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Synthesis and Structural Characterization of [Me4N]2[W2O2(μ-S)(η2-S2)4]·MeCN, a Novel Oxo-thiotungstate(VI)
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A. B. M. Shamsur Rahman
Published/Copyright:
June 2, 2014
Orange red crystals of the new compound [Me4N]2[W2O2 (μ-S2)(η2 -S2)4] MeCN were obtained from the reaction of a solution of [Me4N]2[WOS3] in MeCN with solid AuCN at room temperature. They are monoclinic, space group P21/n, with a = 9.264(2), b = 17.736(3), c = 18.742(5) Å, ß = 95.19(1)°; Z = 4. The crystal structure was determined from single crystal diffractometer data (MoKα-radiation) and refined to R = 0.050 (2955 reflections, 221 variable parameters). It is characterized by binuclear complex anions [(S2)2OWSWO(S2)2]2- with close to C2 symmetry. Each metal center is surrounded by two end-on coordinating disulfide groups at distances ranging from 2.37 to 2.42 Å which together with a bridging sulfur atom (d̄w-s = 2.445 Å) occupy the equatorial positions of a pentagonal bipyramid whose apices are defined by a terminal oxygen atom (d̄w-o~ 1 -725 Å) and one sulfur atom of the neighboring component at a distinctly larger distance (d̄w-s~ 2.82 Å).
Infrared spectra of the complex (KBr powder) showed ν(W-O) and ν(W-S) of bridging W-S-W at 931 (vs) and 454 (m) cm - 1, respectively, ν(W-S) of the WS2 unit appeared in the range between 465 and 438 cm -1. The mass spectrum of the anion showed the molecular mass at m/z 688 for [W2O2 S9]- as well as peaks for other fragments.
Received: 1999-4-19
Published Online: 2014-6-2
Published in Print: 1999-10-1
© 1946 – 2014: Verlag der Zeitschrift für Naturforschung
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Keywords for this article
Crystal Structure;
IR Data;
Chalcogenides;
Complex Sulfides;
Tungsten Compounds
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