Powder samples of NbOF 3 und TaOF 3 were prepared by heating mixtures of NbO 2 F and NbF 5 or TaO 2 F and TaF 5 , respectively, in the corresponding stoichiometric ratio in platinum crucibles under argon atmosphere (180Ϫ220°C). Both oxide fluorides are coulourless with a slight greyish tinge. They are sensitive to moisture and decompose in air at room temperature within hours.Both, NbOF 3 and TaOF 3 crystallize as a variant of the SnF 4 type structure, space group I4/mmm.