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Methyl- and phenylgermanium derivatives of diethyldithiocarbamic acid. The crystal and molecular structure of diphenylbis(N,N-diethyldithiocarbamato)germanium

1988; Elsevier BV; Volume: 143; Issue: 1 Linguagem: Inglês

10.1016/s0020-1693(00)85842-9

1873-3255

Raj K. Chadha, John E. Drake, Anil B. Sarkar,

Synthesis and characterization of novel inorganic/organometallic compounds

Abstract Methyl- and phenylgermanes were reacted with the sodium salt of N,N-diethyldithiocarbamic acid in carbon disulfide at low temperature under rigorous exclusion of moisture. Halogen-exchange reactions were carried out to prepare partially substituted bromo and iodo derivatives. The compounds were characterized by elemental analysis, infrared, Raman, proton and carbon-13 NMR spectroscopy and mass spectrometry. The spectroscopic results indicate monodentate or anisobidentate coordination of the diethyldithiocarbamate group. To confirm this assumption, the crystal structure of a representative compound, (C6H5)2Ge[SC(S)N(C2H5)2]2, was determined by X-ray crystallography. The molecule crystallizes in the C2/c space group with a=20.416(7), b=7.320(3), c=17.137(6) A, β=90.06(3)°, V=2561(2) A3, Z=4, ϱ(obs.)=1.33 g cm−3, ϱ(calc.)=1.36 g cm−3. Using Mo Kα radiation (λ= 0.71069 A), 1689 unique reflections were collected (21 ± 1) °C and the structure was refined to a final R value of 0.0377. The position of the phenyl and monodentate dithiocarbamate groups result in a distorted tetrahedral symmetry about germanium with a bonded GeS distance of 2.271(1) A compared to a non-bonded GeS distance of 3.183 A.