Synthesis of a Novel Nickel(II) Complex with Dithiocarbimate from Sulfonamide

Potassium N-4-methylphenylsulfonyldithiocarbimate, K₂(4-CH₃C₆H₄SO₂N=CS₂), reacted with nickel(II) chloride hexahydrate and tetrabutylammonium bromide to form the bis(N-4-methylphenylsulfonyldithiocarbimate)nickelate(II) tetrabutylammonium salt (Bu₄N)₂[Ni(4-CH₃C₆H₄S₂C=NSO₂)₂]. The elemental analyses, IR and UV-Vis data obtained were consistent with the formation of a diamagnetic planar complex. The ¹H NMR and the ¹³C NMR spectra showed the expected signals for the dithiocarbimate moiety and the tetrabutylammonium cation. The single-crystal structure analysis showed that this substance crystallizes in the triclinic space group with a = 10.474(3) Å, b = 10.767(3) Å, c = 13.657(3) Å and = 81.54(2)°, = 80.44(2)°, = 67.63(2)°, V = 1398.5(8) ų, and Z = 2. The nickel atom is coordinated to four sulfur atoms.     

Preparation and X-Ray crystal structure of a Novel Nickel(II) complex with dithiocarbimate

The reaction of potassiumN-(methanesulfonyl)-dithiocarbimate, K₂[S₂C=NSO₂CH₃], with nickel(II) chloride hexahydrate, NiCl₂·6H₂O, formed the complex anion bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), [Ni(S₂C=NSO₂CH₃)₂]^2}-, which was isolated as its tetra-n-butylammonium salt. The UV-Vis data obtained were consistent with the formation of a nickelsulfur diamagnetic planar complex. The¹H NMR and the¹³C NMR spectra showed the expected signals for then-Bu₄N⁺ cation and the dithiocarbimate moiety. The single-crystal structure analysis showed that tetra-n-butylammonium bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), (Bu₄N)₂[Ni(S₂C=NSO₂CH₃)₂], crystallizes in the monoclinic space groupP2_l/c witha=9.3197(5),b=15.0795(8),c=17.5286(9) å,=91.262(3),V=2462.8(3) å³, andZ=2. The nickel atom is coordinated to four sulfur atoms.