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

• Published in: Polyhedron Vol. 25; no. 10; pp. 2119 - 2126
• Main Authors: de Faria Franca, Eduardo, Oliveira, Marcelo R.L., Guilardi, Silvana, de Andrade, Renato Pereira, Lindemann, Renata Hernandez, Amim, Jorge, Ellena, Javier, De Bellis, Vito M., Rubinger, Mayura M.M.
• Format: Journal Article
• Language: English
• Published: Elsevier Ltd 10.07.2006
• Subjects: Crystal structure; Dithiocarbimate complexes; Nickel complexes; Sulfonamide; Dithiocarbimate complexes; Nickel complexes; Sulfonamide; Crystal structure
• ISSN: 0277-5387
• DOI: 10.1016/j.poly.2005.11.035

Three new N-R-sulfonyldithiocarbimate nickel(II) complexes with the formula (Ph 4P) 2[Ni(RSO 2NCS 2) 2] have been obtained in crystalline form by the reaction of appropriate potassium N-R-sulfonyldithiocarbimate salts and nickel(II) chloride hexahydrate. The compounds were characterized by single crystal X-ray diffraction technique and by IR and NMR spectroscopy. This work describes the syntheses of three compounds containing [Ni(RSO 2N CS 2) 2] 2− anions: (Bu 4N) 2[Ni(CH 3CH 2SO 2N CS 2) 2] ( 1), (Bu 4N) 2[Ni(4-IC 6H 4SO 2N CS 2) 2] ( 2) and (Bu 4N) 2[Ni(2,5-Cl 2C 6H 3SO 2N CS 2) 2] ( 3). They were obtained in the crystalline form by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimate (RSO 2N CS 2K 2) 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 1H NMR and 13C NMR spectra showed the expected signals for the tetrabutylammonium cation and the dithiocarbimate moieties. Single crystal structure analyses showed that 1 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 ¯ . 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.