New Chalcogenogermanates with Adamantane Type Complex Anions: Preparation and Crystal Structures of K4Ge4S10; Rb4Ge4S10, Rb4Ge4Se10, and Cs4Ge4Seio
نویسندگان
چکیده
Z. Naturforsch. 54 b, 1499-1504 (1999); received August 19, 1999 Crystal Structure, Complex Chalcogenides, Alkali Thiogermanate(IV), Alkali Selenogermanate(IV) The title compounds were obtained by reacting stoichiometric quantities of the corresponding dialkalimonochalcogenide, germanium powder and chalcogen at 1073 K. The four compounds are isostructural, crystallizing in space group C2/c, Z = 4 with K4Ge4Sio: a = 15.161(3), b = 15.198(2), c = 8.760(2) Ä, ß = 105.36(3)°, Rb4Ge4Si0: a = 15.282(7), b = 15.341(7), c = 9.061(4) A, ß = 106.10(3)°; Rb4Ge4Sei0: a = 16.095(9), b = 16.09(1), c = 9.390(7) A, ß = 105.79(2)° and Cs4Ge4Se10: a = 16.348(9), b = 16.49(1), c = 9.771(3) A, ß = 107.10(3)°. Their crystal structures were solved and refined from single crystal diffractometer data (MoKa radiation) obtained at 294 K. They are characterized by the formation of discrete adamantanelike complex anions [Ge4Qio]4which are arranged in slabs parallel to (010). Mean Ge-S bond lengths are 2.202 A for K4Ge4Sio and 2.186 A for Rb4Ge4Sio while the mean Ge-Se bond length in both selenides amounts to 2.332(3) A. Terminal and bridging Ge-Q bonds differ by at least 0.1 A. The atomic arrangement corresponds to that of Tl4Ge4Sio.
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