Jain, A. K., Sharma, V., Bohra, R., Sukumar, A. A., Raju, V. S., Drake, J. E., Hursthouse, M. B. and Light, M. E.
Synthesis and characterization of methylbismuth(III) complexes containing dithio ligands: 2. Crystal and molecular structure of [MeBiCl(S2CNEt2)] and transformation of some [MeBi(S2CNR '(2))(2)] to Bi2S3
Journal of Organometallic Chemistry, 691, (19), . (doi:10.1016/j.jorganchem.2006.06.023).
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Reactions of methylbismuth(III) dichloride with sodium salts of dithiocarbmates have been carried out in 1: 1 and 1:2 stoichiometric ratios in anhydrous benzene to yield products of the types [MeBiCl(S2CNR2)] [where R = Me (1), Et (2) and Pr-i (3)] and [GRAPHICS] These complexes were characterized by elemental analyses and by FT-IR and NMR (H-1 and C-13) spectra. The X-ray structure of [MeBiCl(S2CNEt2)](2), indicates the presence of unique (BiClBi)-Cl-...-Bi-... secondary bonds resulting in a distorted square pyramidal environment around the central bismuth(III) atom. TGA of (6) shows a single step break down of the complex to Bi2S3 at 262.8 degrees C. Transformations of (6) and (8) to pure Bi2S3 have been carried out successfully in refluxing xylene (142 degrees C) as revealed by XRD and SEM studies.
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