X-ray diffraction, Cs and H NMR and thermal studies of CdZrCs1.5(H3O)0.5(C2O4)4·xH2O displaying Cs and water dynamic behavior |
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Authors: | E. Jeanneau,B. Bureau,D. Louë r |
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Affiliation: | a Laboratoire de Chimie du Solide et Inorganique Moléculaire (UMR 6511 CNRS), Institut de Chimie, Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France b Laboratoire Verres et Céramiques (UMR 6512 CNRS), Institut de Chimie, Université de Rennes, Avenue du Général Leclerc, 35042 Rennes cedex, France |
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Abstract: | A novel mixed cadmium zirconium cesium oxalate with an open architecture has been synthesized from precipitation methods at room pressure. It crystallizes with an hexagonal symmetry, space group P3112 (no. 151), a=9.105(5) Å, c=23.656(5) Å, V=1698(1) Å3 and Z=3. The structure displays a [CdZr(C2O4)4]2− helicoidal framework built from CdO8 and ZrO8 square-based antiprisms connected through bichelating oxalates, which generates channels along different directions. Cesium cations, hydronium ions and water molecules are located inside the voids of the anionic framework. They exhibit a dynamic disorder which has been further investigated by 1H and 133Cs solid-state NMR. Moreover a phase transition depending both upon ambient temperature and water vapor pressure was evidenced for the title compound. The thermal decomposition has been studied in situ by temperature-dependent X-ray diffraction and thermogravimetry. The final product is a mixture of cadmium oxide, zirconium oxide and cesium carbonate. |
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Keywords: | C. X-ray diffraction D. Crystal structure D. Nuclear magnetic resonance D. Phase transitions |
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