure Determination

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CCDC 1830425: Experimental Crystal Structure Determination

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CCDC 983736: Experimental Crystal Structure Determination

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CCDC 1520091: Experimental Crystal Structure Determination

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CCDC 1030505: Experimental Crystal Structure Determination

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CCDC 883430: Experimental Crystal Structure Determination

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CCDC 995943: Experimental Crystal Structure Determination

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CCDC 294297: Experimental Crystal Structure Determination

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CCDC 1969476: Experimental Crystal Structure Determination

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CCDC 1048365: Experimental Crystal Structure Determination

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CCDC 983489: Experimental Crystal Structure Determination

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CCDC 1482464: Experimental Crystal Structure Determination

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CCDC 1520092: Experimental Crystal Structure Determination

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CCDC 941373: Experimental Crystal Structure Determination

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CCDC 878930: Experimental Crystal Structure Determination

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CCDC 2089144: Experimental Crystal Structure Determination

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CCDC 1471985: Experimental Crystal Structure Determination

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CCDC 1992815: Experimental Crystal Structure Determination

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CCDC 1049500: Experimental Crystal Structure Determination

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CCDC 1025298: Experimental Crystal Structure Determination

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CCDC 1034456: Experimental Crystal Structure Determination

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CCDC 1055519: Experimental Crystal Structure Determination

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CCDC 1418715: Experimental Crystal Structure Determination

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CCDC 2096753: Experimental Crystal Structure Determination

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CCDC 902500: Experimental Crystal Structure Determination

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CCDC 294298: Experimental Crystal Structure Determination

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CCDC 1833100: Experimental Crystal Structure Determination

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CCDC 1898457: Experimental Crystal Structure Determination

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CCDC 1048366: Experimental Crystal Structure Determination

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CCDC 1580449: Experimental Crystal Structure Determination

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CCDC 1867830: Experimental Crystal Structure Determination

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CCDC 909392: Experimental Crystal Structure Determination

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CCDC 1833101: Experimental Crystal Structure Determination

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CCDC 1469225: Experimental Crystal Structure Determination

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CCDC 1049932: Experimental Crystal Structure Determination

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CCDC 1958348: Experimental Crystal Structure Determination

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CCDC 1898455: Experimental Crystal Structure Determination

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CCDC 958829: Experimental Crystal Structure Determination

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CCDC 1510396: Experimental Crystal Structure Determination

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CCDC 987581: Experimental Crystal Structure Determination

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CCDC 1047962: Experimental Crystal Structure Determination

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CCDC 958833: Experimental Crystal Structure Determination

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CCDC 995947: Experimental Crystal Structure Determination

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CCDC 984262: Experimental Crystal Structure Determination

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CCDC 1484384: Experimental Crystal Structure Determination

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CCDC 1957553: Experimental Crystal Structure Determination

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CCDC 1867829: Experimental Crystal Structure Determination

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CCDC 909388: Experimental Crystal Structure Determination

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CCDC 1843195: Experimental Crystal Structure Determination

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CCDC 1992813: Experimental Crystal Structure Determination

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CCDC 1830430: Experimental Crystal Structure Determination

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CCDC 1545085: Experimental Crystal Structure Determination

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CCDC 2044634: Experimental Crystal Structure Determination

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CCDC 1045096: Experimental Crystal Structure Determination

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CCDC 951253: Experimental Crystal Structure Determination

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CCDC 1843197: Experimental Crystal Structure Determination

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CCDC 1550041: Experimental Crystal Structure Determination

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CCDC 1989325: Experimental Crystal Structure Determination

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CCDC 1495414: Experimental Crystal Structure Determination

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CCDC 1049499: Experimental Crystal Structure Determination

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CCDC 1957556: Experimental Crystal Structure Determination

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CCDC 1471984: Experimental Crystal Structure Determination

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CCDC 1969477: Experimental Crystal Structure Determination

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CCDC 1030506: Experimental Crystal Structure Determination

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CCDC 958838: Experimental Crystal Structure Determination

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CCDC 883431: Experimental Crystal Structure Determination

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CCDC 919043: Experimental Crystal Structure Determination

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CCDC 992679: Experimental Crystal Structure Determination

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CCDC 1055523: Experimental Crystal Structure Determination

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CCDC 1055520: Experimental Crystal Structure Determination

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CCDC 2073773: Experimental Crystal Structure Determination

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CCDC 1049501: Experimental Crystal Structure Determination

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CCDC 1874222: Experimental Crystal Structure Determination

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CCDC 1580450: Experimental Crystal Structure Determination

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CCDC 1036871: Experimental Crystal Structure Determination

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CCDC 1529277: Experimental Crystal Structure Determination

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CCDC 995948: Experimental Crystal Structure Determination

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CCDC 1471982: Experimental Crystal Structure Determination

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CCDC 1449346: Experimental Crystal Structure Determination

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CCDC 987580: Experimental Crystal Structure Determination

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CCDC 1883575: Experimental Crystal Structure Determination

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CCDC 1025299: Experimental Crystal Structure Determination

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CCDC 923163: Experimental Crystal Structure Determination

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CCDC 1524200: Experimental Crystal Structure Determination

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CCDC 1907945: Experimental Crystal Structure Determination

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CCDC 1816300: Experimental Crystal Structure Determination

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CCDC 1557653: Experimental Crystal Structure Determination

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CCDC 989258: Experimental Crystal Structure Determination

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CCDC 1520974: Experimental Crystal Structure Determination

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CCDC 1969470: Experimental Crystal Structure Determination

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CCDC 1046978: Experimental Crystal Structure Determination

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CCDC 992678: Experimental Crystal Structure Determination

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CCDC 1049546: Experimental Crystal Structure Determination

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CCDC 1901771: Experimental Crystal Structure Determination

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CCDC 940301: Experimental Crystal Structure Determination

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CCDC 1582395: Experimental Crystal Structure Determination

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CCDC 996269: Experimental Crystal Structure Determination

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CCDC 2073771: Experimental Crystal Structure Determination

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CCDC 2070865: Experimental Crystal Structure Determination

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CCDC 996270: Experimental Crystal Structure Determination

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CCDC 2002706: Experimental Crystal Structure Determination

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CCDC 2096752: Experimental Crystal Structure Determination

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CCDC 989260: Experimental Crystal Structure Determination

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CCDC 1892383: Experimental Crystal Structure Determination

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CCDC 996271: Experimental Crystal Structure Determination

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CCDC 1567349: Experimental Crystal Structure Determination

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CCDC 1529275: Experimental Crystal Structure Determination

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CCDC 2002540: Experimental Crystal Structure Determination

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CCDC 1969471: Experimental Crystal Structure Determination

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CCDC 1545086: Experimental Crystal Structure Determination

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CCDC 1045094: Experimental Crystal Structure Determination

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CCDC 1432272: Experimental Crystal Structure Determination

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CCDC 937587: Experimental Crystal Structure Determination

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CCDC 1039720: Experimental Crystal Structure Determination

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CCDC 984263: Experimental Crystal Structure Determination

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CCDC 996274: Experimental Crystal Structure Determination

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CCDC 995949: Experimental Crystal Structure Determination

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CCDC 1945945: Experimental Crystal Structure Determination

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CCDC 1449347: Experimental Crystal Structure Determination

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CCDC 1510397: Experimental Crystal Structure Determination

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CCDC 1045095: Experimental Crystal Structure Determination

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CCDC 1039718: Experimental Crystal Structure Determination

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CCDC 1524159: Experimental Crystal Structure Determination

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CCDC 2073772: Experimental Crystal Structure Determination

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CCDC 1047964: Experimental Crystal Structure Determination

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CCDC 2011616: Experimental Crystal Structure Determination

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CCDC 1031230: Experimental Crystal Structure Determination

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CCDC 1550275: Experimental Crystal Structure Determination

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CCDC 1958349: Experimental Crystal Structure Determination

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CCDC 953096: Experimental Crystal Structure Determination

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CCDC 1574907: Experimental Crystal Structure Determination

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CCDC 2073774: Experimental Crystal Structure Determination

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CCDC 949950: Experimental Crystal Structure Determination

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CCDC 1049853: Experimental Crystal Structure Determination

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CCDC 951150: Experimental Crystal Structure Determination

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CCDC 1983533: Experimental Crystal Structure Determination

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CCDC 1402554: Experimental Crystal Structure Determination

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CCDC 1550272: Experimental Crystal Structure Determination

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CCDC 1039719: Experimental Crystal Structure Determination

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CCDC 937589: Experimental Crystal Structure Determination

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CCDC 1868872: Experimental Crystal Structure Determination

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CCDC 1550271: Experimental Crystal Structure Determination

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CCDC 1503662: Experimental Crystal Structure Determination

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CCDC 1530054: Experimental Crystal Structure Determination

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CCDC 1559171: Experimental Crystal Structure Determination

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CCDC 942308: Experimental Crystal Structure Determination

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CCDC 1402553: Experimental Crystal Structure Determination

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CCDC 1482465: Experimental Crystal Structure Determination

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CCDC 946980: Experimental Crystal Structure Determination

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CCDC 1054691: Experimental Crystal Structure Determination

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CCDC 1964202: Experimental Crystal Structure Determination

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CCDC 2011615: Experimental Crystal Structure Determination

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CCDC 1024053: Experimental Crystal Structure Determination

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CCDC 1056331: Experimental Crystal Structure Determination

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CCDC 984264: Experimental Crystal Structure Determination

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CCDC 1883574: Experimental Crystal Structure Determination

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CCDC 1063253: Experimental Crystal Structure Determination

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CCDC 1582397: Experimental Crystal Structure Determination

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CCDC 1047963: Experimental Crystal Structure Determination

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CCDC 989261: Experimental Crystal Structure Determination

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CCDC 958834: Experimental Crystal Structure Determination

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CCDC 949613: Experimental Crystal Structure Determination

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CCDC 1055521: Experimental Crystal Structure Determination

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CCDC 937590: Experimental Crystal Structure Determination

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CCDC 1045093: Experimental Crystal Structure Determination

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CCDC 958835: Experimental Crystal Structure Determination

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CCDC 1030504: Experimental Crystal Structure Determination

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CCDC 1431249: Experimental Crystal Structure Determination

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CCDC 1868871: Experimental Crystal Structure Determination

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CCDC 1857503: Experimental Crystal Structure Determination

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CCDC 1957555: Experimental Crystal Structure Determination

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CCDC 1469223: Experimental Crystal Structure Determination

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CCDC 1580311: Experimental Crystal Structure Determination

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CCDC 953476: Experimental Crystal Structure Determination

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CCDC 1454962: Experimental Crystal Structure Determination

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CCDC 953097: Experimental Crystal Structure Determination

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CCDC 1046977: Experimental Crystal Structure Determination

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CCDC 949949: Experimental Crystal Structure Determination

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CCDC 1819913: Experimental Crystal Structure Determination

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CCDC 1883576: Experimental Crystal Structure Determination

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CCDC 2072597: Experimental Crystal Structure Determination

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CCDC 1545087: Experimental Crystal Structure Determination

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CCDC 1469222: Experimental Crystal Structure Determination

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CCDC 1053439: Experimental Crystal Structure Determination

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CCDC 1029369: Experimental Crystal Structure Determination

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CCDC 2089145: Experimental Crystal Structure Determination

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CCDC 1550274: Experimental Crystal Structure Determination

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CCDC 1036537: Experimental Crystal Structure Determination

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CCDC 987579: Experimental Crystal Structure Determination

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CCDC 949948: Experimental Crystal Structure Determination

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CCDC 1580964: Experimental Crystal Structure Determination

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CCDC 902499: Experimental Crystal Structure Determination

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CCDC 1818144: Experimental Crystal Structure Determination

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CCDC 925074: Experimental Crystal Structure Determination

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CCDC 1901770: Experimental Crystal Structure Determination

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CCDC 1545088: Experimental Crystal Structure Determination

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CCDC 1484386: Experimental Crystal Structure Determination

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CCDC 1475076: Experimental Crystal Structure Determination

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CCDC 1867783: Experimental Crystal Structure Determination

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CCDC 927505: Experimental Crystal Structure Determination

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CCDC 1049497: Experimental Crystal Structure Determination

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CCDC 1818143: Experimental Crystal Structure Determination

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CCDC 1898454: Experimental Crystal Structure Determination

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CCDC 1034455: Experimental Crystal Structure Determination

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CCDC 1029370: Experimental Crystal Structure Determination

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CCDC 1977986: Experimental Crystal Structure Determination

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CCDC 937591: Experimental Crystal Structure Determination

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CCDC 1495415: Experimental Crystal Structure Determination

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CCDC 1018429: Experimental Crystal Structure Determination

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CCDC 1530055: Experimental Crystal Structure Determination

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CCDC 1567346: Experimental Crystal Structure Determination

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CCDC 912843: Experimental Crystal Structure Determination

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CCDC 958832: Experimental Crystal Structure Determination

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CCDC 1409933: Experimental Crystal Structure Determination

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CCDC 1408633: Experimental Crystal Structure Determination

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CCDC 1550042: Experimental Crystal Structure Determination

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CCDC 999841: Experimental Crystal Structure Determination

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CCDC 1957554: Experimental Crystal Structure Determination

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CCDC 1964204: Experimental Crystal Structure Determination

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CCDC 986670: Experimental Crystal Structure Determination

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CCDC 1049849: Experimental Crystal Structure Determination

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CCDC 1481782: Experimental Crystal Structure Determination

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CCDC 1503663: Experimental Crystal Structure Determination

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CCDC 1582340: Experimental Crystal Structure Determination

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CCDC 1993352: Experimental Crystal Structure Determination

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CCDC 1440699: Experimental Crystal Structure Determination

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CCDC 1408631: Experimental Crystal Structure Determination

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CCDC 1510399: Experimental Crystal Structure Determination

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CCDC 1400299: Experimental Crystal Structure Determination

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CCDC 2070864: Experimental Crystal Structure Determination

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CCDC 927507: Experimental Crystal Structure Determination

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CCDC 937588: Experimental Crystal Structure Determination

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CCDC 1529486: Experimental Crystal Structure Determination

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CCDC 1409935: Experimental Crystal Structure Determination

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CCDC 1520975: Experimental Crystal Structure Determination

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CCDC 2076621: Experimental Crystal Structure Determination

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CCDC 1992814: Experimental Crystal Structure Determination

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CCDC 1432273: Experimental Crystal Structure Determination

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CCDC 1585318: Experimental Crystal Structure Determination

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CCDC 294299: Experimental Crystal Structure Determination

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CCDC 942307: Experimental Crystal Structure Determination

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CCDC 1053438: Experimental Crystal Structure Determination

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CCDC 1047965: Experimental Crystal Structure Determination

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CCDC 1833099: Experimental Crystal Structure Determination

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CCDC 958831: Experimental Crystal Structure Determination

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CCDC 1901769: Experimental Crystal Structure Determination

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CCDC 1914219: Experimental Crystal Structure Determination

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CCDC 984260: Experimental Crystal Structure Determination

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CCDC 1054690: Experimental Crystal Structure Determination

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CCDC 1056333: Experimental Crystal Structure Determination

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CCDC 1011545: Experimental Crystal Structure Determination

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CCDC 1034458: Experimental Crystal Structure Determination

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CCDC 903521: Experimental Crystal Structure Determination

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CCDC 909389: Experimental Crystal Structure Determination

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CCDC 958836: Experimental Crystal Structure Determination

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CCDC 1830421: Experimental Crystal Structure Determination

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CCDC 1031229: Experimental Crystal Structure Determination

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CCDC 996272: Experimental Crystal Structure Determination

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CCDC 903522: Experimental Crystal Structure Determination

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CCDC 1964203: Experimental Crystal Structure Determination

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CCDC 1857501: Experimental Crystal Structure Determination

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CCDC 948414: Experimental Crystal Structure Determination

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CCDC 1049498: Experimental Crystal Structure Determination

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CCDC 927506: Experimental Crystal Structure Determination

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CCDC 1471986: Experimental Crystal Structure Determination

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CCDC 1567347: Experimental Crystal Structure Determination

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CCDC 931371: Experimental Crystal Structure Determination

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CCDC 891353: Experimental Crystal Structure Determination

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CCDC 989259: Experimental Crystal Structure Determination

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CCDC 143382: Experimental Crystal Structure Determination

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CCDC 1053437: Experimental Crystal Structure Determination

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CCDC 1530056: Experimental Crystal Structure Determination

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CCDC 1567348: Experimental Crystal Structure Determination

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CCDC 1469226: Experimental Crystal Structure Determination

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CCDC 1049850: Experimental Crystal Structure Determination

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CCDC 1901768: Experimental Crystal Structure Determination

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CCDC 1983534: Experimental Crystal Structure Determination

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CCDC 1046979: Experimental Crystal Structure Determination

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CCDC 1036873: Experimental Crystal Structure Determination

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CCDC 1969473: Experimental Crystal Structure Determination

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CCDC 952343: Experimental Crystal Structure Determination

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CCDC 883429: Experimental Crystal Structure Determination

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CCDC 903520: Experimental Crystal Structure Determination

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CCDC 909390: Experimental Crystal Structure Determination

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CCDC 2069070: Experimental Crystal Structure Determination

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CCDC 1409934: Experimental Crystal Structure Determination

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CCDC 1892384: Experimental Crystal Structure Determination

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CCDC 1816301: Experimental Crystal Structure Determination

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CCDC 983737: Experimental Crystal Structure Determination

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CCDC 1520973: Experimental Crystal Structure Determination

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CCDC 1403663: Experimental Crystal Structure Determination

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CCDC 1530805: Experimental Crystal Structure Determination

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CCDC 1557652: Experimental Crystal Structure Determination

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CCDC 984265: Experimental Crystal Structure Determination

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CCDC 1550273: Experimental Crystal Structure Determination

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CCDC 951875: Experimental Crystal Structure Determination

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CCDC 1559172: Experimental Crystal Structure Determination

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CCDC 1553972: Experimental Crystal Structure Determination

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CCDC 1867352: Experimental Crystal Structure Determination

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CCDC 903519: Experimental Crystal Structure Determination

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CCDC 1409932: Experimental Crystal Structure Determination

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CCDC 1484383: Experimental Crystal Structure Determination

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CCDC 1868873: Experimental Crystal Structure Determination

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CCDC 1495416: Experimental Crystal Structure Determination

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CCDC 1969472: Experimental Crystal Structure Determination

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CCDC 953098: Experimental Crystal Structure Determination

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CCDC 2054785: Experimental Crystal Structure Determination

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CCDC 925073: Experimental Crystal Structure Determination

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CCDC 1558468: Experimental Crystal Structure Determination

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CCDC 1958345: Experimental Crystal Structure Determination

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CCDC 1036872: Experimental Crystal Structure Determination

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CCDC 1945944: Experimental Crystal Structure Determination

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CCDC 1898456: Experimental Crystal Structure Determination

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CCDC 909391: Experimental Crystal Structure Determination

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CCDC 1553973: Experimental Crystal Structure Determination

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CCDC 1843194: Experimental Crystal Structure Determination

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CCDC 1574908: Experimental Crystal Structure Determination

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CCDC 1911272: Experimental Crystal Structure Determination

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CCDC 958837: Experimental Crystal Structure Determination

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CCDC 2070863: Experimental Crystal Structure Determination

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CCDC 949947: Experimental Crystal Structure Determination

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CCDC 992680: Experimental Crystal Structure Determination

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CCDC 1443218: Experimental Crystal Structure Determination

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CCDC 1857500: Experimental Crystal Structure Determination

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CCDC 995945: Experimental Crystal Structure Determination

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CCDC 1055522: Experimental Crystal Structure Determination

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CCDC 1524158: Experimental Crystal Structure Determination

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CCDC 1524157: Experimental Crystal Structure Determination

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CCDC 1867351: Experimental Crystal Structure Determination

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CCDC 1510395: Experimental Crystal Structure Determination

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CCDC 1557650: Experimental Crystal Structure Determination

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CCDC 1907944: Experimental Crystal Structure Determination

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CCDC 1510398: Experimental Crystal Structure Determination

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CCDC 996273: Experimental Crystal Structure Determination

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CCDC 1403662: Experimental Crystal Structure Determination

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CCDC 1440698: Experimental Crystal Structure Determination

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CCDC 1045097: Experimental Crystal Structure Determination

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CCDC 1036536: Experimental Crystal Structure Determination

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CCDC 923498: Experimental Crystal Structure Determination

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CCDC 2047766: Experimental Crystal Structure Determination

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CCDC 1557651: Experimental Crystal Structure Determination

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CCDC 931372: Experimental Crystal Structure Determination

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CCDC 1859198: Experimental Crystal Structure Determination

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CCDC 1577623: Experimental Crystal Structure Determination

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CCDC 1960115: Experimental Crystal Structure Determination

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CCDC 1892797: Experimental Crystal Structure Determination

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CCDC 911161: Experimental Crystal Structure Determination

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CCDC 984261: Experimental Crystal Structure Determination

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CCDC 1580963: Experimental Crystal Structure Determination

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CCDC 1495417: Experimental Crystal Structure Determination

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CCDC 921556: Experimental Crystal Structure Determination

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CCDC 1883577: Experimental Crystal Structure Determination

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CCDC 1957552: Experimental Crystal Structure Determination

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CCDC 2011617: Experimental Crystal Structure Determination

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CCDC 1529276: Experimental Crystal Structure Determination

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