Clusters of the Heavier Elements of Main Groups 14–16: A Novel Synthetic Route for Polyanions in Molten Crown Ether
DOI:
https://doi.org/10.2533/chimia.1998.158Abstract
A novel procedure allows the synthesis of homoatomic polyanions directly from the elements E (E = Sn, As, Sb, Te) in molten A/18-crown-6 as reaction medium (A = K, Rb) at temperatures between 40 and 80° [1]. The reactions are carried out by adding E to mixtures of A and 18-crown-6 that proved to form stable melts under these conditions. Further work off using ethylenediamine or DMF as solvent yielded single crystals of the following compounds: [K(18-crown-6)]4Sn9 (1), [K(18-crown-6)]3KSn9·en (2), [K(18-crown-6)]3As7 (3), [K([2.2.2]crypt)]2[K(18-crown-6)]Sb7·0.5en (4), [Rb(18-crown-6)]3Sb7 (5), [K(18-crown-6)]2Te4 (6), and [K(18-crown-6)]2Te4·en (7). In all compounds short contacts between the Zintl ions and A-atoms are observed. The influence of cation-anion interactions on the structure of these anions is discussed.
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