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Synthesis and Characterization of A [W 2 O 2 F 9 ] ( A = Li – Cs)
Author(s) -
Stene Riane E.,
Scheibe Benjamin,
Karttunen Antti J.,
Petry Winfried,
Kraus Florian
Publication year - 2020
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.202000289
Subject(s) - chemistry , raman spectroscopy , alkali metal , crystallography , salt (chemistry) , crystal structure , lewis acids and bases , single crystal , metal , x ray crystallography , infrared spectroscopy , characterization (materials science) , diffraction , catalysis , nanotechnology , organic chemistry , materials science , physics , optics
Herein, we report upon the in situ formation of WOF 4 and its subsequent reaction with A F ( A = Li – Cs) in aHF to produce A [W 2 O 2 F 9 ] ( A = Li – Cs). Structural analysis of the obtained compounds was performed using single‐crystal X‐ray diffraction. A comparison of the single‐crystal structures obtained here to the previously reported A [Mo 2 O 2 F 9 ] ( A = Li – Cs) and H 3 O[W 2 O 2 F 9 ] salts is given. Additionally, IR and Raman spectroscopy were used to characterize each salt. These spectra were compared to calculated ones for the solid‐state structure of each salt using the DFT‐PBE0 density functional method. The calculated spectra were used to assign bands in the experimental spectra. Both MoOF 4 and WOF 4 gave similar reaction products under similar reaction conditions. It was concluded that the oxyfluorides show similar Lewis acid‐base reactions with the alkali metal fluorides in aHF solutions.