The crystal structure of bis(dithiobenzil)nickel

Abstract

A three-dimensional X-ray crystal structure analysis has been carried out on Ni(SCPhCPhS)2 at 115°K. In a monoclinic unit ceil having a= 5·836, b= 10·97, c= 18·36 Å, β= 91·4°, and space group P21/n, there are two molecules so that the nickel atoms lie on the centres of symmetry and are co-ordinated by four sulphur atoms. The sulphur atoms were located by Patterson methods, and the other atoms from difference Fourier syntheses. Atomic co-ordinates for all atoms, isotropic vibration parameters for hydrogen atoms, and anisotropic vibration parameters for the other atoms were refined by least-squares until R was 0·111. In the chelate ring Ni–S = 2·101 ± 0·002, C–S = 1·71 ± 0·01, C–C = 1·37 ± 0·014Å; S–Ni–S = 89·8 ± 0·1°, Ni–S–C = 107·3 ± 0·3°, S–C–C = 118 ± 1°. Each phenyl group is planar with an average C–C bond length of 1·38 ± 0·01 Å; neither is coplanar with the chelate ring. The C–C distance from the chelate ring to the phenyl group is 1·47 ± 0·014Å. The nickel atom is strictly four-co-ordinate, the nearest additional neighbours being four hydrogen atoms at 3·2 Å.