Preparation, crystal structure and spectroscopic characterization of nickel(II) complexes with dithiocarbimate derivated of sulfonamides

This work describes the syntheses of three compounds containing [Ni(RSO2N=CS2)(2)](2-) anions: (Bu4N)(2)[Ni(CH3CH2SO2N=CS2)(2)] (1), (Bu4N)(2)[Ni((4)-IC6H4SO2N=CS2)(2)] (2) and (Bu4N)(2)[Ni(2,5-Cl2C6H3SO2N=CS2)(2)] (3). They were obtained in the crystalline form by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimate (RSO2N=CS2K2) with nickel(II) chloride hexahydrate in methanol/water. Elemental analyses were consistent with the proposed formulae. UV-Vis and IR data are consistent with the formation of nickel-sulfur diamagnetic planar complexes. The H-1 NMR and C-13 NMR spectra showed the expected signals for the tetrabutylammonium cation and the dithiocarbimate moieties. Single crystal structure analyses showed that I crystallizes in the monoclinic space group P2(1)/n, 2 crystallizes in the monoclinic space group P2(1)/c and 3 crystallizes in the triclinic space group P (1) over bar. In these compounds the Ni atom is coordinated to four S atoms in a distorted square plane geometry due to the asymmetric bidentade chelation by each ligand. (c) 2006 Elsevier Ltd. All rights reserved.