Bis(pentafluorophenyl)nickel(<scp>II</scp>) thio-molybdates and -tungstates. Crystal structure of [NBu₄]₂[Ni₂(C₆F₅)₄(µ-WS₄)]

Abstract

The complexes [NBu4]2[Ni2(C6F5)4(µ-MS4)](M = Mo 1 or W 2) have been prepared by reaction of [NBu4]2[Ni2(C6F5)4(µ-OH)2] with [NH4]2[MS4] in ethanol in 1 : 1 molar ratio. When the bis(hydroxo) complex was treated with [NH4]2[MO4 –nSn] and NBu4OH the complexes [NBu4]2[Ni(C6F5)2(µ-MO4 –nSn)](M = Mo, n= 4 3, 3 4, or 2 5; M = W, n= 4 6 or 2 7) were obtained. Conductance and spectroscopic (IR and 19F NMR) measurements have been made. In complexes 1 and 2 two Ni(C6F5)2 subunits are bridged by a tetradentate bridging MS42– anion, whereas a bidentate terminal S-bonded MO4 –nSn2– anion is present in 3–7. A single-crystal X-ray diffraction study has established that the anion of complex 2 consists of a central S2WS2 tetrahedral subunit bridging two terminal square-planar Ni(C6F5)2 subunits.