Single-Crystal Structure of HP-Sc<sub>2</sub>TeO<sub>6</sub> Prepared by High-Pressure/High-Temperature Synthesis

oleh: Raimund Ziegler, Martina Tribus, Clivia Hejny, Gunter Heymann

Format: Article
Diterbitkan: MDPI AG 2021-12-01

Deskripsi

The first high-pressure scandium tellurate HP-Sc<sub>2</sub>TeO<sub>6</sub> was synthesized from an NP-Sc<sub>2</sub>TeO<sub>6</sub> normal-pressure precursor at 12 GPa and 1173 K using a multianvil apparatus (1000 t press, Walker-type module). The compound crystallizes in the monoclinic space group <i>P</i>2/<i>c</i> (no. 13) with <i>a</i> = 729.43(3), <i>b</i> = 512.52(2), <i>c</i> = 1095.02(4) pm and <i>β</i> = 103.88(1)°. The structure was refined from X-ray single-crystal diffractometer data: <i>R</i><sub>1</sub> = 0.0261, <i>wR</i><sub>2</sub> = 0.0344, 568 <i>F</i><sup>2</sup> values and 84 variables. HP-Sc<sub>2</sub>TeO<sub>6</sub> is isostructural to Yb<sub>2</sub>WO<sub>6</sub> and is built up from TeO<sub>6</sub> octahedra, typical for tellurate(VI) compounds. During synthesis, a reconstructive transition from <i>P</i>321 (normal-pressure modification) to <i>P</i>2/<i>c</i> (high-pressure modification) takes place and the scandium–oxygen distances as well as the coordination number of scandium increase. However, the coordination sphere around the Te<sup>6+</sup> cations gets only slightly distorted. High-temperature powder XRD investigations revealed a back-transformation of HP-Sc<sub>2</sub>TeO<sub>6</sub> to the ambient-pressure modification above 973 K.