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CTURE OF INORGANIC COMPOUNDS

Synthesis and Structure of Zinc Iodide Complex with Thiocarbamide, [Zn(CH4N2S)2I2] D. V. Albova, E. A. Buravlevb, E. V. Savinkinab, and I. A. Zamilatskovb a

b

Faculty of Chemistry, Moscow State University, Moscow, 119992 Russia Moscow State University of Fine Chemical Technology, pr. Vernadskogo 86, Moscow, 119571 Russia email: [email protected] Received March 25, 2012

Abstract—A complex compound of zinc iodide with thiocarbamide [Zn(CH4N2S)2I2] is obtained and its structure is studied by Xray diffraction. Crystals are monoclinic, a = 10.494(2) Å, b = 7.473(2) Å, c = 14.871(4) Å, β = 91.354(18)°, V = 1165.9(5) Å3, space group P21/c, Z = 4. The structural unit of the crystal is molecular complex [Zn(CH4N2S)2I2], in which the zinc atom is coordinated by sulfur atoms of two thio carbamide molecules and two iodine atoms. DOI: 10.1134/S1063774513010033

INTRODUCTION

Table 1. Crystal data, parameters of data collection, and char acteristics of the structure refinement of [Zn(CH4N2S)2I2]

This work is part of our study of the interaction between iodides of group 12 elements and amides and thioamides and a determination of the structure of the complex compounds that were obtained [1–6]. Com plex compounds of cadmium halides with thiocarba mide [Cd(CH4N2S)2X2] (X = Cl, Br, or I) have similar molecular structures [7, 8]: the metal atom is tetrahe drally coordinated by two halogen atoms and sulfur atoms of two thiocarbamide molecules. The [Zn(CH4N2S)2Cl2] complex of zinc chloride with this ligand has an analogous structure [9]. The structure of cadmium chloride with thiocarbamide of a different composition [Cd(CH4N2S)4Cl2] was described in [10]. In this compound, the cadmium atom is octahedrally coordinated by four thiocarbamide molecules and two chlorine atoms. The aim of this work is to synthesize a complex of zinc iodide with thiocarbamide and deter mine its crystal structure.

Crystal system, space group, Z Monoclinic, P21/c, 4 a, b, c, Å 10.4940(19), 7.473(2), 14.871(4) β, deg 91.354(18) V, Å3 1165.9(5) 3 Dx , g/cm 2.686 AgKα , 0.56087 Radiation, λ, Å –1 μ, mm 4.066 T, К 293(2) Crystal size, mm 0.30 × 0.30 × 0.30 Diffractometer EnrafNonius CAD4 ω/2θ Scan mode θmax, deg 28.44 –10 ≤ h ≤ 10, 0 ≤ k ≤ 7, Limiting indices h, k, l 0 ≤ l ≤ 14 Number of reflections: mea 1220/1159/924 sured/unique/with I > 2σ(I) Refinement method Least squares on F2 Number of reduced pa 100 rameters 2 Weighting scheme 1/[s2( F o ) + (0.100P)2],

EXPERIMENTAL In order to prepare complex [Zn(CH4N2S)2I2], zinc iodide (1.00 g, 3.13 mmol) and thiocabamide (0.48 g, 6.26 mmol) were dissolved in water (10 ml). The resulting solution was allowed to stand in air up to the precipitation of colorless crystals (yield 65%). The Xray diffraction study of the crystals was per formed. The crystal data, parameters of data collec tion, and characteristics of structure refinement are given in Table 1. The refinement was performed with the SHELXL97 program package [11]. The IR spectrum of complex [Zn(CH4N2S)2I2] in va