Synthetic, structural, and spectroscopic studies of the ligating properties of organic disulphides: X-ray structure of copper(I) iodide–diethyl disulphide (2/1)

Abstract

The synthesis of a series of derivatives of copper(I) halides with organic disulphides is reported. Although most of these complexes are unstable with respect to loss of ligand, the compound 2Cul·Et₂S₂ was sufficiently stable to be subjected to a single-crystal X-ray structure determination. Crystals are monoclinic, space group P2₁/n, with cell dimensions (at –100 ± 5 °C)a= 8.163(4), b= 15.651(3), c= 8.746(4)Å, β= 100.73(2)°, and Z= 4. The structure was solved with data collected at –100(5)°C using direct methods followed by difference-Fourier techniques, and refined to R 0.038 (R′ 0.047) for 1 157 observed reflections. The structure consists of double chains of copper atoms bridged by two iodines, with alternative pairs of copper atoms also bridged by diethyl disulphide molecules. The geometry of the disulphide is compared with that of related complexes, and Raman spectral studies of the ν(S–S) stretching frequency of the series of complexes are reported.