Structure and internal dynamics of bis(piperazine-1,4-diium) pentachloroantimonate (III) monohydrate
Ouled Mohamed Sghaier M.2, Hołderna-Natkaniec K.1, Czarnecki P.1, Woźniak-Braszak A.1, Chaabouni S.2
- 1Faculty of Physics, Adam Mickiewicz University, 61-614 Poznań, Umultowska 85, Poland
- 2Laboratory of Materials Science and Environment, Faculty of Sfax, BP 1171, 3000 Sfax, Tunisia
Polyhedron, 79, pp.37-42, 2014
DOI:: 10.1016/j.poly.2014.04.030
Abstract:
Bis(piperazine-1,4-diium) pentachloroantimonate (III) monohydrate, has been synthesized and characterized by X-ray diffraction at 293 K, thermogravimetric analysis (TGA), differential thermal analysis (DTA), IR and Raman measurements. It crystallizes in the monoclinic system with space group P21/n. The unit cell dimensions are: a = 9.5409(2) Å, b = 14.1455(1) Å, c = 10.0525(7) Å, β = 99.113(8)°, with Z = 4. The molecule of this compound consists of piperazine-1,4-diium cation, [SbCl5]2- anions and water molecules. The distorted [SbCl5]2- square pyramids sharing two common Cl atoms are held together making bioctahedra of the form [Sb2Cl10]4-. The compound is stabilized by intermolecular N-H⋯Cl, O-H⋯Cl and N-H⋯O hydrogen bridge bonds. Analysis of dielectric spectroscopy permitted identification of a phase transitions at: 70 K. At 372 K dehydration takes place, while at 509 K the process of decomposition starts [24]. The 1H NMR measurements were performed in a broad temperature range. The data are interpreted in terms of different dynamics of piperazine cation and crystallization water in different environments. © 2014 Elsevier Ltd. All rights reserved.
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