Preparation, structure and properties of three [MoxW4−xS4(H2O)12]5+ (x = 1–3) and [MoW3Se4(H2O)12]5+ cuboidal complexes alongside [Mo4S4(H2O)12]5+ and [Mo4Se4(H2O)12]5+

McLean, Iain J.; Hernández-Molina, Rita; Sokolov, Maxim N.; Seo, Mi‐Sook; Вировец, А. В.; Elsegood, Mark R. J.; Clegg, William; Sykes, A. G.

doi:10.1039/a803396j

Cited by 19 publications

(23 citation statements)

References 28 publications

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“…As seen in Table 2, sulfido dithiolene complexes are easier to oxidize than their selenido analogues. This tendency has also been observed for the cubane‐type Mo 3 Q 4 and Mo 4 Q 4 clusters 12. Owing to their low redox potentials, anions 1 2– and 2 2– are easily oxidized.…”

Section: Resultssupporting

confidence: 58%

Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

et al. 2013

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Section: Resultssupporting

confidence: 58%

Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

et al. 2013

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“…Synthesis of Cyano Complexes. Preparative routes used previously to obtain Mo 4 E 4 n + cuboidal clusters (E = S, Se), n = 4, 5, and 6, include dimerization of chalcogenide Mo 2 complexes and addition of a mononuclear complex to a Mo 3 triangular chalcogenide complex. , Self-assembly routes have also been developed for molybdenum. ,, The β-[W 4 S 4 (μ-dtp) 2 (dtp) 4 ] and α-[W 4 S 4 (μ-dtp) 3 (dtp) 3 ] cuboidal W 4 S 4 6+ core complexes have been obtained from [W(CO) 6 ] and Na 2 [WO 4 ] or K 3 [W 2 Cl 9 ] in the presence of P 2 S 5 in ethanol . Poor reproducibility and low yields are however noted in the latter case.…”

Section: Resultsmentioning

confidence: 99%

Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano Complexes with Cuboidal M₄(μ₃-E)₄ (M = Mo, W; E = S, Se, Te) Cores

Fedin¹,

Kalinina²,

Samsonenko³

et al. 1999

Inorg. Chem.

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Four new tungsten and molybdenum cyano complexes of formula KCs(5)[W(4)S(4)(CN)(12)].CH(3)OH.2H(2)O (1), K(6)[W(4)Se(4)(CN)(12)].6H(2)O (2), K(6)[W(4)Te(4)(CN)(12)].5H(2)O (3), and K(7)[Mo(4)Te(4)(CN)(12)].12H(2)O (5) have been prepared by high-temperature 430-450 degrees C reaction of the polymeric chain compounds {W(3)S(7)Br(4)}(x)(), {W(3)Se(7)Br(4)}(x)(), {Mo(3)Te(7)I(4)}(x)() and solid-state WTe(2) with KCN, and crystallization from aqueous solutions. In addition Cs(6)[Mo(4)Te(4)(CN)(12)].2H(2)O (4) has been prepared by oxidation of 5 with bromine water. The molecular structures have been investigated by X-ray crystallography. Mixed-valence (3.5) compounds 1-4 are diamagnetic. Mixed-valence (3.25) compound 5 is paramagnetic (&mgr; = 2.03 &mgr;(B) at 77 K). In addition to the structural data for these complexes IR and UV-vis spectroscopy have been used to characterize the complexes. Cyclic-voltammetry data have shown that M(4)E(4)(n)()(+) (M = Mo, W; E = S, Se, Te) cubes are capable of existing in three oxidation states ranging from the most oxidized (n = 6; 10 electrons) to the most reduced electron-precise (n = 4; 12 electrons). The (77)Se, (125)Te, and (183)W NMR spectra of the cubes (1-3) demonstrate unambiguously the unaltered environments of the W and E atoms in aqueous solution.

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“…The occupation of the chlorine atom in the counteranion and the two water molecules was refined to give values of 30% for the chlorine atom and 95% and 50% for the two O(100) and O(101) water molecules, respectively. Finally the occupancy was fixed to 33% for Cl (10), 100% for O(100) and 50% for O(101) in order to balance the overall positive charge. This model precludes the presence of H 3 O ϩ cations in the structure.…”

Section: Crystallographymentioning

confidence: 99%

“…In the case of their Se analogues the situation is similar (they are somewhat more difficult to reduce). 10 The potentials of the [Mo 3 CuQ 4 (H 2 O) 10 ] 5ϩ/4ϩ couples are not too negative (Q = S, Ϫ0.35 V; Q = Se, Ϫ0.30 V) and the 4ϩ cube can be handled even in strongly acidic solutions. The change to [W 3 CuS 4 (H 2 O) 10 ] 5ϩ would shift this potential to a much more negative value, thus making the 4ϩ state unobservable in acidic solutions because of its efficient oxidation by H ϩ .…”

Section: New Cuboidal Clustersmentioning

confidence: 99%

Aqueous solution chemistry of [Mo3CuSe4]n+ (n = 4, 5) and [W3CuQ4]5+ (Q = S, Se) clusters

et al. 2004

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The triangular cluster [Mo3Se4(H2O)9]4+ reacts with Cu turnings to give a new heterometallic cuboidal cluster [Mo3CuSe4(H2O)10]4+(purple; UV/Vis lambda(epsilon): 352(3907), 509(2613)). The reaction of [Mo3Se4(H2O)9]4+ with CuCl afforded the 5+ cube [Mo3CuSe4(H2O)10]5+(red; UV/Vis lambda(epsilon): 356(5406), 500(3477)). In contrast, [W3Se4(H2O)9]4+ both with Cu and CuCl gives the 5+ cube, [W3CuSe4(H2O)10]5+(yellow-green; UV/Vis lambda(epsilon): 312(5327), 419(3256) and 628(680)). Cyclic voltammetry of [M3CuQ4(H2O)10]5+ in 2 M HCl (M = Mo, W; Q = S, Se) shows a reversible one-electron reduction wave for the Mo clusters, but no reduction occurs for the W clusters prior to H+ reduction. In HCl solutions, Cl is coordinated to the Cu site of the clusters, alongside some less extensive coordination to Mo and W, and for [W3(CuCl)S4(H2O)6Cl3]+, isolated as the supramolecular adduct with cucurbit[6]uril, [W3(CuCl)S4(H2O)6Cl3]2Cl2 x C36H36N24O12 x 12H2O, the crystal structure was determined (Cu-W 2.856(4) angstroms, W-W 2.7432(15) angstroms, Cu-Cl 2.167(13) angstroms).

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Preparation, structure and properties of three [MoxW4−xS4(H2O)12]5+ (x = 1–3) and [MoW3Se4(H2O)12]5+ cuboidal complexes alongside [Mo4S4(H2O)12]5+ and [Mo4Se4(H2O)12]5+

Cited by 19 publications

References 28 publications

Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano Complexes with Cuboidal M₄(μ₃-E)₄ (M = Mo, W; E = S, Se, Te) Cores

Aqueous solution chemistry of [Mo3CuSe4]n+ (n = 4, 5) and [W3CuQ4]5+ (Q = S, Se) clusters

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Preparation, structure and properties of three [MoxW4−xS4(H2O)12]5+ (x = 1–3) and [MoW3Se4(H2O)12]5+ cuboidal complexes alongside [Mo4S4(H2O)12]5+ and [Mo4Se4(H2O)12]5+

Cited by 19 publications

References 28 publications

Mo3Q7 (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Mo3Q7 (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano Complexes with Cuboidal M4(μ3-E)4 (M = Mo, W; E = S, Se, Te) Cores

Aqueous solution chemistry of [Mo3CuSe4]n+ (n = 4, 5) and [W3CuQ4]5+ (Q = S, Se) clusters

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Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Mo₃Q₇ (Q = S, Se) Clusters Containing Dithiolate/Diselenolate Ligands: Synthesis, Structures, and Their Use as Precursors of Magnetic Single‐Component Molecular Conductors

Synthesis, Structure, and Properties of Molybdenum and Tungsten Cyano Complexes with Cuboidal M₄(μ₃-E)₄ (M = Mo, W; E = S, Se, Te) Cores