Synthesis of [SCo3(CO)7(S2COMe)] and the structure of its PPh3 derivative |
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Authors: | László Markó Giuliana Gervasio Pier Luigi Stanghellini György Bor |
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Affiliation: | (1) Institute of Organic Chemistry, University of Veszprém, H-8200 Veszprém, Hungary;(2) Institute of General and Inorganic Chemistry, University of Turin, I-10125 Turin, Italy;(3) Department of Industrial and Engineering Chemistry, Swiss Federal Institute of Technology (E.T.H.), CH-8092 Zürich, Switzerland |
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Abstract: | Summary The title compound has been prepared in reasonable yield by reaction of a methanolic solution of CoCl2 and MeOCS2K with CO. I.r. spectra have been analyzed both in the C-O stretching region and in the region of the main vibrations of the xanthate ligand: an explanation of the appearance of only 4 out of 7 i.r.-active (CO) modes is proposed. The structure of the triphenylphosphine derivative has been solved by x-ray diffraction analysis: [SCo3(CO)6(PPh3)(S2COMe)] crystallizes in the triclinic space group P¯1, witha = 10.710(3),b = 10.199(3) andc = 16.208(4) Å, = 113.57(2)°, = 98.14(2)°, = 104.32(2)°, Z = 2, (MoK) = 0.7107 Å. The final R value is 0.045 [4461 reflections with F > 6 (F)]. The molecule is formed by an SCo3 cluster, in which each Co atom coordinates two CO groups. The chelating xanthate ligand is equatorially bonded to two cobalt atoms forming a nonplanar pentaatomic ring; the phosphine is equatorially bonded to the other cobalt atom. |
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