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A 6 Nb 4 S 22 (A = Rb and Cs), compounds with the tetrameric complex anion [Nb 4 S 22 ] 6− : Preparation via the molten flux method and crystal structure determination
Author(s) -
Bensch W.,
Dürichen P.
Publication year - 1996
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.19966221125
Subject(s) - niobium , crystallography , ternary operation , crystal structure , ion , chemistry , metal , coordination number , polyhedron , rod , x ray crystallography , sulfur , diffraction , physics , organic chemistry , optics , medicine , geometry , mathematics , alternative medicine , pathology , computer science , programming language
The new ternary niobium polysulfides A 6 Nb 4 S 22 were prepared at a low temperature of 350°C via the molten flux method by reacting A 2 S 3 (A = Rb, Cs) with niobium metal and additional sulfur. The crystal structure is characterized by [Nb 4 S 22 ] 6− anions. Two Nb 2 S 10 subunits are joined by a S 2 2− . Nb 5+ is coordinated by S 2 2− and S 2− ligands according to [Nb 2 (μ‐η 2 , η 1 ‐S 2 )(η 2 ‐S 2 ) 3 (S) 2 ] 2 (μ‐η 1 ‐S 2 ) 6− . Every Nb is in a sixfold coordination, and the polyhedra can be regarded as strongly distorted pentagonal pyramids. Within the unit cell the anions are stacked in “rods” parallel to the crystallographic b‐axis. These stacks are arranged in “layers” and the A + ions are located between the layers.