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Bromo dimethyl sulfoxide osmium(II) complexes. Molecular structure of cis,fac-[OsBr2(dmso-S)3(dmso-O)]

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Abstract

Bromo dimethyl sulfoxide osmium(II) complexes were synthesized: trans-[OsBr2(dmso-S)4] (1) was obtained by the reaction of K2[OsBr6] with DMSO in the presence of SnBr2 at 100°C and cis,fac-[OsBr2(dmso-S)3(dmso-O)] (2) was prepared by thermal isomerization of 1 in a DMSO solution at 150°C. The coordination mode of DMSO molecules was determined by IR and 1H and 13C NMR spectroscopy. X-ray diffraction analysis showed that compound 2 crystallizes in the monoclinic system, space group P21/n; a = 8.4711(5) Å, b = 27.7876(15) Å, c = 8.5569(5) Å, β = 115.7110(10)°; Z = 4. The coordination polyhedron of osmium is a distorted octahedron; the osmium environment is formed by two cis-arranged bromine atoms and three fac-S-coordinated and one O-coordinated DMSO molecules. The interconversion of complexes in solutions was studied by UV/Vis and 1H and 13C NMR spectroscopy. In chloroform and DMSO, complex 2 isomerizes to cis-[OsBr2(dmso-S)4] and (in the light) to 1. The complexes trans-[OsX2(dmso-d6)4], where X = Cl, Br, were isolated from DMSO-d 6 and characterized by the IR spectra.

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Authors and Affiliations

  1. Peoples Friendship University of Russia, ul. Miklukho-Maklaya 6, Moscow, 117198, Russia

    O. V. Rudnitskaya, E. K. Kultyshkina & E. V. Dobrokhotova

  2. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, Leninskii pr. 31, Moscow, 117907, Russia

    O. N. Shishilov

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  1. O. V. Rudnitskaya
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  2. E. K. Kultyshkina
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  3. E. V. Dobrokhotova
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  4. O. N. Shishilov
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Correspondence to O. V. Rudnitskaya.

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Original Russian Text © O.V. Rudnitskaya, E.K. Kultyshkina, E.V. Dobrokhotova, O.N. Shishilov, 2014, published in Zhurnal Neorganicheskoi Khimii, 2014, Vol. 59, No. 9, pp. 1166–1173.

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Rudnitskaya, O.V., Kultyshkina, E.K., Dobrokhotova, E.V. et al. Bromo dimethyl sulfoxide osmium(II) complexes. Molecular structure of cis,fac-[OsBr2(dmso-S)3(dmso-O)]. Russ. J. Inorg. Chem. 59, 935–942 (2014). https://doi.org/10.1134/S0036023614090149

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  • DOI: https://doi.org/10.1134/S0036023614090149

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