“…␦ in BiO ␦ F 3−2␦ can be as low as 0.02; hence, although the high-energy milling was conducted under He, it is possible that some oxygen anions, present as an impurities, stabilized the tysonite form. According to Ardashnikova et al, 14 a thermal treatment at 350°C in an inert atmosphere causes the metastable high-pressure fluoride to transform back into the orthorhombic form whereas the oxyfluoride remains stable. Our material did transform into orthorhombic BiF 3 during annealing, supporting the fact that this is indeed the high-pressure tysonite BiF 3 as opposed to the oxyfluoride.…”