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) Å, b=16.086(5) Å, c=17.078(6) Å, α=β=γ=90.00°, V=4131.5(24) Å3, orthorhombic, Pbnb (Z=4). Diffraction data (MoKα radiation, 2θmax=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.