High-temperature, high-pressure hydrothermal synthesis, crystal structure, and solid-state NMR spectroscopy of Cs2(UO2)(Si 2O6) and variable-temperature powder X-ray diffraction study of the hydrate phase Cs2(UO2)(Si2O 6)·0.5H2O

Chih Shan Chen, Ray Kuang Chiang, Hsien Ming Kao, Kwang Hwa Lii

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Abstract

A new uranium(VI) silicate, Cs2(UO2)(Si 2O6), 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)(Si2O 6)· 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.

Original languageEnglish
Pages (from-to)3914-3918
Number of pages5
JournalInorganic Chemistry
Volume44
Issue number11
DOIs
StatePublished - 30 May 2005

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