Synthesis of new thiol derivatives of [Os3(CO)12]; crystal structure of [Os3(CO)10(μ-H) {μ-SC(CH3)3}]

Article abstract of DOI:10.1016/0020-1693(95)04832-4

The clusters [Os₃(CO)₁₀(μ-H) {μ-SC(CH₃)₃}] (1) and [Os₃(CO)₁₀(μ-H) {μ-SC₆H₁₁}] (2) have been synthesized by addition of the appropriate thiol RSH (R = C(CH₃)₃, C₆H₁₁) to [Os₃(CO)₁₁(NCMe)] or [Os₃(CO)₁₀(NCMe)₂] in dichloromethane. Clusters 1 and 2 have been characterized by IR, NMR, mass spectrometry and, in the case of 1, X-ray crystallography. Compound 1 crystallizes in space group P21/n (a = 9.507(1), b = 12.860(1), c = 17.838(3) A, β = 99.77(1)°, Z = 4). The molecule conforms to an idealized C_s symmetry. The bond distances in the osmium triangle average 2.860 A; there is no significant elongation of the Os-Os edge in 1 that is bridged by the hydride and the thiolate moiety.