0000000000067151
AUTHOR
Marius Andruh
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 …
Polynuclear copper(II) complexes with hexadentate Schiff base directed by the counter ion. Syntheses, crystal structures and magnetic properties
Abstract Four new complexes, [Cu 9 L 6 ( µ 3 -ClO 4 ) 2 ](ClO 4 ) 4 ·4CHCl 3 1 , [Cu 3 L 2 (H 2 O) 2 ](ClO 4 ) 2 ·3H 2 O 2 , [Cu 6 L 4 (N 3 ) 2 ](ClO 4 ) 2 3 and [Cu 2 L(CH 3 COO) 2 ] 4 , where H 2 L stands for the Schiff base N , N ′-bis[(2-hydroxybenzilideneamino)-propyl]-piperazine, were obtained and structurally characterized. Compounds 1 , 2 and 3 contain the Cu 3 L 2 2+ entities in which L 2− acts in an unsymmetrical mode with N 3 O donor set wrapped around marginal copper(II) and with the remained NO sets bound to the central copper ion. The marginal copper(II) ions are in distorted square pyramidal environment, whereas that of the central one is square planar. In 1 , the peripheral …
[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…
[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-…
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.
[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…
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…
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…
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…
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…
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…
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…
[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.…
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…
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…
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.
An original 1D Cu–Co heterometallic compound: synthesis, structure and magnetic properties
A novel heterobimetallic system, 1∞[LCuIICoII(NCS)2] (1), was obtained by reacting the neutral mononuclear complex [LCu] with cobalt(II) acetate in the presence of potassium thiocyanate (L is the dianion of the Schiff base resulting from the 2 ∶ 1 condensation of 3-methoxysalicylaldehyde with 1,3-propanediamine). The crystallographic investigation of 1 reveals a one-dimensional alternating zig-zag chain-like structure, made of dinuclear {LCuCo} units linked by thiocyanate bridges. The copper(II) ion is pentacoordinate to the N2O2 donor set of the Schiff base ligand in the basal plane, with the apical position occupied by the sulfur atom. The cobalt ion displays a strongly distorted (4 + 2) …
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…
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…
Aggregation of [Ln(12)(III)] clusters by the dianion of 3-formylsalicylic acid. Synthesis, crystal structures, magnetic and luminescence properties
Three isostrucutral dodecanuclear clusters with the general formula [Ln(12)(fsa)(12)(mu f(3)-OH)(12)(DMF)(12)]center dot nDMF (fsa(2-) is the dianion of 3-formylsalicylic acid; Ln = Eu 1, Gd 2, Dy 3) have been obtained from the reaction of fromylsalicyclic acid (H(2)fsa), tetrabutylammonium hydroxide and Ln(NO3)(3)center dot 6H(2)O in methanol/DMF. Their structure consists of four vertex-sharing heterocubanes. Each heterocubane unit is assembled from four Ln(III) ions, three mu(3)-OH groups and one mu(3)-oxygen atom arising from the fsa(2-) carboxylato group. The photophysical properties of the europium derivative investigated at both 300 and 80 K sustain a relative intense emission obtaine…
Magnetism in Heterobimetallic and Heterotrimetallic Chains Based on the Use of [W V (bipy)(CN) 6 ] – as a Metalloligand
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 …
Magnetic Molecular Rectangles Constructed from Functionalized Nitronyl‐Nitroxide Ligands and Lanthanide(III) Ions
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…
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.
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…
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.
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.
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…
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…
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…
New complexes of Ni(II) and Co(III) with a Schiff-base ligand derived from o -vanillin. Crystal structure, magnetic and catalytic properties of a dissymmetric binuclear nickel(II) complex
Abstract A binuclear complex, [Ni2L2(NO3)(H2O)(CH3CN)]ClO4·CH3CN (1), has been obtained using a Schiff-base ligand (HL) derived from o-vanillin and 4-(2-aminoethyl)morpholine. The crystal structure of 1 has been solved. Both Ni(II) ions are hexacoordinated, but they display different coordination spheres. The exchange interaction between the two nickel ions is antiferromagnetic (J = −7.9 ± 0.2 cm−1; H = −JS1S2), in line with the DFT calculations. Compound 1 has been tested as a catalyst in the epoxidation of various olefins. The reaction of the same ligand with a mixture of cobalt(II) perchlorate and nitrate affords a mononuclear Co(III) complex, [CoL2(H2O)]ClO4·CH3OH (2).
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)…
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).
[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.
[Cr(AA)(C2O4)2]− and [Cu(bpca)]+ as building blocks in designing new oxalato-bridged CrIIICuII 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 CrIIICuII 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…
Trinuclear Nickel(II) and Cobalt(II) Complexes Constructed from Mannich–Schiff‐Base Ligands: Synthesis, Crystal Structures, and Magnetic Properties
CCDC 995944: Experimental Crystal Structure Determination
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CCDC 995946: Experimental Crystal Structure Determination
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CCDC 1825561: Experimental Crystal Structure Determination
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CCDC 2044705: Experimental Crystal Structure Determination
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CCDC 1520091: Experimental Crystal Structure Determination
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CCDC 995943: 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 1049500: Experimental Crystal Structure Determination
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CCDC 1049932: Experimental Crystal Structure Determination
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CCDC 995947: Experimental Crystal Structure Determination
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CCDC 1957553: Experimental Crystal Structure Determination
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CCDC 2044634: Experimental Crystal Structure Determination
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CCDC 1550041: 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 1049501: Experimental Crystal Structure Determination
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CCDC 995948: Experimental Crystal Structure Determination
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CCDC 1049546: Experimental Crystal Structure Determination
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CCDC 940301: Experimental Crystal Structure Determination
Related Article: Alina S. Dinca, Julia Vallejo, Sergiu Shova, Francesc Lloret, Miguel Julve and Marius Andruh|2013|Polyhedron|65|238|doi:10.1016/j.poly.2013.08.049
CCDC 1892383: Experimental Crystal Structure Determination
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CCDC 995949: Experimental Crystal Structure Determination
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CCDC 1558560: 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 1825562: Experimental Crystal Structure Determination
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CCDC 949950: Experimental Crystal Structure Determination
Related Article: Adrian E. Ion, Simona Nica, Augustin M. Madalan, Catalin Maxim, Miguel Julve, Francesc Lloret, Marius Andruh|2014|CrystEngComm|16|319|doi:10.1039/C3CE41592A
CCDC 1558856: Experimental Crystal Structure Determination
Related Article: Ildiko Buta, Liliana Cseh, Carmen Cretu, Diana Aparaschivei, Catalin Maxim, Peter Lönnecke, Evamarie Hey-Hawkins, Nicolae Stanica, Eva Ohler, Eva Rentschler, Marius Andruh, Otilia Costisor|2017|Inorg.Chim.Acta|475|133|doi:10.1016/j.ica.2017.10.024
CCDC 1482465: Experimental Crystal Structure Determination
Related Article: Alina S. Dinca, Natalia Candu, Sergiu Shova, Francesc Lloret, Miguel Julve, Vasile I. Parvulescu, Marius Andruh|2016|RSC Advances|6|86569|doi:10.1039/C6RA18989J
CCDC 1957555: Experimental Crystal Structure Determination
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CCDC 1826839: Experimental Crystal Structure Determination
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CCDC 2010168: Experimental Crystal Structure Determination
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CCDC 953097: Experimental Crystal Structure Determination
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CCDC 949949: Experimental Crystal Structure Determination
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CCDC 1029369: Experimental Crystal Structure Determination
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CCDC 1558855: Experimental Crystal Structure Determination
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CCDC 949948: Experimental Crystal Structure Determination
Related Article: Adrian E. Ion, Simona Nica, Augustin M. Madalan, Catalin Maxim, Miguel Julve, Francesc Lloret, Marius Andruh|2014|CrystEngComm|16|319|doi:10.1039/C3CE41592A
CCDC 1580964: Experimental Crystal Structure Determination
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CCDC 1049497: Experimental Crystal Structure Determination
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CCDC 1029370: Experimental Crystal Structure Determination
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CCDC 2044706: Experimental Crystal Structure Determination
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CCDC 1550042: Experimental Crystal Structure Determination
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CCDC 1957554: Experimental Crystal Structure Determination
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CCDC 1582340: Experimental Crystal Structure Determination
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CCDC 1558561: Experimental Crystal Structure Determination
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CCDC 1839534: Experimental Crystal Structure Determination
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CCDC 1049498: Experimental Crystal Structure Determination
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CCDC 1892384: Experimental Crystal Structure Determination
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CCDC 2010169: Experimental Crystal Structure Determination
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CCDC 953098: Experimental Crystal Structure Determination
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CCDC 1574908: Experimental Crystal Structure Determination
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CCDC 949947: Experimental Crystal Structure Determination
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CCDC 2044707: Experimental Crystal Structure Determination
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CCDC 995945: Experimental Crystal Structure Determination
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CCDC 1580963: Experimental Crystal Structure Determination
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CCDC 1957552: Experimental Crystal Structure Determination
Related Article: Mihaela I. Mocanu, Andrei A. Patrascu, Mihaela Hillebrand, Sergiu Shova, Francesc Lloret, Miguel Julve, and Marius Andruh|2019|Eur.J.Inorg.Chem.|2019|4773|doi:10.1002/ejic.201901076
CCDC 1580965: Experimental Crystal Structure Determination
Related Article: Mihaela I. Mocanu, Sergiu Shova, Frances Lloret, Miguel Julve, Marius Andruh|2018|J.Coord.Chem.|71|693|doi:10.1080/00958972.2018.1434877
CCDC 1825560: Experimental Crystal Structure Determination
Related Article: Alina S. Dinca, Alexei Mindru, Diana Dragancea, Carmen Tiseanu, Sergiu Shova, Samuele Cornia, Luca M. Carrella, Eva Rentschler, Marco Affronte, Marius Andruh|2019|Dalton Trans.|48|1700|doi:10.1039/C8DT04602F