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Orange red crystals of the new compound [Me 4 N] 2 [W 2 O 2  (μ-S 2 )(η 2  -S 2 ) 4 ] MeCN were obtained from the reaction of a solution of [Me 4 N] 2 [WOS 3 ] in MeCN with solid AuCN at room temperature. They are monoclinic, space group P2 1 /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 [(S 2 ) 2 OWSWO(S 2 ) 2 ] 2-  with close to C 2  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 (d̄ w-s  = 2.445 Å) occupy the equatorial positions of a pentagonal bipyramid whose apices are defined by a terminal oxygen atom (d̄ w-o  ~  1 -725 Å) and one sulfur atom of the neighboring component at a distinctly larger distance (d̄ w-s  ~  2.82 Å).

Synthesis and Structural Characterization of [Me 4 N] 2 [W 2 O 2 (μ-S)(η 2 -S 2 ) 4 ]·MeCN, a Novel Oxo-thiotungstate(VI)