High-temperature, high-pressure hydrothermal synthesis, crystal structures, and spectroscopic studies of a uranium(IV) phosphate (Na10U 2P6O24) and the isotypic cerium(IV) phosphate (Na10Ce2P6O24)

Yu Hsien Lai, Yu Chih Chang, Tsz Fung Wong, Wan Ju Tai, Wen Jung Chang, Kwang Hwa Lii

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Abstract

A uranium(IV) phosphate, Na10U2P6O 24, was synthesized under hydrothermal conditions at 570 C and 160 MPa and structurally characterized by single-crystal X-ray diffraction. The valence state of uranium was established by UV-vis and U 4f X-ray photoelectron spectroscopy. The powder sample has a second-harmonic-generation signal, confirming the absence of a center of symmetry in the structure. The structure contains UO8 snub-disphenoidal polyhedra that are linked to monophosphate tetrahedra by vertex and edge sharing such that a three-dimensional framework with intersecting 12-sided circular and rectangular channels is formed. All 10 sodium sites are situated inside the channels and are fully occupied. This is the first uranium(IV) phosphate synthesized under high-temperature, high-pressure hydrothermal conditions. The isotypic cerium(IV) phosphate, Na10Ce2P6O24, was also synthesized under the same hydrothermal conditions. It is the first structurally characterized Ce(IV) phosphate with a P/Ce ratio of 3. Crystal data of Na 10U2P6O24: orthorhombic, P2 12121 (No. 19), a = 6.9289(3) Å, b = 16.1850(7) Å, c = 18.7285(7) Å, V = 2100.3(2) Å3, Z = 4, R1 = 0.0304, and wR2 = 0.0522. Crystal data of Na10Ce2P6O24: orthorhombic, P2 12121 (No. 19), a = 6.9375(14) Å, b = 16.215(3) Å, c = 18.765(4) Å, V = 2111.0(7) Å3, Z = 4, R1 = 0.0202, and wR2 = 0.0529.

Original languageEnglish
Pages (from-to)13639-13643
Number of pages5
JournalInorganic Chemistry
Volume52
Issue number23
DOIs
StatePublished - 2 Dec 2013

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