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Preparation, crystal structure, and infrared characterization of the first thiocyanato‐oxy‐antimonate(III) [(CH 3 ) 4 N] 2 [Sb 6 O 4 (NCS) 12 ]
Author(s) -
Bertazzi N.,
Alonzo G.,
Saiano F.,
Battaglia L. P.
Publication year - 1995
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.19956211216
Subject(s) - antimonate , crystallography , triclinic crystal system , antimony , chemistry , thiocyanate , crystal structure , infrared spectroscopy , ion , stereochemistry , antimonide , inorganic chemistry , organic chemistry
Abstract The salt [(CH 3 ) 4 N] 2 [Sb 6 O 4 (NCS) 12 ] is the first identified thiocyanato‐oxy‐antimonate(III) complex. Reported are details of the synthesis, relevant infrared data and its x‐ray structure. The compound crystallizes in the triclinic space group P 1 with Z = 2 (C 10 H 12 N 7 O 2 S 6 Sb 3 ) and unit cell dimensions a = 11.314(6), b = 12.846(3), c = 8.679(2) Å; α = 91.93(3)°, β = 90.31(3)° and γ = 99.13(3)°. It contains centrosymmetric [Sb 6 O 4 (NCS) 12 ] 2− anions packed with isolated tetramethyl‐ammonium cations. The fundamental structural element of the anion is provided by the fusion of three SbOSbO rings forming a zig‐zag portion of a ribbon, only slightly pleated. Peculiar is the unequivalence of the six thiocyanate ligands, though all primarily N‐bonded to antimony atoms. Three thiocyanates are terminal while other three are asymmetrically N‐bridging between two centers; two of this latter type are also interconnecting the anions via Sb⋅⋅⋅S contacts. There are three different antimony environments, the primary bonding at Sb being to one nitrogen and three oxygens, to one oxygen and three nitrogens and to two atoms of each type.