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Synthesis and Characterization of Manganese Tetrafluoride β‐MnF 4
Author(s) -
Kraus Florian,
Ivlev Sergei I.,
Bandemehr Jascha,
Sachs Malte,
Pietzonka Clemens,
Conrad Matthias,
Serafin Michael,
Müller Bernd G.
Publication year - 2020
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.202000048
Subject(s) - crystal structure , crystallography , manganese , octahedron , raman spectroscopy , impurity , thermal decomposition , materials science , powder diffraction , lattice (music) , chemistry , physics , organic chemistry , acoustics , optics , metallurgy
The crystal structure of β‐MnF 4 has finally been elucidated. It crystallizes in the non‐centrosymmetric space group R 3 c , no. 161, h R 360, with the lattice parameters a = 19.390(3), c = 12.940(3) Å, V = 4213.3(14) Å 3 , Z = 72, T = 100 K. It is a 4 a × 4 a superstructure of the VF 3 (FeF 3 ) structure type. The Mn atoms are coordinated octahedron‐like by F atoms, of which two are bound terminal, while the other act as μ‐bridging F atoms to other Mn atoms forming a three‐dimensional infinite network structure which can be described by the Niggli formula 3 ∞ [MnF 4/2 F 2/1 ]. Voids on the metal sites, which are occupied in the VF 3 structure, are grouped together in the shape of a “star” with approximate D 3 h symmetry. We prepared β‐MnF 4 photochemically according to the literature and obtained a phase‐pure powder as evidenced by X‐ray diffraction at room temperature. The lattice parameters are a = 19.566(3), c = 12.984(2) Å, V = 4304(1) Å 3 . IR and Raman spectra recorded on the powder show that β‐MnF 4 has also been obtained free of moisture, HF, and O 2 + containing compounds, however MnF 3 is likely present as a magnetic impurity. We observe thermal decomposition of MnF 4 to MnF 2 and not MnF 3 .