Structural studies in main group chemistry : XVII. The crystal and molecular structure of phenylchlorobis(diethyldithiocarbamato)tin(IV)

Abstract

The crystal structure of the title compound has been determined by single crystal X-ray diffraction from diffractometer data using Patterson and Fourier techniques. Crystals are monoclinic, space group P2 1/ n, with Z  4 in each unit cell of dimensions a  19.764(8), b  15.760(8), c  7.121(4) Å, β  93.7(1)°. The structure was refined by block-diagonal least squares methods to R 0.059 for 3022 observed reflections. The tin atoms are six-coordinated in a distorted octahedral fashion by the phenyl group, chlorine atom, and two chelating diethyldithiocarbamato residues, the phenyl group and chlorine atom occupying mutually cis positions (SnC 2.154(5); SnCl 2.438(6), mean SnS 2.583(7) Å). The structures of few monoorganotin(IV) derivatives have been determined. Methylstannane and the methyltin trihalides, MeSnX 3 X  Cl, Br, I, all possess tetrahedral structures in the vapour phase [2], whilst [(MeSn) 4S 6], which has an adamantane-type structure [3] and [PhCl 2SnFe(CO) 2(C 5H 5)] [4] both have four-coordinated tin in the crystal. However, in [(C 10H 8N 2)(CO) 3MoClSnMeCl 2] [5] and [(C 4H 10S 2)(CO) 3WClSnMeCl 2] [6] the coordination number at tin is raised to five by a chlorine atom which bridges both metals. Seven-coordination at tin is observed in [MeSn(NO 3) 3] in which all three nitrate groups chelate the metal [7]. The reaction of [PhSnCl3] with potassium diethyldithiocarbamate in a 1 : 3