Synthesis, crystal structure and reactivity of OS 3(CO) 9(μ 3-η 2-C 2Ph 2)(μ-C(OMe)Ph)

Abstract

Os 3(CO) 9(μ 3-η 2-C 2Ph 2)(μ-C(OMe)Ph) ( 1) has been prepared by treatment of Os 3(CO) 10(μ 3-η 2C 2 Ph 2) sequentially with PhLi and MeOSO 2CF 3. Protonation of 1 with HBF 4 gives {[Os 3(CO) 9(μ-η 3-C 3Ph 3) +][BF 4 -]}( 2), which leads to the well-known (μ-H)Os 3(CO) 9(μ 3-η 3-C 3Ph 3) ( 3) and Os 3(CO) 9(μ 3-η 2-C 2Ph 2)(μ-CHPh) ( 4) upon hydride attack. Thermolysis of 1 in refluxing hexane produces mainly Os 3 (CO) 9(μ 3-η 2-C 2Ph 2)(μ-CH 2) ( 5). Compound 1 crystallizes in the space group P 1 with a = 10.032 (1) Å, b = 10.119(2) Å, c = 16.972(2) Å, α = 97.06(2)°, β = 94.65(1)°, γ = 98.80(2)°, V = 1681.0(5) Å 3, Z = 2 and R F = 3.2%.