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1999 (1)
1Author    A.B M Shamsur, Rahman, H. Boiler, K. O. KleppRequires cookie*
 Title    Synthesis and Structural Characterization of [Me4N]2[W202(/i-S)(r72-S2)4]*MeCN, a Novel Oxo-thiotungstate(VI)  
 Abstract    Orange red crystals of the new compound [Me4 N]2 [W2 0 2 (^ -S 2)(?/2 -S2)4 ] MeCN were ob­ tained from the reaction of a solution of [Me4 N ]2 [WOS3 ] in MeCN with solid AuCN at room temperature. They are monoclinic, space group P2|//?, with a = 9.264(2), b = 17.736(3), c = 18.742(5) A, ß = 95.19(1)°; Z = 4. The crystal structure was determined from single crystal diffractometer data (M oKa-radiation) and refined to R = 0.050 (2955 reflections, 221 variable parameters). It is characterized by binuclear complex anions [(S2)2 0 WSWO(S2)2 r 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 A which together with a bridging sulfur atom (dw-s = 2.445 A) occupy the equatorial positions of a pentagonal bipyramid whose apices are defined by a terminal oxygen atom (dw -o ~ 1 -725 A) and one sulfur atom of the neighboring component at a distinctly larger distance (dw -s ~ 2.82 A). Infrared spectra of the complex (KBr powder) showed z/(W-O) and i^(W-S) of bridging W-S-W at 931 (vs) and 454 (m) cm -1, respectively, u{ W-S) of the W S2 unit appeared in the range between 465 and 438 crrT 1. The mass spectrum of the anion showed the molecular mass at m/z 6 8 8 for [W2 0 2 S9 ]~ as well as peaks for other fragments. 
  Reference    Z. Naturforsch. 54b, 1318—1322 (1999); received April 19 1999 
  Published    1999 
  Keywords    Crystal Structure, IR Data, Chalcogenides, Complex Sulfides, Tungsten Compounds 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1318.pdf 
 Identifier    ZNB-1999-54b-1318 
 Volume    54