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Cluster Oxalate Complexes [W3(μ3-Q)(μ2-Q)3 (C2O4)3(H2O)3]2− (Q=S, Se): Mechanochemical Synthesis and Crystal Structure

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Abstract

Mechanochemical reaction of cluster coordination polymers \(^1_{\infty}[\hbox{W}_3\hbox{Q}_7\hbox{Br}_4]\) (Q=S, Se) with solid \(\hbox{K}_2\hbox{C}_2\hbox{O}_4\) leads to the cluster core excision with the formation of anionic complexes \([\hbox{W}_3\hbox{Q}_7(\hbox{C}_2\hbox{O}_4)_3]^{2-}\). Extraction of the reaction mixture with water followed by crystallization gives crystalline \(\hbox{K}_2[\hbox{W}_3\hbox{S}_7(\hbox{C}_2\hbox{O}_4)_3]\cdot 0.5 \hbox{KBr}\cdot 5\hbox{H}_2\hbox{O}\) (main product) and \(\hbox{K}_2[\hbox{W}_3(\upmu_3 \hbox{-S})(\upmu_2 \hbox{-S})_3 (\hbox{H}_2\hbox{O})_3(\hbox{C}_2\hbox{O}_4)_3]\cdot 0.5\hbox{H}_2\hbox{C}_2\hbox{O}_4 \cdot 3\hbox{H}_2\hbox{O}\) (1) (minor product). In the case of the Se cluster, the \(\hbox{W}_3\hbox{Se}_7\) complex could not be isolated, and the treatment of the aqueous extract with PPh3 gave \(\hbox{K}_2[\hbox{W}_3(\upmu_{3}\hbox{-Se})(\upmu_2\hbox{-Se})_3 (\hbox{H}_2\hbox{O})_3(\hbox{C}_2\hbox{O}_4)_3]\cdot \hbox{H}_2\hbox{O}\) (2) in a low yield. Alternatively, it was obtained from \([\hbox{W}_3\hbox{Se}_4(\hbox{H}_2\hbox{O})_9]^{4+}\) and \(\hbox{K}_2\hbox{C}_2\hbox{O}_4\) in high yield. Both 1 and 2 were characterized by X-ray structure analysis.

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Acknowledgements

A grant from the Russian Science Support Foundation to MNS is gratefully acknowledged. The work was supported by INTAS (2356) and the Russian Foundation for Basic Research (grants 05-03-32126). ALG thanks Haldor Topsoe A/S for a fellowship.

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Authors and Affiliations

  1. Nikolaev Institute of Inorganic Chemistry, Russian Academy of Sciences, Lavrentiev Avenue 3, Novosibirsk, 630090, Russia

    Maxim N. Sokolov, Artyom L. Gushchin, Dmitrii Yu. Naumov, Olga A. Gerasko & Vladimir P. Fedin

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  1. Maxim N. Sokolov
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  2. Artyom L. Gushchin
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  3. Dmitrii Yu. Naumov
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  4. Olga A. Gerasko
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  5. Vladimir P. Fedin
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Correspondence to Vladimir P. Fedin.

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Dedicated to Academician I. I. Moiseev on the occasion of his 75th birthday and in recognition of his outstanding contribution to cluster chemistry.

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Sokolov, M.N., Gushchin, A.L., Naumov, D.Y. et al. Cluster Oxalate Complexes [W3(μ3-Q)(μ2-Q)3 (C2O4)3(H2O)3]2− (Q=S, Se): Mechanochemical Synthesis and Crystal Structure. J Clust Sci 16, 309–318 (2005). https://doi.org/10.1007/s10876-005-0026-9

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