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Lookup NU author(s): Dr Maxim Sokolov, Dr Mark Elsegood, Professor William Clegg, Emeritus Prof Alfred Sykes
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Three heterometallic Mo3M′S4 derivatives (M′ = Pt, Rh, Re) of the incomplete single-metal depleted cube [Mo3S4(H2O)9]4+ have been prepared by reactions with [PtCl4]2- (+ H3PO2 reductant), RhCl3 and [Re(CO)5Br], repectively. With [PtCl4]2-, the initial product gives, on standing for 2-3 days, the edge-linked double cube [{Mo3PtS4(H2O)9}2] 8+, which is diffcult to elute in Dowex cation-exchange chromatography. In the reaction with RhCl3, chloro products, e.g. [Mo3RhCl3S4(H2O)9] 4+, precede formation of [Mo3RhS4(H2O)12]7+, which is also diffcult to elute, and with [Re(CO)5Br], the product [Mo3Re(CO)3S4(H2O)9] 5+ is obtained. Analyses are consistent with oxidation state assignments Pt0, RhIII and ReI, where the reactions proceed by addition of these forms to [Mo3S4(H2O)9]4+. The analyses and X-ray crystal structure of (Mo2NH2)[Mo3Re(CO)3S4 (NCS)4] are consistent with the formation of an Mo3ReS4 single cube. Yields are high in the first two cases, but much lower in the Re case. Alternative preparations are described in the case of Rh and Re. All three products decay on heating, with reformation of trinuclear [Mo3S4 (H2O)9]4+, which can be recovered by Dowex chromatography. As compared to heterometallic derivatives so far considered, those with M′ = Pt, Rh, Re are much more substitution (and redox) inert, and are air stable. Analogues from [W3S4(H2O)9]4+ with M′ = Pt, Rh have been prepared using similar procedures.
Author(s): Sokolov MN, Villagra D, El-Hendawy AM, Kwak C-H, Elsegood MRJ, Clegg W, Sykes AG
Publication type: Article
Publication status: Published
Journal: Journal of the Chemical Society, Dalton Transactions
Year: 2001
Issue: 18
Pages: 2611-2615
ISSN (print): 1472-7773
ISSN (electronic): 1364-5447
Publisher: Royal Society of Chemistry
URL: http://dx.doi.org/10.1039/b104755h
DOI: 10.1039/b104755h
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