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Synthesis and Characterization of the Hexafluoridomolybdates(V) A [MoF 6 ] ( A = Li – Cs)
Author(s) -
Stene Riane E.,
Scheibe Benjamin,
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.202000141
Subject(s) - chemistry , anhydrous , tetragonal crystal system , alkali metal , crystal structure , crystallography , inorganic chemistry , hydrogen fluoride , phase (matter) , x ray crystallography , diffraction , organic chemistry , physics , optics
The hexafluoridomolybdates(V), A [MoF 6 ] ( A = Li – Cs), were synthesized by reacting molybdenum pentafluoride (MoF 5 ) with the alkali metal fluorides in anhydrous hydrogen fluoride (aHF) solution. Single crystals of A [MoF 6 ] ( A = Li, Na, Rb, Cs) were grown from solution and analyzed by single‐crystal X‐ray diffraction. The vibrational spectrum of each salt is reported in detail and compared to previously reported spectra. During analysis of the cubic modification of Na[MoF 6 ] it was noticed that a phase transition occurs around 228 K. Some details regarding this phase transition are discussed. Attempts to determine the structure of the low‐temperature phase of Na[MoF 6 ] lead to the observation of the Na[MoF 6 ] · 2HF solvate. Additionally, in an attempt to synthesize Na[MoF 7 ] by the oxidation of Na[MoF 6 ] in chlorine trifluoride (ClF 3 ), a tetragonal modification of Na[MoF 6 ] was observed. The crystal structures of the Na[MoF 6 ] · 2HF solvate and tetragonal modification of Na[MoF 6 ] are also discussed in detail.