Simultaneous electron diffraction and mass spectrometric study of vapo
r over hydrolyzed NbF5 war carried out. Conditions providing the prese
nce of niobium oxytrifluoride in the gas phase have been revealed and
structural parameters of the NbOF3 molecule, corresponding to the r(al
pha) configuration of C-3v symmetry, have been determined: r(alpha)(Nb
=O) 1.688(7) Angstrom; r(alpha)(Nb-F) 1.861(4) Angstrom; r(alpha)(O-F)
2.857(23) Angstrom; r(alpha)(F-F)3.079(22) Angstrom; L(alpha)(O-Nb-F)
107.1(1.5)degrees; L(alpha)(F-Nb-F) 111.6(1.4)degrees.