Reactions of polysulphide with metal–phosphine species. Synthesis and X-ray crystal structure of [{Ni(bppte)(µ-OH)}2][ClO4]2·(CH3)2CO
Abstract
The reaction of [Ni(H2O)6][ClO4]2 in the presence of 1,1,1-tris(diphenylphosphinomethyl)ethane, tppme, with [Sn]2– leads to the formation of the dimeric hydroxo-complex [{Ni(bppte)(µ-OH)}2][ClO4]2·(CH3)2CO, bppte = PPh2SCH2C(CH3)(CH2PPh2)2, which was structurally characterized by X-ray diffraction. Crystal data are: a= 19.046(7), b= 18.195(6), c= 13.349(5)Å, β= 97.76(4)°, space group P21/a, and Z= 2. In the centrosymmetric dimeric hydroxo-bridged cation each metal atom displays square-planar co-ordination, the third arm of the ligand, PPh2SCH2, being unco-ordinated. The unexpected formation of hydroxo complexes is discussed.