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…

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.

Magnetic phase transition and magnetic bistability in oxamato-based CoIICuII bimetallic MOF thin films

Abstract Thin films of an anionic oxamato-bridged cobalt(II)–copper(II) 3D MOF have been growth at 120 °C in DMSO through a one-pot reaction from Co(NO3)2·6H2O and (Me4N)2[Cu(2,6-Et2pa)2]·6H2O (2,6-Et2pa = N-2,6-diethylphenyloxamate) over Si(111) surfaces functionalized with carboxylic acid terminating groups. These heterobimetallic CoII2CuII3 MOF thin films (2) of about ten nanometers thickness show a ferrimagnetically ordered phase below ca. 10 K with a relatively large magnetic hysteresis similar to that of the bulk material of formula (Me4N)2[Co2Cu3(2,6-Et2pa)6]·5H2O (1).

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…

Metamagnetic Behavior in [M (tvp) (NCS)2] Coordination Polymers (M = Fe(II) and Co(II); tvp = 1,2-di-(4-pyridyl)-ethylene)

Abstract We report the synthesis and magnetic properties of two new coordination polymers of formula [M(tvp)(NCS)2] (M = Fe(II) and Co(II)). The magnetic data reveal the occurrence of metamagnetic behavior. Switching from bulk antiferromagnetic to ferromagnetic behavior occurs for magnetic fields greater than 1300 G (Fe(II)) and 450 G (Co(II)) at temperatures lower than 4 K. Both compounds are isomorphous. A molecular structure is suggested in the light of the magnetic properties and precedent data on related systems.

Light Induced Excited Pair Spin State in an Iron(II) Binuclear Spin-Crossover Compound

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…

Critical temperature of the LIESST effect in iron(II) spin crossover compounds

Abstract The light-induced crossover in a series of iron(II) compounds has been investigated by irradiating the sample at 10 K with a Kr + laser coupled to an optical fiber within a SQUID cavity. The temperature dependence of the molar fraction of the light-induced metastable HS state has been recorded for 22 compounds. The critical LIESST temperature, T c (LIESST), has been defined as the temperature for which the light-induced HS information was erased in the SQUID cavity. The dependence of T c (LIESST) as a function of the thermal spin crossover temperature, T 1/2 , has been discussed. The effect of cooperation has been analyzed and the influence of horizontal and vertical displacements …

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…

Spin-crossover in the [Fe(abpt)2(NCX)2] (X=S, Se) system: Structural, Magnetic, calorimetric and photomagnetic studies

[EN] The compounds [Fe(abpt)(2)(NCS)(2)] (1) and [Fe(abpt)(2)(NCSe)(2)] (2) with abpt = 4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole have been synthesized. The X-ray structures have been determined at 293 K. 1 and 2 are isostructural and crystallize in the monoclinic space group P2(1)/n with Z = 2, a = 8.538(8), b = 10.246(8), c = 16.45(2) Angstrom, beta = 93.98(9)degrees for 1 and a = 8.623(2), b = 10.243(3), c = 16.585(3) Angstrom, beta = 93.19(2)degrees for 2. In both complexes, the coordination core has a similar pseudo-octahedral geometry with the NCS- (1) and NCSe- (2) groups in the trans-position. Variable-temperature magnetic susceptibility data give evidence for a low-spin (LS)high…

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…

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…

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…

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…

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.

Spin crossover in six-coordinate [Fe(L)2(NCX)2] compounds with L = DPQ = 2,3-bis-(2′-pyridyl)-quinoxaline, ABPT = 4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole and X = S, Se: synthesis, magnetic properties and single crystal studies

[EN] The iron(II) compounds of formulae [Fe(DPQ)2(NCS)2]·CO(CH)3)2(DPQ = 2,3-bis-(2¿-pyridyl)-quinoxaline) (1) and [Fe(ABPT)2-(NCX)2] (ABPT = 4-amino-3,5-bis(pyridin-2-yl)-1,2,4-triazole) X = S (2) and Se (3) were synthesized and the crystal structure of 1 determined by X-ray diffraction methods. It crystallizes in the monoclinic system . The structure is made up of discrete [Fe(DPQ)2(NCS)2] units. Each metal atom is in a distorted FeN6 octahedral environment, the Fe¿N bonds ranging from 2.013(8) Å to 2.425(8) Å. Variable-temperature magnetic susceptibility data in the temperature range 290¿4.2 K revealed that 1 is high spin, in contrast to 2 and 3 which show a moderately cooperative high s…

Direct monitoring of spin state in dinuclear iron(II) coordination compounds

So far there has been no direct method to determine the spin state of molecules in dinuclear iron(II) compounds. The molecular fractions of high-spin (HS) and low-spin (LS) species have been deduced from magnetic susceptibility and zero-field Mossbauer spectroscopy data irrespective of whether they belong to LS–LS, LS–HS and HS–HS pairs. However, the distinction of pairs becomes possible if Mossbauer measurements are carried out in an external magnetic field. The proposed method opens new possibilities in the study of spin crossover phenomena in dinuclear compounds.

Polymorphism and Pressure Driven Thermal Spin Crossover Phenomenon in [Fe(abpt)2(NCX)2] (X=S, and Se): Synthesis,Structure and Magnetic Properties

The monomeric compounds [Fe(abpt 2(NCX)2(X = S (1), Se (2) and abpt = 4-amino- 3,5-bis(pyridin-2-yl)-1,2,4-triazole) have been synthesized and characterized. They crystallize in the monoclinic P21/n space group with a = 11.637(2) A, b = 9.8021(14) A, c = 12.9838(12) A, β = 101.126(14)°, and Z=2 for 1, and a= 11.601(2) A, b = 9.6666(14) A, c = 12.883(2) A, β = 101.449(10)°, and Z = 2 for 2. The unit cell contains a pair mononuclear [Fe(abpt)2(NCX)21 units related by a center of symmetry. Each iron atom, located at a molecular inversion center, is in a distorted octahedral environment. Four of the six nitrogen atoms coordinated to the Fe(II) ion belong to the pyridine-N(1) and triazole-N(2) r…

Two-dimensional assembling of 4,4'-bipyridine and 4,4'-azopyridine bridged iron(II) linear coordination polymers via hydrogen bond

[EN] Novel two-dimensional polymers, [Fe(L-1)(H2O)(2)(NCX)(2)]. L-1 (L-1 =4.4'-bipyridine (bipy)) (1, 2) and [Fe(L-2)(CH3OH)(2)-(NCX)(2)]. L-2 (L-2 =4,4'-azopyridine (azpy)) (3) and X = S (1, 3), Se (2), have been synthesized and characterized by X-ray crystallography. The structures reveal the formation of tranzs-L-bridged [Fe(NCX)(2)(Y)(2)] where Y=H2O, CH3OH linear chains assembled into two-dimensional networks by hydrogen bonds between the uncoordinated ligand L and the coordinated solvent molecules.

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…

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 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…

Generalized “one-pot” preparative strategy to obtain highly functionalized silica-based mesoporous spherical particles

In this work we present a synthesis strategy for the preparation of Stöber-type mesoporous particles functionalized with inorganic species. The procedure is based on a combination of the Atrane and the Stöber methods. Both as a source of silicon and of the incorporated heteroelements (Fe, Zn, Al, Ti) the corresponding atrane complexes are used as hydrolytic reagents. These complexes are easily formed by reaction with triethanolamine. Mesoporosity is achieved using surfactant micelles as templates. Obtaining uniform spherical particles is achieved by optimizing the amount of water-ethanol in the reaction medium. The particle sizes have been modulated by controlling simple parameters such as …

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 1969476: Experimental Crystal Structure Determination

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CCDC 1989325: Experimental Crystal Structure Determination

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CCDC 1969477: Experimental Crystal Structure Determination

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CCDC 2073773: Experimental Crystal Structure Determination

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CCDC 1529277: Experimental Crystal Structure Determination

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CCDC 1969470: Experimental Crystal Structure Determination

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CCDC 1901771: Experimental Crystal Structure Determination

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CCDC 2073771: Experimental Crystal Structure Determination

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CCDC 1586972: Experimental Crystal Structure Determination

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CCDC 1529275: Experimental Crystal Structure Determination

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CCDC 1969471: Experimental Crystal Structure Determination

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CCDC 2073772: Experimental Crystal Structure Determination

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CCDC 2011616: Experimental Crystal Structure Determination

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CCDC 1580082: Experimental Crystal Structure Determination

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CCDC 2073774: Experimental Crystal Structure Determination

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CCDC 2011615: Experimental Crystal Structure Determination

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CCDC 1866320: Experimental Crystal Structure Determination

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CCDC 1901770: Experimental Crystal Structure Determination

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CCDC 1910060: Experimental Crystal Structure Determination

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CCDC 1529486: Experimental Crystal Structure Determination

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CCDC 2076621: Experimental Crystal Structure Determination

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CCDC 1901769: Experimental Crystal Structure Determination

Related Article: Tatiana R. G. Simões, Maria Vanda Marinho, Jorge Pasán, Humberto O. Stumpf, Nicolás Moliner, Francesc Lloret, Miguel Julve|2019|Dalton Trans.|48|10260|doi:10.1039/C9DT01277J

CCDC 1901768: Experimental Crystal Structure Determination

Related Article: Tatiana R. G. Simões, Maria Vanda Marinho, Jorge Pasán, Humberto O. Stumpf, Nicolás Moliner, Francesc Lloret, Miguel Julve|2019|Dalton Trans.|48|10260|doi:10.1039/C9DT01277J

CCDC 1586971: Experimental Crystal Structure Determination

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CCDC 1969473: Experimental Crystal Structure Determination

Related Article: Maria-Gabriela Alexandru, Diana Visinescu, Beatrice Cula, Sergiu Shova, Renato Rabelo, Nicolás Moliner, Francesc Lloret, Joan Cano, Miguel Julve|2021|Dalton Trans.|50|14640|doi:10.1039/D1DT02512K

CCDC 1969472: Experimental Crystal Structure Determination

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CCDC 2047766: Experimental Crystal Structure Determination

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CCDC 2011617: Experimental Crystal Structure Determination

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