The reactions of thiacyclohexane (TCH) with Os3(CO)io(NCMe)2, Os3(CO)u(NCMe), and Os3(CO)i2 have been investigated. The reaction of TCH with OssfCO) io(NCMe) 2 at 25 °C yielded the disubstituted product Os3(CO)io(TCH)2, 1, in 86% yield. At 97 °C, compound 1 was I-1 transformed into four new compounds: OssiCOlgOi-SC^C^C^C^CH/u-Hh, 2 (20%),and Os3(CO)9(m-SCH2CH2CH2CH2CH)(m-H), 5 (13%). Compounds 2,3, and 5 were characterized by single crystal X-ray diffraction analysis. These three products were formed by the loss of one TCH ligand. In compounds 5 and 2 the remaining TCH ligand has undergone activation of one and two CH bonds, respectively, a to the sulfur atom and the TCH ligand was transformed into a metalated triply bridging ligand. Compounds 2 and 5 are interconvertible isomers.Compounds 2,3, and 5 were also obtained from the pyrolysis of 4 at 97 °C and from the reaction of Os3(CO)i2 with TCH at 125 °C. Crystallographic data for 2: space group, PI, a = 9.2559(9)
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