Synthesis, molecular characterization by infrared spectroscopy, and crystal structure determination by X-ray powder diffractometry of [ZnCl2(TdTz)] [TdTz=2-(3,4-dichlorophenyl)imino-N-(2-thiazin-2-yl)thiazolidine

Abstract

Abstract The title zinc(II) complex, dichloro[2-(3,4-dichlorophenyl)imino-κN-N-(2-thiazin-κN-2-yl)thiazolidine]zinc(II), was synthesized in the form of small crystals unsuitable for structure determination by X-ray single-crystal diffractometry. It was therefore characterized firstly in the solid state by elemental analysis and infrared spectroscopy, and then its crystal structure was determined by X-ray powder diffractometry. The procedure followed to resolve the crystal structure used direct-space methods with a ‘Monte Carlo/parallel tempering’ search algorithm, where the starting configuration was obtained by means of infrared spectroscopy and molecular mechanics. A final refinement of the crystal structure was performed using the Rietveld method. It was found that the environment around the zinc(II) ion may be described as a distorted tetrahedral geometry, with the metallic atom coordinated to two chlorine atoms [Zn–Cl(1) = 2.158(5) A; Zn–Cl(2) = 2.145(4) A], one imino nitrogen [Zn–N(3) = 2.237(4) A] and one thiazine nitrogen [Zn–N(1) = 2.273(5) A]. In addition, we also report in this study the crystal structure of the 2-(3,4-dichlorophenyl)imino-N-(2-thiazin-2-yl)thiazolidine (TdTz) ligand determined by X-ray single-crystal diffractometry.