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C–Gd 2 S 3 und C–Tb 2 S 3 : Darstellung und Röntgenstrukturanalyse von Einkristallen
Author(s) -
Schleid Thomas,
Weber Frank A.
Publication year - 1998
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/(sici)1521-3749(199804)624:4<557::aid-zaac557>3.0.co;2-l
Subject(s) - dodecahedron , crystallography , trigonal crystal system , crystal structure , molar ratio , sulfur , rare earth , metal , caesium , chemistry , single crystal , materials science , mineralogy , inorganic chemistry , metallurgy , biochemistry , catalysis
C–Gd 2 S 3 and C–Tb 2 S 3 : Synthesis and X‐Ray Structure Analysis of Single Crystals Pale yellow, bead‐shaped single crystals of C‐type Gd 2 S 3 (a = 838.47(9) pm) and Tb 2 S 3 (a = 835.23(9) pm) are obtained upon the oxidation of the respective rare‐earth metal (M = Gd and Tb) with sulfur (molar ratio 2 : 3) in evacuated silica tubing at 700 °C in the presence of fluxing CsCl within five days. Their crystal structure belongs to a cation‐deficient Th 3 P 4 ‐type variant (cubic, I43d) according to M 2.667 □ 0.333 S 4 (Z = 4) or M 2 S 3 (Z = 5.333) offering coordination numbers of eight (S 2– arranged as trigonal dodecahedra) to the cations. In spite of the high Cs + activity in molten CsCl, no cesium incorporation into the M 5.333 □ 0.667 S 8 ‐frame structure ( e. g. as CsM 5 S 8 with Z = 2) can be achieved, judged from refined occupation factors of M 3+ very close to x = 8/9 for M 3x S 4 .