Syntheses, crystal structure and spectroscopic characterization of novel 1,2-bis(diphenylphosphine)ethane(N-R-sulfonyldithiocarbimato)nickel(II) complexes
摘要:
Three new complexes of the general formula: [Ni(RSO2N=CS2)(dppe)], where R = CH3(1), CH3CH2 (2), 2-CH3C6H4 (3) and dppe = 1,2-bis(diphenylphosphine)ethane, were obtained in crystalline form by the one-pot reaction of the appropriate potassium N-R-sulfonyldithiocarbimate: RSO2N=CS2K2 center dot 2H(2)O and 1,2-bis(diphenylphosphine)ethane with nickel(II) chloride hexahydrate in ethanol/water mixture. The complex 1 forms monoclinic crystals (P2(1)/c) with two molecules in the asymmetric unit (Z = 8), while the crystals of the complexes 2 and 3 are orthorhombic, Pbca (Z = 8) and P2(1)2(1)2(1) (Z = 4) respectively, with one molecule in the asymmetric unit. All complexes present a distorted square-planar environment around the Ni atom. The elemental analyses and the IR, H-1 NMR, C-13 NMR and P-31 NMR spectra are consistent with the formation of the nickel(II) complexes with mixed ligands. (c) 2007 Elsevier Ltd. All rights reserved.