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<p>A systematic study of the thermal decomposition of osmium(IV) complexes [H(dmso)<sub>2</sub>]<sub>2</sub>[OsX<sub>6</sub>] and [H(dmso)<sub>2</sub>][OsX<sub>5</sub>(dmso)] (dmso = dimethylsulfoxide; X = Cl, Br) was carried out. According to column chromatography (CC) data, the major thermolysis products in the temperature range of 100–140 ℃ (X = Cl) and 80–120 ℃ (X = Br) are the dimethyl sulfide (dms) osmium(IV) complexes <i>trans-</i>[OsX<sub>4</sub>(dms)<sub>2</sub>] (X = Cl, Br) with yields of up to 85% (X = Cl) and 95% (X = Br). It also yielded a small amount of the dinuclear complex [Os<sub>2</sub>OCl<sub>6</sub>(dms)<sub>4</sub>]. IR spectra of [OsX<sub>4</sub>(dms)<sub>2</sub>] support the assumed <i>trans</i> conformation, <sup>1</sup>H NMR spectra show only one signal for the dms ligands. UV − Vis absorption spectra allowed to trace different species within distinct CC fractions, with the first fraction agreeing with the isolated crystalline material [OsX<sub>4</sub>(dms)<sub>2</sub>]. The structures were determined by single crystal X-ray diffraction. The two polymorphic modifications were found for <i>trans</i>-[OsCl<sub>4</sub>(dms)<sub>2</sub>]. The dinuclear [Os<sub>2</sub>OCl<sub>6</sub>(dms)<sub>4</sub>] includes an oxide bridge between two <i>trans</i>-[OsCl<sub>3</sub>(dms)<sub>2</sub>] fragments.</p>

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Synthesis and structure of the dimethyl sulfide complexes [OsX4(dms)2] (Х = Cl, Br) and [Os2OCl6(dms)4]

  • 期刊论文

  • 发表日期：

    2026年5月9日

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  • Olga V. Rudnitskaya,
  • Ekaterina V. Dobrokhotova,
  • Tatiana A. Tereshina,
  • Ekaterina K. Kultyshkina,
  • Daniil S. Pshenichnyy,
  • Elena A. Fortalnova,
  • Ivan V. Ananyev,
  • Ilya A. Yakushev,
  • Victor N. Khrustalev

摘要

A systematic study of the thermal decomposition of osmium(IV) complexes [H(dmso)2]2[OsX6] and [H(dmso)2][OsX5(dmso)] (dmso = dimethylsulfoxide; X = Cl, Br) was carried out. According to column chromatography (CC) data, the major thermolysis products in the temperature range of 100–140 ℃ (X = Cl) and 80–120 ℃ (X = Br) are the dimethyl sulfide (dms) osmium(IV) complexes trans-[OsX4(dms)2] (X = Cl, Br) with yields of up to 85% (X = Cl) and 95% (X = Br). It also yielded a small amount of the dinuclear complex [Os2OCl6(dms)4]. IR spectra of [OsX4(dms)2] support the assumed trans conformation, 1H NMR spectra show only one signal for the dms ligands. UV − Vis absorption spectra allowed to trace different species within distinct CC fractions, with the first fraction agreeing with the isolated crystalline material [OsX4(dms)2]. The structures were determined by single crystal X-ray diffraction. The two polymorphic modifications were found for trans-[OsCl4(dms)2]. The dinuclear [Os2OCl6(dms)4] includes an oxide bridge between two trans-[OsCl3(dms)2] fragments.