UF 4 and the High‐Pressure Polymorph HP‐UF 4

Abstract A laboratory‐scale synthesis of UF 4 is presented that utilizes the reduction of UF 6 with sulfur in anhydrous hydrogen fluoride. An excess of sulfur can be removed by vacuum sublimation, yielding pure UF 4 , as shown by powder X‐ray diffraction, micro X‐ray fluorescence analysis, infrared...

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Published inChemistry : a European journal Vol. 25; no. 30; pp. 7366 - 7374
Main Authors Scheibe, Benjamin, Bruns, Jörn, Heymann, Gunter, Sachs, Malte, Karttunen, Antti J., Pietzonka, Clemens, Ivlev, Sergei I., Huppertz, Hubert, Kraus, Florian
Format Journal Article
LanguageEnglish
Published 28.05.2019
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Summary:Abstract A laboratory‐scale synthesis of UF 4 is presented that utilizes the reduction of UF 6 with sulfur in anhydrous hydrogen fluoride. An excess of sulfur can be removed by vacuum sublimation, yielding pure UF 4 , as shown by powder X‐ray diffraction, micro X‐ray fluorescence analysis, infrared and Raman spectroscopy, as well as magnetic measurements. Furthermore, a single‐crystalline, high‐pressure modification of UF 4 was obtained in a multi‐anvil press at elevated temperatures. The high‐pressure polymorph HP‐UF 4 was characterized by means of single‐crystal and powder X‐ray diffraction, as well as by magnetic measurements, and presents a novel crystal structure type. Quantum‐chemical calculations show the HP‐modification to be 10 kJ mol −1 per formula unit higher in energy compared to UF 4 .
ISSN:0947-6539
1521-3765
DOI:10.1002/chem.201900639