Enhancement of the Intermolecular Magnetic Exchange through Halogen···Halogen interactions in Bisadeninium Rhenium(IV) Salts

Two novel ReIV salts of general formula [H2ade]2[ReIVX6]X2·4H2O [H2ade2+ = 9H-adenine-1,7-diium; X = Cl(1) and Br(2)] have been synthesized and magneto-structurally characterized. 1 and 2 are isostructural salts that crystallize in the orthorhombic system with space group Fdd2. Both compounds are made up of discrete mononuclear [ReIVX6]2- and X- anions and doubly protonated adenine cations. The six-coordinate rhenium(IV) ion is bonded to six halide ligands [X = Cl (1) and Br (2)] in an octahedral geometry. Short intermolecular ReIV−X···X−ReIV interactions, as well as ReIV−X···H−N(H2ade) and ReIV−X···H−Ow hydrogen bonds, are present in the crystal lattice of 1 and 2. Magnetic suscep-tibility…

Hexakis(dimethylformamide)iron(II) complex cation in hexahalorhenate(IV)-based salts: synthesis, X-ray structure and magnetic properties

Two iron(II)-rhenium(IV) compounds of general formula [FeII(dmf)6][ReIVX6] [X = Cl (1) and Br (2); dmf = N,N-dimethylformamide] have been prepared and characterized. X-ray powder diffraction measurements on samples of 1 and 2 support the same structure for both systems. The crystal structure of 1 was determined by single-crystal X-ray diffraction. 1 crystallizes in the triclinic system with space group Pī. Each iron(II) is six-coordinate and bonded to six oxygens from six dmf molecules building a distorted octahedral environment. Rhenium(IV) is six-coordinate by six halide anions in an almost regular octahedral geometry. The magnetic properties were investigated from variable-temperature ma…

Water Dissociation of a Dinuclear Bis(3,5‐dimethylpyrazolyl)methane Copper(II) Complex: X‐ray Diffraction Structure, Magnetic Properties, and Characteristic Absorption of the (CuN 2 Cl 2 ) 2 Core

Halogen⋯halogen interactions in the self-assembly of one-dimensional 2,2′-bipyrimidine-based CuIIReIV systems

Two one-dimensional CuIIReIV coordination polymers of the general formula {[ReIVCl4(μ-bpym)CuIIX2]·solvent}n [where bpym = 2,2′-bipyrimidine, X = Cl (1) and Br (2), and solvent = H2O (1) and CHCl3 (2)] have been prepared and characterised structurally and magnetically. Both compounds crystallise in the monoclinic system with space groups P21/c (1) and P21/n (2). Each CuII ion is bonded to two cis nitrogen atoms from the bpym ligand and to four halogen atoms. Two of these halogen atoms are placed in the equatorial plane and the other two are filling the axial positions of the CuII ion, thus generating a distorted octahedral environment for this metal ion in 1 and 2. In both compounds, the Re…

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.

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.

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.

Molecular Self-Assembly in a Family of Oxo-Bridged Dinuclear Ruthenium(IV) Systems

A series of six novel RuIV compounds of formula (H2bpy)2[{RuCl5}2(μ-O)] (1), (PPh4)2[{RuCl4(H2O)}2(μ-O)]·4H2O (2), (PPh4)2[{RuCl4(MeCN)}2(μ-O)] (3), (PPh4)2[{RuCl4(dmf)}2(μ-O)] (4), (PPh4)2[{RuCl4(...

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.

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…

Spin state of a single-molecule magnet (SMM) creating long-range ordering on ferromagnetic layers of a magnetic tunnel junction – a Monte Carlo study

Paramagnetic single-molecule magnets (SMMs) interacting with the ferromagnetic electrodes of a magnetic tunnel junction (MTJ) produce a new system. The properties and future scope of new systems differ dramatically from the properties of isolated molecules and ferromagnets. However, it is unknown how far deep in the ferromagnetic electrode the impact of the paramagnetic molecule and ferromagnet interactions can travel for various levels of molecular spin states. Our prior experimental studies showed two types of paramagnetic SMMs, the hexanuclear Mn6 and octanuclear Fe–Ni molecular complexes, covalently bonded to ferromagnets produced unprecedented strong antiferromagnetic coupling between …

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…

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…

Field-induced slow relaxation of magnetisation in two one-dimensional homometallic dysprosium(iii) complexes based on alpha- and beta-amino acids.

Two one-dimensional dysprosium(III) complexes based on α-glycine (gly) and β-alanine (β-ala) amino acids, with the formula {[Dy2(gly)6(H2O)4](ClO4)6·5H2O}n (1) and {[Dy2(β-ala)6(H2O)4](ClO4)6·H2O}n (2), have been synthesised and characterised structurally and magnetically. Both compounds crystallise in the triclinic system with the space group P. In 1, two DyIII ions are eight-coordinate and bound to six oxygen atoms from six gly ligands and two oxygen atoms from two water molecules, showing different geometries (bicapped trigonal prism and square antiprism). In 2, two DyIII ions are nine-coordinate and bound to seven oxygen atoms from six β-ala ligands and two oxygen atoms from two water m…

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…

A [Cr2Ni] coordination polymer: slow relaxation of magnetization in quasi-one-dimensional ferromagnetic chains

The reaction of [Cr3IIIO(OAc)6(H2O)3]NO3·AcOH with 2-hydroxynaphthaldehyde, 2-amino-isobutyric acid and NiCl2·6H2O in MeOH, under basic and solvothermal conditions, led to the formation of the quasi-1D coordination polymer {[CrIII2NiII(L)4(MeOH)2]}n (where L = the dianion of the Schiff base between 2-hydroxynaphthaldehyde and 2-amino-isobutyric acid), which behaves as a ferromagnetic chain, displaying slow relaxation of magnetization.

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.

Pentachloro(pyrazine)rhenate(iv) complex as precursor of heterobimetallic pyrazine-containing ReIV2MII (M = Ni, Cu) species: synthesis, crystal structures and magnetic properties

Three novel Re(IV) mononuclear complexes of formulae NBu4[ReC15(pyz)] (1), NH2Me2[ReCl5(pyz)] (2) and NH4[ReCl5(pyz)].0.75H2O (3), (pyz being pyrazine; NBu4+ = tetra-n-butylammonium cation, NH2Me2+ = dimethylammonium cation and NH4+ = ammonium cation), were synthesized by ligand substitution reaction from [ReCl6]2- anion and pyrazine in N,N-dimethylformamide (DMF). In addition, two new heterobimetallic compounds, the salt namely [ReCl5(pyz)]2[Ni(cyclam)](4) (cyclam = 1,4,8,11-tetraazacyclotetradecane) and the heterotrinuclear [{ReCl5(mu-pyz)}2Cu(DMF)4] (5) complex, were prepared by using as precursor 1 and 3, respectively. Compounds 1-5 were characterized by single-crystal X-ray diffraction…

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…

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.

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

Field-induced slow relaxation of magnetisation in an anionic heterotetranuclear [ZnIIReIV3] system

The compound (NBu4)4[ZnII{ReIVCl4(μ-ox)}3] (1) [NBu4+ = tetra-n-butylammonium cation and ox2− = oxalate dianion] is the first example of an oxalato-bridged ZnII system coordinated to a 5d metal ion that exhibits slow relaxation of magnetisation.

Ligand substitution in cis-bis(acetonitrile)tetrachlororhenium(IV) complex with N,N-dimethylformamide and N,N-dimethylacetamide

Abstract The preparation, crystal structures, and magnetic properties of two novel mononuclear ReIV complexes of formula cis-[ReIVCl4(dmf)2] (1) and cis-[ReIVCl4(dma)2] (2) (dmf = N,N-dimethylformamide and dma = N,N-dimethylacetamide) have been studied. Both ReIV systems were synthesized through ligand substitution reactions from the cis-[ReIVCl4(MeCN)2] precursor, upon heating in the employed solvent. 1 and 2 crystallize in the monoclinic crystal system with space group C2/c. Each ReIV ion exhibits a distorted octahedral environment, being bonded by two oxygen atoms from two dmf (1) and dma (2) molecules and four chloride ions. In the crystal lattice of 1 and 2, the mononuclear ReIV comple…

Anion-Assisted Crystallization of a Novel Type of Rhenium(IV)-Based Salt

A novel rhenium(IV)–manganese(II) double salt of formula (NBu4)10[{ReCl4(ox)}3Mn]2[ReCl6] (1) (NBu4+ = tetra-n-butylammonium cation and ox2– = oxalate dianion) has been prepared through the simultaneous use of two different anionic ReIV complexes, namely, [ReCl4(ox)]2– and [ReCl6]2–, in the presence of MnII ion, the [ReCl6]2– anion playing a key role in the crystallization process. 1 has been magnetically characterized and its crystal structure determined by single-crystal X-ray diffraction. The study of the magnetic properties reveals the occurrence of intramolecular antiferromagnetic exchange between ReIV and MnII ions. Remarkably, 1 is the first reported example of ReIV salt based on two…

Detection of Hypoxanthine from Inosine and Unusual Hydrolysis of Immunosuppressive Drug Azathioprine through the Formation of a Diruthenium(III) System

Hypoxanthine (hpx) is an important molecule for both biochemistry research and biomedical applications. It is involved in several biological processes associated to energy and purine metabolism and has been proposed as a biomarker for a variety of disease states. Consequently, the discovery and development of systems suitable for the detection of hypoxanthine is pretty appealing in this research field. Thus, we have obtained a stable diruthenium (III) compound in its dehydrated and hydrated forms with formula [{Ru(&micro

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 …

Thioester-functionalised and oxime-based hexametallic manganese(iii) single-molecule magnets

Two novel hexametallic MnIII complexes of formulae [Mn6(μ3-O)2(H2N-sao)6(3-atpa)2(EtOH)6]·2EtOH·2H2O (1) and [Mn6(μ3-O)2(H2N-sao)6(6-atha)2(EtOH)6]·6EtOH (2) [H2N-saoH2 = salicylamidoxime, 3-hatpa = 3-(acetylthio)propionic acid, 6-hatha = 6-(acetylthio)hexanoic acid] have been synthesised by using thioester-carboxylate ligands and magnetostructurally characterised. 1 crystallises in the triclinic system with space group P and 2 crystallises in the monoclinic system with space group P21/c. The study of the dc and ac magnetic susceptibility reveals single-molecule magnet behaviour for both compounds with spin-ground states S = 12 and S = 4 for 1 and 2, respectively. Hence, 1 and 2 are new mem…

Exploring room-temperature transport of single-molecule magnet-based molecular spintronics devices using the magnetic tunnel junction as a device platform

A device architecture utilizing a single-molecule magnet (SMM) as a device element between two ferromagnetic electrodes may open vast opportunities to create novel molecular spintronics devices. Here, we report a method of connecting an SMM to the ferromagnetic electrodes. We utilized a nickel (Ni)–AlOx–Ni magnetic tunnel junction (MTJ) with the exposed side edges as a test bed. In the present work, we utilized an SMM with a hexanuclear [Mn6(μ3-O)2(H2N-sao)6(6-atha)2(EtOH)6] [H2N-saoH = salicylamidoxime, 6-atha = 6-acetylthiohexanoate] complex that is attached to alkane tethers terminated with thiols. These Mn-based molecules were electrochemically bonded between the two Ni electrodes of an…

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.

Hexabromorhenate(IV) salt of a trans-dioxorhenium(V) cation: X-ray structure and magnetic properties

Abstract A novel rhenium(IV)–rhenium(V) compound of formula NBu4[ReVO2(py)4][ReIVBr6] (1) (NBu4+ = tetra-n-butylammonium cation and py = pyridine) has been prepared and characterized. The crystal structure of 1 was determined by single crystal X-ray diffraction. 1 crystallizes in the monoclinic system with space group Cc. The rhenium(IV) ion is six-coordinate by six Br atoms [average value of the ReIV–Br bonds lengths being ca. 2.509(1) A], while rhenium(V) ion is six-coordinate by two axial oxo groups and four N atoms from four pyridine ligands [average values of the ReV O and ReV–N bonds lengths being ca. 1.77 and ca. 2.14 A, respectively]. The magnetic properties were investigated from s…

Magneto-structural study on a series of rhenium(IV) complexes containing biimH2, pyim and bipy ligands

Abstract Three rhenium(IV) mononuclear compounds of formulae [ReCl4(biimH2)] · 2DMF (1), [ReCl4(pyim)] · DMF (2) and [ReCl4(bipy)] (3) (biimH2 = 2,2′-biimidazole, pyim = 2-(2′-pyridyl)imidazole, bipy = 2,2′-bipyridine and DMF = N,N-dimethylformamide) have been prepared and characterized. The crystal structure of 2 was determined by single crystal X-ray diffraction. Compound 2 crystallizes in the monoclinic system with P21/c as space group. The rhenium atom is six-coordinated by four Cl atoms and two nitrogen atoms from a bidentate pyim ligand [average values of Re–Cl and Re–N bonds lengths being 2.330(2) and 2.117(4) A, respectively]. The magnetic properties were investigated from susceptib…

Aquapentachlororhenate(iv): a singular and promising building block for metal assembly

The novel ReIV compound of formula PPh4[ReIVCl5(H2O)] (1) is the first example of a ReIV compound containing a coordinated water molecule which has been magnetostructurally studied.

A Gadolinium(III) Complex Based on the Thymine Nucleobase with Properties Suitable for Magnetic Resonance Imaging

The paramagnetic gadolinium(III) ion is used as contrast agent in magnetic resonance (MR) imaging to improve the lesion detection and characterization. It generates a signal by changing the relaxivity of protons from associated water molecules and creates a clearer physical distinction between the molecule and the surrounding tissues. New gadolinium-based contrast agents displaying larger relaxivity values and specifically targeted might provide higher resolution and better functional images. We have synthesized the gadolinium(III) complex of formula [Gd(thy)2(H2O)6](ClO4)3·2H2O (1) [thy = 5-methyl-1H-pyrimidine-2,4-dione or thymine], which is the first reported compound based on gadolinium…

Synthesis, Crystal Structure, Magnetic Properties, and Theoretical Studies of [{Cu(mepirizole)Br}2(μ-OH)(μ-pz)] (Mepirizole = 4-Methoxy-2-(5-methoxy-3-methyl-1H-pyrazol-1-yl)-6-methylpyrimidine; pz = Pyrazolate), a Novel μ-Pyrazolato−μ-Hydroxo-Dibridged Copper(II) Complex

A novel mu-pyrazolato-mu-hydroxo-dibridged copper(II) complex has been synthesized and structurally characterized: [(Cu(mepirizole)Br)2(mu-OH)(mu-pz)] (mepirizole=4-methoxy-2-(5-methoxy-3-methyl-1H-pyrazol-1-yl)-6-methylpyrimidine; pz=pyrazolate). The title compound crystallizes in the monoclinic system, space group P2(1)/c, with a=15.618(2) A, b=15.369(3) A, c=16.071(3) A, and beta=112.250(1) degrees. The structure is built up of dinuclear [(Cu(mepirizole)Br)2(mu-OH)(mu-pz)] units with five-coordinated copper(II) ions (CuBrN3O chromophores) linked by mu2-OH and mu2-pyrazolato bridges that are well separated from each others. The intramolecular copper-copper distance is 3.378(3) A. Magnetic…

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…

Coexistence of metamagnetism and slow relaxation of magnetization in ammonium hexafluoridorhenate.

The (NH4)2[ReF6] (1) salt was studied by X-ray diffraction, Raman spectroscopy, theoretical calculations, and magnetic measurements. 1 crystallizes in the trigonal space group Pm1 (Re–F = 1.958(5) A). In the Raman spectrum of 1, splitting of the observed peaks was observed and correlated to the valence frequencies of vibration of the [ReF6]2− anion. The study of the magnetic properties of 1, through DC and AC magnetic susceptibility measurements, reveals the coexistence of metamagnetism and slow relaxation of magnetization at low temperature, which is unusual in the molecular systems based on the paramagnetic 5d metal ions reported so far.

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 …

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 …

Ferromagnetic exchange interaction in a new Ir(iv)-Cu(ii) chain based on the hexachloroiridate(iv) anion.

The iridium(IV) complex (NBu4)2[IrCl6] (1) has been synthetised, characterised and used as a precursor to prepare the new chloro-bridged heterobimetallic IrIV–CuII chain of formula {IrCl5(μ-Cl)Cu(viim)4}n (2) [viim = 1-vinylimidazole]. The crystal structure and magnetic properties of 1 and 2 have been investigated. Both compounds crystallise in the monoclinic system with space group C2/c. Each IrIV ion in both 1 and 2 is six-coordinate and bonded to six chloride ions in a regular octahedral geometry. In compound 2, the CuII ion exhibits an axially elongated octahedron with four N atoms, from four monodentate viim ligands, that form the equatorial plane, and two chloride ions that occupy the…

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 …

Synthesis and characterisation of a novel ferrimagnetic chain based on copper(II) and rhenium(IV)

Abstract A novel one-dimensional copper(II)–rhenium(IV) coordination polymer of formula {[ReIVBr4(μ-ox)CuII(pyim)2]·MeCN}n (1) [ox = oxalate anion, pyim = 2-(2′-pyridyl)imidazole] has been prepared and characterised. Powder X-ray diffraction measurements on a sample of 1 support the purity of the bulk sample, whereas single-crystal X-ray diffraction shows that 1 crystallises in the orthorhombic system with space group Pbca. The crystal structure of 1 is made up of [CuII(pyim)2]2+ cations and [ReBr4(ox)]2− anions linked through bridging bromide and oxalate groups, which generate alternating CuII and ReIV chains. Variable-temperature magnetic susceptibility measurements performed on 1 reveal …

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.

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…

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.

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.

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…

Hexahalorhenate(iv) salts of protonated ciprofloxacin: antibiotic-based single-ion magnets

Two novel Re(IV) compounds of formula [H2cip][Hcip][ReCl6]Cl·H2O (1) and [Hcip]2[ReBr6] (2) [(H2cip)2+/(Hcip)+ = ciprofloxacindiium cation / ciprofloxacinium cation] have been synthesized and studied structurally and magnetically. 1 crystallizes in the monoclinic system with space group P21/c, whereas 2 crystallizes in the orthorhombic system with space group Pbca. 1 and 2 are hexahalorhenate(IV) salts obtained with the protonated ciprofloxacin antibiotic. In their crystal lattice, the [ReX6]2− [X = Cl(1) and Br(2)] anions are well separated from each other through the protonated ciprofloxacindiium (1) and ciprofloxacinium (1 and 2) cations, which are arranged without generating intermolecu…

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…

Hexachlororhenate(IV) salts of ruthenium(III) cations: X-ray structure and magnetic properties

Abstract Two novel rhenium(IV)–ruthenium(III) compounds of formulae [RuCl(NH3)5]2[ReCl6]Cl2 (1) and [RuCl2(en)2]2[ReCl6]·2CH3CN (2) (en = 1,2-ethylenediamine) have been prepared and characterized. Their crystal structures were determined by single-crystal X-ray diffraction. 1 crystallizes in the monoclinic system with C2/m as space group, whereas 2 crystallizes in the triclinic system with space group P(−1). The crystal structures of 1 and 2 are made up of discrete [ReCl6]2− anions and [RuCl(NH3)5]2+ (1) or [RuCl2(en)2]+ (2) cations held together by N–H···Cl hydrogen bonds, van der Waals and electrostatic forces. The magnetic properties were investigated from susceptibility measurements per…

Hexanuclear manganese(III) single-molecule magnets based on oxime and azole-type ligands

Abstract Two novel hexanuclear manganese(III) complexes belonging to the Mn6 family of single-molecule magnets (SMMs), of formulae [Mn6(μ3-O)2(H2N-sao)6(bta)2(EtOH)6]·2EtOH·4H2O (1) and [Mn6(μ3-O)2(H2N-sao)6(pta)2(EtOH)6]·4EtOH (2) [H2N-saoH2 = salicylamidoxime, bta = 1,2,3-benzotriazolate anion, pta = 5-phenyl-tetrazolate anion], have been synthesized and characterized structurally and magnetically. Both compounds crystallize in the triclinic system with space group P 1 ¯ (1 and 2). In their crystal packing, adjacent Mn6 complexes are connected through non-coordinating solvent molecules, which are H-bonded to N atoms of azole rings and –NH2 groups of salicylamidoxime ligand. The study of t…

A novel series of rhenium-bipyrimidine complexes: synthesis, crystal structure and electrochemical properties

Four novel rhenium complexes of formula [ReCl(4)(bpym)] (1), [ReBr(4)(bpym)] (2) PPh(4)[ReCl(4)(bpym)] (3) and NBu(4)[ReBr(4)(bpym)] (4) (bpym = 2,2'-bipyrimidine, PPh(4) = tetraphenylphosphonium cation and NBu(4) = tetrabutylammonium cation), have been synthesized and their crystal structures determined by single-crystal X-ray diffraction. The structures of 1 and 2 consist of [ReX(4)(bpym)] molecules held together by van der Waals forces. In both complexes the Re(iv) central atom is surrounded by four halide anions and two nitrogen atoms of a bpym bidentate ligand in a distorted octahedral environment. The structures of 3 and 4 consist of [ReX(4)(bpym)](-) anions and PPh(4)(+) () or NBu(4)…

Pressure induced enhancement of the magnetic ordering temperature in rhenium(IV) monomers

Materials that demonstrate long-range magnetic order are synonymous with information storage and the electronics industry, with the phenomenon commonly associated with metals, metal alloys or metal oxides and sulfides. A lesser known family of magnetically ordered complexes are the monometallic compounds of highly anisotropic d-block transition metals; the ‘transformation' from isolated zero-dimensional molecule to ordered, spin-canted, three-dimensional lattice being the result of through-space interactions arising from the combination of large magnetic anisotropy and spin-delocalization from metal to ligand which induces important intermolecular contacts. Here we report the effect of pres…

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.

CCDC 1029762: Experimental Crystal Structure Determination

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CCDC 1568973: Experimental Crystal Structure Determination

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CCDC 1048366: Experimental Crystal Structure Determination

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CCDC 1568972: Experimental Crystal Structure Determination

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CCDC 1848843: Experimental Crystal Structure Determination

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CCDC 1991872: Experimental Crystal Structure Determination

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CCDC 1848844: Experimental Crystal Structure Determination

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CCDC 1557653: Experimental Crystal Structure Determination

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CCDC 1586972: Experimental Crystal Structure Determination

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CCDC 1534670: Experimental Crystal Structure Determination

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CCDC 1550275: Experimental Crystal Structure Determination

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CCDC 1580082: Experimental Crystal Structure Determination

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CCDC 2046049: Experimental Crystal Structure Determination

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CCDC 1550272: Experimental Crystal Structure Determination

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CCDC 1922348: Experimental Crystal Structure Determination

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CCDC 1550271: Experimental Crystal Structure Determination

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CCDC 1534665: Experimental Crystal Structure Determination

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CCDC 1503662: Experimental Crystal Structure Determination

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CCDC 1049976: Experimental Crystal Structure Determination

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CCDC 1885666: Experimental Crystal Structure Determination

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CCDC 1054691: Experimental Crystal Structure Determination

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CCDC 1534671: Experimental Crystal Structure Determination

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CSD 1962857: Experimental Crystal Structure Determination

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CCDC 1866320: Experimental Crystal Structure Determination

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CCDC 1534674: Experimental Crystal Structure Determination

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CCDC 1556333: Experimental Crystal Structure Determination

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CCDC 1534667: Experimental Crystal Structure Determination

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CCDC 1550274: Experimental Crystal Structure Determination

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CCDC 1534666: Experimental Crystal Structure Determination

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CCDC 1910060: Experimental Crystal Structure Determination

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CCDC 1534669: Experimental Crystal Structure Determination

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CCDC 1018429: Experimental Crystal Structure Determination

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CCDC 1534675: Experimental Crystal Structure Determination

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CCDC 1029763: Experimental Crystal Structure Determination

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CCDC 1556332: Experimental Crystal Structure Determination

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CCDC 986670: Experimental Crystal Structure Determination

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CCDC 1503663: Experimental Crystal Structure Determination

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CCDC 1054690: Experimental Crystal Structure Determination

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CCDC 1011545: Experimental Crystal Structure Determination

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CCDC 1991873: Experimental Crystal Structure Determination

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CCDC 1586971: Experimental Crystal Structure Determination

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CCDC 1447970: Experimental Crystal Structure Determination

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CCDC 1922347: Experimental Crystal Structure Determination

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CCDC 983737: Experimental Crystal Structure Determination

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CCDC 1534673: Experimental Crystal Structure Determination

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CCDC 1557652: Experimental Crystal Structure Determination

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CCDC 1550273: Experimental Crystal Structure Determination

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CCDC 2046050: Experimental Crystal Structure Determination

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CCDC 1534672: Experimental Crystal Structure Determination

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CCDC 1534668: Experimental Crystal Structure Determination

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CCDC 1557650: 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 1011546: Experimental Crystal Structure Determination

Related Article: José Martínez-Lillo, John Kong, Miguel Julve, Euan K. Brechin|2014|Cryst.Growth Des.|14|5985|doi:10.1021/cg5011693

CCDC 1910059: Experimental Crystal Structure Determination

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CCDC 854108: Experimental Crystal Structure Determination

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CCDC 1550276: Experimental Crystal Structure Determination

Related Article: Anders H. Pedersen, Miguel Julve, José Martínez-Lillo, Joan Cano, Euan K. Brechin|2017|Dalton Trans.|46|16025|doi:10.1039/C7DT02216F