caa a22 4500 463184297 CHVBK 20180406164848.0 cr unu---uuuuu 170326e20070701xx s 000 0 eng 10.1007/s10870-007-9197-6 doi (NATIONALLICENCE)springer-10.1007/s10870-007-9197-6 Synthesis and Characterization of the Osmium Compound cis (CO) - ClOs(CO)2(bpcd)[C(O)Et] [Elektronische Daten] [William Watson, Shih-Huang Huang, Michael Richmond] 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=1.717Mg/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. Springer Science+Business Media, LLC, 2007 Triosmium cluster nationallicence Diphosphine ligand nationallicence Photochemistry nationallicence C-H bond activation nationallicence CO insertion nationallicence Watson William Department of Chemistry, Texas Christian University, 76129, Fort Worth, TX, USA aut Huang Shih-Huang Department of Chemistry, University of North Texas, 76203, Denton, TX, USA aut Richmond Michael Department of Chemistry, University of North Texas, 76203, Denton, TX, USA aut Journal of Chemical Crystallography Kluwer Academic Publishers-Plenum Publishers; http://www.springer-ny.com 37/7(2007-07-01), 479-482 1074-1542 37:7<479 2007 37 10870 https://doi.org/10.1007/s10870-007-9197-6 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10870-007-9197-6 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Watson William Department of Chemistry, Texas Christian University, 76129, Fort Worth, TX, USA aut NATIONALLICENCE 700 1- Huang Shih-Huang Department of Chemistry, University of North Texas, 76203, Denton, TX, USA aut NATIONALLICENCE 700 1- Richmond Michael Department of Chemistry, University of North Texas, 76203, Denton, TX, USA aut NATIONALLICENCE 773 0- Journal of Chemical Crystallography Kluwer Academic Publishers-Plenum Publishers; http://www.springer-ny.com 37/7(2007-07-01), 479-482 1074-1542 37:7<479 2007 37 10870 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer