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Synthesis and Crystal Structures of Cs 5 Nb 2 S 4 X 9 – Double Salts Containing New Cluster Anions [Nb 2 (μ‐S 2 ) 2 X 8 ] 4– (X = Cl, Br)
Author(s) -
Sokolov Maxim,
Imoto Hideo,
Saito Taro,
Fedorov Vladimir
Publication year - 1999
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(199906)625:6<989::aid-zaac989>3.0.co;2-g
Subject(s) - isostructural , chemistry , crystallography , octahedron , crystal structure , halogen , tetragonal crystal system , halide , oxonium ion , cluster (spacecraft) , aqueous solution , ion , stereochemistry , inorganic chemistry , alkyl , computer science , programming language , organic chemistry
Bis(disulfide)bridged Nb(+4) cluster halide complexes [Nb 2 S 4 X 8 ] 4– (X = Cl, Br) were prepared by acid hydrolysis of [Nb 2 S 4 (NCS) 8 ] 4– in concentrated aqueous HCl or HBr, solution from which they can be isolated as double salts Cs 5 [Nb 2 S 4 X 8 ]X (X = Cl, 1 ; X = Br, 2 ). The crystal structures of 1 and 2 were determined. The isolation and X‐ray structure of oxonium salt (H 3 O) 5 [Nb 2 S 4 Cl 8 ]Cl ( 3 ) is also reported. 1 – 3 contain new [Nb 2 S 4 X 8 ] 4– anions which can also be viewed as excised building blocks of polymeric solids NbS 2 X 2 . The extra halogen resides in the center of octahedron formed by six Cs + or H 3 O + ions. All the three salts are isostructural and crystallize in tetragonal space group Immm with the following parameters: a = 10.269(2), b = 16.343(2), c = 7.220(1) Å for 1 , a = 10.934(1), b = 16.613(2), c = 7.470(1) Å for 2 , a = 9.639(1), b = 16.031(1), c = 7.071(1) Å for 3 . The parameters of the Nb 2 S 4 core are only slightly affected by the change from Cl to Br.