Selective synthesis of triangular cluster oxido-sulfidocomplexes of Mo and W: High yield preparations of [Mo3O2S2(H2O)9]4+, [W3O2S2(H2O)9]4+, [W2MoO2S2(H2O)9]4+ and their derivatization
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comunitat-uji-handle2:10234/7013
comunitat-uji-handle3:10234/8638
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http://dx.doi.org/10.1016/j.ica.2010.06.017 |
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Title
Selective synthesis of triangular cluster oxido-sulfidocomplexes of Mo and W: High yield preparations of [Mo3O2S2(H2O)9]4+, [W3O2S2(H2O)9]4+, [W2MoO2S2(H2O)9]4+ and their derivatizationAuthor (s)
Date
2010Publisher
ElsevierISSN
0020-1693Bibliographic citation
Inorganica Chimica Acta, 363, 13, p. 3330-3337Type
info:eu-repo/semantics/articleVersion
info:eu-repo/semantics/publishedVersionSubject
Abstract
Reaction of [Mo2O2(μ-S)2(H2O)6]2+ with Mo(CO)6 or metallic Mo under hydrothermal conditions (140 °C, 4 M HCl) gives oxido-sulfido cluster aqua complex [Mo3(μ3-S)(μ-O)2(μ-S)(H2O)9]4+ (1). Similarly, [W3(μ3-S)(μ-O)2(μ ... [+]
Reaction of [Mo2O2(μ-S)2(H2O)6]2+ with Mo(CO)6 or metallic Mo under hydrothermal conditions (140 °C, 4 M HCl) gives oxido-sulfido cluster aqua complex [Mo3(μ3-S)(μ-O)2(μ-S)(H2O)9]4+ (1). Similarly, [W3(μ3-S)(μ-O)2(μ-S)(H2O)9]4+ (2) is obtained from [W2O2(μ-S)2(H2O)6]2+ and W(CO)6. While reaction of [Mo2O2(μ-S)2(H2O)6]2+ with W(CO)6 mainly proceeds as simple reduction to give 1, [W2O2(μ-S)2(H2O)6]2+ with Mo(CO)6 produces new mixed-metal cluster [W2Mo(μ3-S)(μ-O)2(μ-S)(H2O)9]4+ (3) as main product. From solutions of 1 in HCl supramolecular adduct with cucurbit[6]uril (CB[6]) {[Mo3O2S2(H2O)6Cl3]2CB[6]}Cl2⋅18H2O (4) was isolated and structurally characterized. The aqua complexes were converted into acetylacetonates [M3O2S2(acac)3(py)3]PF6 (M3 = Mo3, W3, W2Mo; 5a–c), which were characterized by X-ray single crystal analysis, electrospray ionization mass spectrometry and 1H NMR spectroscopy. Crystal structure of (H5O2)(Me4N)4[W3(μ3-S)(μ2-S)(μ2-O)2(NCS)9] (6), obtained from 2, is also reported. [-]
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