Synthesis, Spectroscopic Study and Crystal Structure Determination by X‐ray Powder Diffractometry of [CdCl2(TzTn)] [TzTn=2‐(3,4‐dichlorophenyl)imino‐N‐(2‐thiazolin‐2‐yl)tetrahydro‐1,3‐thiazine

Abstract

AbstractThe cadmium(II) complex, dichloro[2‐(3,4‐dichlorophenyl)imino‐κN‐N‐(2‐thiazolin‐κN‐2‐yl)tetrahydro‐1,3‐thiazin]cadmium(II), was synthesized in the form of fine powder with small crystals unsuitable for structure determination by X‐ray single‐crystal diffractometry, and was therefore characterized by X‐ray powder diffractometry. To that end, the molecular structure was first analyzed using various instrumental techniques including elemental analysis, FAB‐mass spectroscopy, and infrared spectroscopy, and then optimized via molecular modeling with a semi‐empirical quantum‐chemistry model. From the optimized molecule, the crystal structure wasresolved within the methodological framework of the direct‐space methods using a ‘Monte‐Carlo/parallel tempering’ search algorithm, and then refined using the Rietveld method. It was found that the title compound crystallizes in the triclinic system, with the space group $\rm P{\bar 1}$, two C13H13Cl4CdN3S2 molecules in the asymmetric unit, and the following unit cell dimensions: a = 13.558(4) Å, b = 13.579(7) Å, c = 10.117(4) Å, α = 91.07(3)°, β = 95.44(3)°, and γ = 93.03(3)°. It was also found that the environment around the cadmium(II) ion may be described as distorted tetrahedral, with the metallic atom coordinated to two chlorine atoms [Cd(A)‐Cl(1A) = 2.44(3) Å; Cd(A)‐Cl(2A) = 2.44(3) Å; Cd(B)‐Cl(1B) = 2.45(3) Å; Cd(B)‐Cl(2B) = 2.45(3) Å], one imino nitrogen atom [Cd(A)‐N(3A) = 2.37(10) Å; Cd(B)‐N(3B) = 2.37(9) Å], and one thiazoline nitrogen atom [Cd(A)‐N(1A) = 2.33(8) Å; Cd(B)‐N(1B) = 2.33(10) Å].