High-Temperature, High-Pressure Hydrothermal Synthesis, Crystal Structure, and Solid-State NMR Spectroscopy of Cs<sub>2</sub>(UO<sub>2</sub>)(Si<sub>2</sub>O<sub>6</sub>) and Variable-Temperature Powder X-ray Diffraction Study of the Hydrate Phase Cs<sub>2</sub>(UO<sub>2</sub>)(Si<sub>2</sub>O<sub>6</sub>)·0.5H<sub>2</sub>O
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A new uranium(VI) silicate, Cs2(UO2)(Si2O6), has been synthesized by a high-temperature, high-pressure hydrothermal method and characterized by single-crystal X-ray diffraction and solid-state NMR spectroscopy. It crystallizes in the orthorhombic space group Ibca (No. 73) with a = 15.137(1) Å, b = 15.295(1) Å, c = 16.401(1) Å, and Z = 16. Its structure consists of corrugated achter single chains of silicate tetrahedra extending along the c axis linked together via corner-sharing by UO6 tetragonal bipyramids to form a 3-D framework which delimits 8- and 6-ring channels. The Cs+ cations are located in the channels or at sites between channels. The 29Si and 133Cs MAS NMR spectra are consistent with the crystal structure as determined from X-ray diffraction, and the resonances in the spectra are assigned. Variable-temperature in situ powder X-ray diffraction study of the hydrate Cs2(UO2)(Si2O6)·0.5H2O indicates that the framework structure is stable up to 800 °C and transforms to the structure of the title compound at 900 °C. A comparison of related uranyl silicate structures is made.
