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NEt 4 [SiSCl 3 ] · 0.5CCl 4  was obtained from NEt 4 SH and SiCl 4  in liquid H 2 S and subsequent crystallization from CH 2 Cl 2 /CCl 4 . The analogous reaction with GeCl 4  was performed without solvent at room temperature. Raman and IR spectra are in accord with simple anionic species with C 3v  symmetry. The crystal structure of NEt 4 [SiSCl 3 ] · 0.5 CCl 4  was determined from X-ray diffraction data (849 independent observed reflexions, R - 0.030). Crystal data: tetragonal, space group P4̄c2 , Z = 4, a = 1196.0, c = 1200.7 pm. Both, cation and anion occupy positions on twofold rotation axes, with the consequence of positional disorder for the [SiSCl 3 ] -  ion by statistical superposition of the sulfur and one chlorine position. The general packing of cations and anions resembles the NaCl type, the CCl 4  molecules occupying interstices. NEt 4 [GeSCl 3 ] · 0.5 CCl 4  is isotypic (a = 1204, c = 1201 pm); NEt 4 [GeSCl 3 ] also crystallizes in the tetragonal system (a = 1048.4, c = 1274.4 pm).

zeitschrift für naturforschung b

Darstellung und Schwingungsspektren von Thiotrichlorosilicat und -germanat. Die Kristallstruktur von NEt 4 [SiSCl 3 ] · 0,5 CCl 4 / Preparation and Synthesis of Thiotrichloro Silicate and Germanate. Crystal Structure of NEt 4 [SiSCl 3 ] · 0.5 CCl 4