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Journal of Structural Chemistry

2013 year, number 6

CRYSTAL ARCHITECTURE AND THERMAL DECOMPOSITION OF TWO NEW ORGANICALLY TEMPLATED CADMIUM SULFATES

R. Jlassi1, W. Rekik1, H. NaГЇli1, T. Mhiri1, T. Bataille2
1Laboratoire Physico-Chimique de l'Г©tat Solide, DГ©partement de Chimie, FacultГ© des Sciences de Sfax, UniversitГ© de Sfax, Sfax, Tunisia
2Sciences Chimiques de Rennes (CNRS, UMR 6226), UniversitГ© de Rennes 1, Rennes Cedex, France
Keywords: hybrid material, slow evaporation, X-ray diffraction, crystal structure, thermal decomposition, supramolecular

Abstract

Two organic-inorganic hybrid compounds (C 5H 14N 2)[Cd(H 2O) 6](SO 4) 2 (I) and R-(C 5H 14N 2) [Cd(H 2O) 6](SO 4) 2 (II) are synthesized by the slow evaporation method and characterized by single crystal X-ray diffraction, thermogravimetry, temperature-dependent X-ray diffraction, and infrared spectroscopy. The first compound crystallizes in the centrosymmetric space group P 2 1/ n with the following unit cell parameters: a = 6.6208(2) Å, b = 10.6963(3) Å, c = 12.9318(4) Å, V = 893.05(6) Å 3, and Z = 2. Its structure is solved by direct methods and refined by the least-squares analysis [ R 1 = 0.0389 and wR 2 = 0.0821]. This compound shows a crystallographic disorder II destroys the inversion symmetry and leads to a fully ordered structure. Indeed, compound II crystallizes in the non-centrosymmetric space group P 2 1 with the following unit cell parameters: a = 6.6306(1) Å, b = 10.7059(2) Å, c = 12.9186(1) Å, V = 894.67(2) Å 3, and Z = 2. The crystal structure of both compounds is built from isolated anions, disordered 2-methylpiperazinediium, (C 5H 14N 2) 2+ in compound I or R-2-methylpiperazinediium R-(C 5H 14N 2) 2+ in compound II, and divalent metal cations surrounded by six water molecules. These different entities are connected together only by a 3D hydrogen bond network. The thermodiffractometry and the thermogravimetric analyses indicate that the decomposition of the supramolecular precursors proceeds through several stages leading to cadmuim oxide.