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Crystal Growth and Structure Refinement of K 4 Ge 9
Author(s) -
Ponou Simeon,
Fässler Thomas F.
Publication year - 2007
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200600308
Subject(s) - crystallography , ampoule , niobium , cluster (spacecraft) , crystal structure , metal , single crystal , crystal (programming language) , germanium , atom (system on chip) , chemistry , materials science , silicon , organic chemistry , computer science , embedded system , programming language
Deep‐red moisture and air sensitive single crystals of K 4 Ge 9 were obtained by reacting GeO 2 and elemental Ge with metallic W and K at high temperature in a niobium ampoule. The crystal structure of the compound was determined by single crystal X‐ray diffraction experiments. K 4 Ge 9 crystallizes in a polar space group R 3 c (No. 161), Z = 4 with a = 21.208(1) and c = 25.096(2) Å. The compound contains discrete Ge 9 4− Wade's nido ‐clusters which are packed according to a hierarchical atom‐to‐cluster replacement of the Cr 3 Si prototype and are separated by K + cations. Two independent [Ge 9 ] 4− clusters A (at Cr positions) and B (at Si positions) are found with a ratio A:B = 3:1. The B ‐type cluster satisfactorily represents orientational disorder around the three‐fold axis.