[NI-2(SC4H9)(6)](2-), A NOVEL BINUCLEAR N ICKEL-THIOLATE COMPLEX WITHNIS4 TETRAHEDRA SHARING EDGES AND [NI(SC(6)H(4)SIME(3))(4)](2-), A STRUCTURALLY RELATED MONONUCLEAR COMPLEX ION

Reaction of nickel(II) chloride with sodium or potassium tert-butane t hiolate in acetonitrile affords the isotypical compounds [Ni-2(StC(4)H (9))(6)]Na-2 . 4MeCN (1) and [Ni-2(StC(4)H(9))(6)]K-2 . 4 MeCN (2), re spectively, Crystal data: 1: a = 9.859(3), b = 11.877(3), c = 19.675(5 ) Angstrom, beta = 96.11(2)degrees, space group P2(1)/n, Z = 2; 2: a = 9.854(2), b = 11.915(3), c = 20.558(5) Angstrom, beta = 99.62(2)degre es, space group P2(1)/n, Z = 2. The structures were refined to R = 0.0 599 (1) and 0.0562 (2), respectively. Both compounds contain the compl ex ion [Ni-2(StC(4)H(9))(6)](2-) (3), which is not only the first exam ple of a tetrahedral nickel complex with alkane thiolate ligands, but also the first polynuclear nickel complex containing tetrahedral NiS4- units sharing a common edge. Reaction of nickel(II) chloride and sodiu m (2-trimethylsilyl)thiophenolate in acetonitrile leads to [Ni(SC(6)H( 4)SiMe(3))(4)](2-) (5) With tetrahedral stereochemistry. The mononucle ar complex ion is isolated as [Ph(4)P](2)[Ni(SC(6)H(4)SiMe(3))(4)]. 5M eCN (4) with a = 13.771(2), b 14.163(2), c = 25.873(4) Angstrom, alpha = 77.44(1), beta = 75.13(1), gamma = 72.46(1)degrees, space group P ( 1) over bar and Z = 2. The final refinement converged to R = 0.0445.