Perthiocarboxylate complex. Synthesis, structure and spectroscopic characterization of the tetrameric copper(I) o-tolylperthiocarboxylate, [Cu(S)SSCC 7H 7] 4

Abstract

The [CuS 3C o-tolyl] 4 complex has been prepared through different routes. Its Crystal structure has been determined by X-ray diffraction methods. Crystals are triclinic, space group P 1 , with a = 12.810(5), b = 13.051(6), c = 12.789(5) Å, α, = 94.88(2), β = 98.61(2), γ = 104.11(3) o, and Z = 2. The structure has been solved from diffractometer data by direct and Fourier methods and refined by block-matrix least-squares to R = 0.058 for 4674 observed reflections. The structure consists of discrete tetramers, in which a tetrahedron of copper atoms is bonded to four o-tolylperthiocarboxylato ligands: each of these ligands bridges two metal atoms through its terminal perthio atom, while the other terminal sulfur atom is coordinated only to one of these two metal copper atoms, so that five membered CuSSCS chelate rings are formed. The spectral characteristics (electronic, infrared, 1H and 13C NMR spectra) of the title compound are reported and discussed in comparison with those of the dimeric [CuS 3C o-tolyl] 2·py 2 and of the polymeric [CuS 2C o-tolyl] n complexes.