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

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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) Å, α = 74.900(3)°, β = 76.150(3)°, γ = 76.221(2)°, V = 1718.2(5) Å3, Z = 2, D cacl = 1.717 Mg/m3; R = 0.0453, R w = 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.

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Acknowledgment

Financial support from the Robert A. Welch Foundation (Grants P-0074-WHW and B-1093-MGR) is appreciated.

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Authors and Affiliations

  1. Department of Chemistry, Texas Christian University, Fort Worth, TX, 76129, USA

    William H. Watson

  2. Department of Chemistry, University of North Texas, Denton, TX, 76203, USA

    Shih-Huang Huang & Michael G. Richmond

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  1. William H. Watson
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  2. Shih-Huang Huang
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  3. Michael G. Richmond
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Correspondence to William H. Watson or Michael G. Richmond.

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Watson, W.H., Huang, SH. & Richmond, M.G. Synthesis and Characterization of the Osmium Compound cis(CO)–ClOs(CO)2(bpcd)[C(O)Et]. J Chem Crystallogr 37, 479–482 (2007). https://doi.org/10.1007/s10870-007-9197-6

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  • DOI: https://doi.org/10.1007/s10870-007-9197-6

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