Syntheses, crystal structure and spectroscopic characterization of novel N-R-sulfonyldithiocarbimate and triphenylphosphine nickel(II) complexes
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- 作者：Oliveira ; Marcelo R.L. ; Vieira ; Heulla P. ; Perpé ; tuo ; Genivaldo J. ; Janezak ; Jan ; De Bellis ; Vito M.
- 关键词：Dithiocarbimates ; Triphenylphosphine ; Nickel complexes ; Crystal structures
- 刊名：Polyhedron
- 出版年：2002
- 出版时间：October 1, 2002
- 年：2002
- 卷：21
- 期：22
- 页码：2243-2250
- 全文大小：616 K
文摘
Three new complexes of the general formula: [Ni(PPh3)2(RSO2N
CS2)] where R=2-CH3C6H4 (1), 4-CH3C6H4 (2) and 4-BrC6H4 (3) were obtained in crystalline form by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimates (K2(RSO2NCS2)) and triphenylphosphine with nickel(II) chloride in ethanol–water. The 1 complex crystallizes in the centrosymmetric space group of the triclinic system with two molecules per unit cell, while 2 and 3 complexes crystallize in the Pbca space group of the orthorhombic system with eight molecules per unit cell. The X-ray single-crystal analysis showed that all complexes present a similarly distorted square-planar configuration around the nickel atom due to the steric effect of the triphenylphosphine ligands and the didendate chelation by the two sulfur atoms of the dithiocarbimate ligand. The IR and UV–Vis spectral data are consistent with the formation of almost square-planar nickel complexes. The 1H NMR, 13C NMR, 31P NMR spectra showed the expected signals for the triphenylphosphine and the dithiocarbimate moieties.
CS2)] where R=2-CH3C6H4 (1), 4-CH3C6H4 (2) and 4-BrC6H4 (3) were obtained in crystalline form by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimates (K2(RSO2NCS2)) and triphenylphosphine with nickel(II) chloride in ethanol–water. The 1 complex crystallizes in the centrosymmetric space group of the triclinic system with two molecules per unit cell, while 2 and 3 complexes crystallize in the Pbca space group of the orthorhombic system with eight molecules per unit cell. The X-ray single-crystal analysis showed that all complexes present a similarly distorted square-planar configuration around the nickel atom due to the steric effect of the triphenylphosphine ligands and the didendate chelation by the two sulfur atoms of the dithiocarbimate ligand. The IR and UV–Vis spectral data are consistent with the formation of almost square-planar nickel complexes. The 1H NMR, 13C NMR, 31P NMR spectra showed the expected signals for the triphenylphosphine and the dithiocarbimate moieties.