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UF 4 and the High‐Pressure Polymorph HP‐UF 4
Author(s) -
Scheibe Benjamin,
Bruns Jörn,
Heymann Gunter,
Sachs Malte,
Karttunen Antti J.,
Pietzonka Clemens,
Ivlev Sergei I.,
Huppertz Hubert,
Kraus Florian
Publication year - 2019
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201900639
Subject(s) - anhydrous , raman spectroscopy , sublimation (psychology) , powder diffraction , analytical chemistry (journal) , single crystal , diffraction , materials science , x ray crystallography , sulfur , crystal structure , crystallography , chemistry , psychology , physics , organic chemistry , optics , psychotherapist , chromatography , metallurgy
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 .
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