Synthesis, structure of a new acceptor TBA₂S₆ and preparation, physical properties of ET₃S₆

A general procedure for the synthesis of the tetrabutylammoium hexasulphide, TBA₂S₆, is first described. The structure of TBA₂S₆ has been determined by X-ray crystallography. Lattice parameters and space group information are as follows: a = 15.039(5) angstroms, b = 16.086(5) angstroms, c = 17.078(6) angstroms, α = β = γ = 90.00°, V = 4131.5(24) angstroms³, orthorhombic, Pbnb (Z = 4). Diffraction data (MoK_α radiation, 2θ_max = 50) is collected by Rigaku-AFC6 diffract meter. The structure was solved and refined by direct method and full-matrix least-squares procedures to R-value of 0.0645. The complex ET₃S₆ has been prepared through electrocrystallization ways. The conductivity of this salt at room temperature is 2.3 S cm^-1. It shows weak metallic behavior above 240 K. Below this temperature, it becomes a semiconductor. The XPS spectra indicated the presence of three different kinds of S atoms in the salt. The ESR line width is found to be 44.478 G at room temperature.