Synthesis and Characterization of the Osmium Compound cis(CO)–ClOs(CO)2(bpcd)[C(O)Et

Abstract

Photochemical activation of the triosmium cluster Os3(CO)12 in CH2Cl2 solvent and ethylene, followed by treatment with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd), furnishes the new octahedral compound cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] in low yield. The title compound has been isolated and characterized in solution by IR and 1H NMR spectroscopies, with the solid-state structure of cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] determined by X-ray diffraction analysis. cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] crystallizes in the triclinic space group P-1, a = 10.043(2), b = 11.455(2), c = 16.221(3) A, α = 74.900(3)°, β = 76.150(3)°, γ = 76.221(2)°, V = 1718.2(5) A3, Z = 2, Dcacl = 1.717 Mg/m3; R = 0.0453, Rw = 0.0778 for 6703 observed reflections with I > 2σ(I). The presence of the chlorine and propanioyl groups in cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] is structurally confirmed, and the origin of the these groups from the reaction solvent and ethylene is discussed.