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Chlorine-atom abstraction and cluster fragmentation in the reaction of H3Re3(CO)10(MeCN)2 with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray diffraction structure of fac-ClRe(CO)3(bpcd)

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Treatment of the activated trirhenium cluster H3Re3(CO)10(MeCN)2 with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) in CH2Cl2 does not afford the expected cluster product H3Re3(CO)10(bpcd) but rather the mononuclear complex fac-ClRe(CO)3(bpcd). The identity of fac-ClRe(CO)3(bpcd) was determined in solution by IR and NMR (1H and 31P) spectroscopies and the solid-state structure was established by X-ray diffraction analysis. fac-ClRe(CO)3(bpcd) crystallizes in the triclinic space P-1, a = 9.958(2) Å, b = 11.991(3) Å, c = 13.676(3) Å, α = 73.230(4)°, β = 73.806(4)°, γ = 77.409(4)°, V = 1484.6(6) Å3, Z = 2, and d calc = 1.723 Mg/m3; R = 0.0367, R w  = 0.0857 for 4253 reflections with I > 2σ(l).

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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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Correspondence to William H. Watson.

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Watson, W.H., Kandala, S. & Richmond, M.G. Chlorine-atom abstraction and cluster fragmentation in the reaction of H3Re3(CO)10(MeCN)2 with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray diffraction structure of fac-ClRe(CO)3(bpcd). J Chem Crystallogr 36, 71–75 (2006). https://doi.org/10.1007/s10870-005-9029-y

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