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Telluride clusters of molybdenum: Synthesis, structures, and NMR spectra

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Abstract

High-temperature reactions of Mo, chalcogen (S or Se), Te, and Br2 in molar ratio Mo: S/Se: Te: Br = 3: 1: 6: 4 were carried out. The reaction products were subjected to mechanochemical activation with K(Dtp) (Dtp = (EtO)2PS2) in a vibrational mill, resulting in the formation of new compounds [Mo3(μ3-Q)0.5(μ3-O)0.5(μ2-Te2)3(Dtp)3](Dtp) (Q = Se (I) and S (II)). The structure of compound I has been established by X-ray diffraction analysis. Solutions of compounds I and II contain mixtures of [Mo3(μ3-Q)(μ2-Te2)3(Dtp)3]+ and [Mo3(μ3-O)(μ2-Te2)3(Dtp)3]+, which is confirmed by mass spectrometry and 31P, 77Se, and 125Te NMR spectroscopy. Quantum-chemical calculations of the 125Te NMR chemical shifts were performed. The compounds are also characterized by IR spectroscopy, Raman spectroscopy, and elemental analysis. Structure I contains short nonvalent contacts between the sulfur atom of the out-of-sphere Dtp anion and the axial tellurium atoms of the cluster.

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Authors and Affiliations

  1. Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, pr. akademika Lavrent’eva 3, Novosibirsk, 630090, Russia

    A. L. Gushchin, M. R. Ryzhikov, A. V. Virovets & M. N. Sokolov

  2. Novosibirsk State University, ul. Pirogova 2, Novosibirsk, 630090, Russia

    A. L. Gushchin & M. N. Sokolov

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  1. A. L. Gushchin
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  2. M. R. Ryzhikov
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  3. A. V. Virovets
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  4. M. N. Sokolov
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Correspondence to A. L. Gushchin.

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Original Russian Text © A.L. Gushchin, M.R. Ryzhikov, A.V. Virovets, M.N. Sokolov, 2013, published in Koordinatsionnaya Khimiya, 2013, Vol. 39, No. 2, pp. 92–97.

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Gushchin, A.L., Ryzhikov, M.R., Virovets, A.V. et al. Telluride clusters of molybdenum: Synthesis, structures, and NMR spectra. Russ J Coord Chem 39, 181–186 (2013). https://doi.org/10.1134/S1070328413020036

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  • DOI: https://doi.org/10.1134/S1070328413020036

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