Synthesis, crystal structure, phase transition and thermal behaviour of a new dabcodiium hexaaquanickel(II) bis(sulphate), (C6H14N2)[Ni(H2O)6](SO4)2 |
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Authors: | W Rekik H Naïli T Bataille |
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Institution: | a Laboratoire de l’Etat Solide, Département de Chimie, Faculté des Sciences de Sfax, BP 802, 3018 Sfax, Tunisia b Sciences Chimiques de Rennes (CNRS, UMR 6226), Groupe Matériaux Inorganiques: Chimie Douce et Réactivité, Université de Rennes I, Avenue du Général Leclerc, 35042 Rennes Cedex, France |
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Abstract: | A new dabcodiium-templated nickel sulphate, (C6H14N2)Ni(H2O)6](SO4)2, has been synthesised and characterised by single-crystal X-ray diffraction at 20 and −173 °C, differential scanning calorimetry (DSC), thermogravimetry (TG) and temperature-dependent X-ray powder diffraction (TDXD). The high temperature phase crystallises in the monoclinic space group P21/n with the unit-cell parameters: a = 7.0000(1), b = 12.3342(2), c = 9.9940(2) Å; β = 90.661(1)°, V = 862.82(3) Å3 and Z = 2. The low temperature phase crystallises in the monoclinic space group P21/a with the unit-cell parameters: a = 12.0216(1), b = 12.3559(1), c = 12.2193(1) Å; β = 109.989(1)°, V = 1705.69(2) Å3 and Z = 4. The crystal structure of the HT-phase consists of Ni2+ cations octahedrally coordinated by six water molecules, sulphate tetrahedra and disordered dabcodiium cations linked together by hydrogen bonds. It undergoes a reversible phase transition (PT) of the second order at −53.7/−54.6 °C on heating-cooling runs. Below the PT temperature, the structure is fully ordered. The thermal decomposition of the precursor proceeds through three stages giving rise to the nickel oxide. |
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Keywords: | Chemical synthesis Crystal structure Phase transition Order-disorder Thermal behaviour Organometallic |
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