Synthesis and Structure of the Dimethyl Sulfide Complexes [OsX 4 (dms) 2 ] (Х = Cl, Br) and [Os 2 OCl 6 (dms) 4 ]
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A systematic study of the thermal decomposition of osmium(IV) complexes [H(dmso) 2 ] 2 [OsX 6 ] and [H(dmso) 2 ][OsX 5 (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- [OsX 4 (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 [Os 2 OCl 6 (dms) 4 ]. IR spectra of [OsX 4 (dms) 2 ] support the assumed trans conformation, 1 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 4 (dms) 2 ]. The structures were determined by single crystal X-ray diffraction. The two polymorphic modifications were found for trans -[OsCl 4 (dms) 2 ]. The dinuclear [Os 2 OCl 6 (dms) 4 ] includes an oxide bridge between two trans -[OsCl 3 (dms) 2 ] fragments.
