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1.
Dalton Trans ; 2020 Jan 24.
Artigo em Inglês | MEDLINE | ID: mdl-31976497

RESUMO

By changing the stoichiometric ratios, the one-pot reaction of the glycinehydroxamic acid (H2glyha) ligand with copper(ii) and lanthanide(iii) salts in the presence of diamagnetic [Na2{Fe(CN)5(NO)}] led to two series of isostructural complexes, which can be designated as heterotrimetallic dimeric clusters [{LnCu5(glyha)5}{Fe(CN)5(NO)}(H2O)4]2·xNO3·yH2O (x = 2, y = 11 for La (1), x = 2, y = 11 for Pr (2), and x = 2, y = 11 for Nd (3)) and heterotetrametallic coordination polymers [Na{LnCu5(glyha)5}{Fe(CN)5(NO)}2(H2O)x·yH2O]n (x = 6, y = 4 for Sm (4), x = 6, y = 0 for Gd (5), x = 6, y = 4 for Tb (6), x = 5, y = 5 Dy (7), and x = 6, y = 4 for Ho (8)). Each molecular structure contains LnIII[15-metallacrown-5] nodes and diamagnetic [Fe(CN)5(NO)]2- linkers. The resulting products demonstrate diversified structural frameworks due to the radius effect of LnIII ions and different bridging fashions of diamagnetic [Fe(CN)5(NO)]2- linkers. An analysis of magnetic susceptibilities reveals that 7 exhibits ferromagnetic coupling between CuII and DyIII ions and field-induced SMM behavior.

2.
Dalton Trans ; 46(38): 13027-13034, 2017 Oct 14.
Artigo em Inglês | MEDLINE | ID: mdl-28937171

RESUMO

Herein, a new family of LnIII[18-metallacrown-6] compounds with the formula [Fe6O2Ln(tBu-sao)6(OH)(MeO)4(MeOH)(H2O)]·6MeOH [Ln = DyIII (1), TbIII (2), GdIII (3), and YIII (4), tBu-saoH2 = 3,5-di-tert-butylsalicylaldoxime] was synthesized through one-pot reactions using tBu-saoH2, Fe(ClO4)3·6H2O, and Ln(NO3)3·6H2O. The four compounds are isostructural, and the encapsulation of a Ln ion in the ring cavity of 18-metallacrown-6 (18-MC-6) was exhibited for the first time. The structural analysis shows a ship-like 18-MC-6 core with a beset lanthanide ion connecting six ring oxygen atoms (OMC). Magnetic measurements reveal domain antiferromagnetic coupling interactions between metal ions and field-dependent slow magnetic relaxation in 1-3.

3.
Inorg Chem ; 56(5): 2481-2489, 2017 Mar 06.
Artigo em Inglês | MEDLINE | ID: mdl-28199094

RESUMO

Two novel POM-based inorganic-organic hybrids, [Cu6II(2,2'-bipy)6(Mo6O22)(SiW12O40)]n (1), and {[Cu6II(ppz)6(H2O)5(MoO4)(SiW12O40)]·4H2O}n (2) (2,2'-bipy = 2,2'-bipyridine, Hppz = 3-(pyrid-2-yl)pyrazole), have been constructed from heteropolytungstates and molybdates. Two compounds have been identified by single crystal X-ray diffraction, elemental analysis, and FT-IR. Compound 1 shows a 1D (one-dimensional) chain structure constructed from classical Keggin heteropolytungstate [SiW12O40]4- clusters and [Cu6(2,2'-bipy)6] modified isopolymolybdates [Mo6O22]8-. Compound 2 also represents a 1D chain-like motif built from classical Keggin heteropolytungstate [SiW12O40]4- clusters and [Cu8(ppz)6(H2O)5] modified molybdates MoO42-. Compound 1 represents the first example of POM-based inorganic-organic hybrid with mixed heteropolytungstates and isopolymolybdates. ESI-MS (electrospray ionization mass spectrometry) technique was employed to reveal the species and their evolutions in the hydrothermal reaction, whereby trivacant [SiW9] building block gradually transforms to classical Keggin [SiW12] during assembly process. Furthermore, the electrocatalytic and magnetic properties were discussed in details.

4.
Inorg Chem ; 55(17): 9006-11, 2016 Sep 06.
Artigo em Inglês | MEDLINE | ID: mdl-27548500

RESUMO

A planar hexanuclear cobalt ring was clamped by two bivacant α1-[PW10O37](9-) with the assistance of the pyridazine bridges to form a novel sandwiched Co(II)-polyoxometalate cluster compound, [Na(H2O)6][Co3(OH) (pydz)4(H2O)7][Co6(PW10O37)2(pydz)4(H2O)6]·43H2O (1; pydz = pyridazine).This cluster was identified by X-ray single-crystal diffraction, elemental analysis, Fourier transform IR and UV-visible spectroscopies, and cyclic voltammetry (CV). Structural analysis reveals that 1 comprises a hexahydrated sodium, a trinuclear [Co3(OH) (pydz)4(H2O)7](5+) cationic cluster, and an anionic [Co6(PW10O37)2(pydz)4(H2O)6](6-) sandwiched cluster, thus giving an intrinsical intercluster compound. The isolation of such cluster was dependent on the in situ transformation of trivacant [α-P2W15O56](12-) to α1-[PW10O37](9-) under the hydrothermal condition. The CV shows reversible multielectron waves from the redox of W(VI) in 1. Cluster 1 exhibits remarkable electrocatalytic activity toward the reduction of nitrite. Magnetism studies indicated a weak anti-ferromagnetic exchange interaction between Co(II) ions within 1.

5.
Dalton Trans ; 45(20): 8404-11, 2016 May 28.
Artigo em Inglês | MEDLINE | ID: mdl-27108482

RESUMO

Modified classical trivacant Wells-Dawson α-[P2W15O56](12-) and the assembly of related sandwiched transition metal clusters are of interest, but surprisingly few reports of these materials exist because of the sensitivity of α-[P2W15O56](12-) to the assembly environment. Herein, we describe the pH-controlled assembly of two novel Dawson-sandwiched clusters, (H2bpz)6[Co2(P2W16O57)2]·22H2O (1, bpz = 3,3',5,5'-tetramethyl-4,4'-bipyrazole) and (H2bpz)6[Co3H2(P2W16O57)(P2W15O56)(H2O)]·12H2O (2), involving the in situ transformation of α-[P2W15O56](12-). Both clusters were characterized by X-ray single-crystal diffraction, FT-IR spectroscopy, UV-Visible spectroscopy, thermogravimetric analysis, powder X-ray diffraction, and elemental analyses. X-ray crystallography showed that both heteropolytungstates become divacant α-[P2W16O57](8-) and symmetrically encapsulate two edge-shared CoO6 octahedra in the interior in 1, while only one divacant α-[P2W16O57](8-) is observed in 2, which combined with another trivacant α-[P2W15O56](12-) to asymmetrically clamp three edge-shared CoO6 octahedra. The α-[P2W16O57](8-) heteropolytungstate should be generated in situ from α-[P2W15O56](12-)via self-decomposition equilibria in solution. Their electrochemical behaviors reveal characteristic multi-electron redox processes related to W(VI) centers. The electrocatalytic reduction performances toward nitrite, hydrogen peroxide, chlorate, bromate and iodate were fully measured and discussed; among these species, both clusters exhibit the best electrocatalytic activity towards the reduction of bromate. Magnetic measurements indicate weak ferromagnetic exchange interactions between Co atoms sandwiched by vacant polyoxometalates.

6.
Acta Crystallogr Sect E Struct Rep Online ; 67(Pt 7): m826-7, 2011 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-21836837

RESUMO

The asymmetric unit of the title complex, {[Cd(C(9)H(7)N(3)O(6)S(3))(C(12)H(8)N(2))]·0.42H(2)O}(n), contains a Cd(II) atom, one doubly deprotonated 2,2',2''-[1,3,5-triazine-2,4,6-triyltris(sulfanediyl)]triacetic acid ligand (HTTTA(2-)), a 1,10-phenanthroline (phen) ligand and a fractionally occupied water mol-ecule [site occupancy = 0.421 (15)]. The Cd(II) atom is six-coordinated within a distorted octa-hedral coordination geometry. Six coordination arises from four O atoms derived from three different HTTTA(2-) ligands, and two N atoms of the chelating phen mol-ecule. The incompletely deprotonated triazine ligand adopts a µ(3)-η(1):η(1):η(2) coordination mode, resulting in the formation of chains along the c axis based on Cd(2)O(2) dimeric units. Adjacent chains are stacked through π-π stacking [3.533 (2) Šbetween phen and triazine rings] and C-H⋯O inter-actions, forming supra-molecular sheets in the ab plane. Intra-and intermolecular O-H⋯O hydrogen bonds are also observed.

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