Synthesis and redetermination of the crystal structure of NbF.

Single crystals of NbF, niobium(V) fluoride, have been obtained by the reaction of niobium metal in a stream of dilute elemental fluorine at 473 K and subsequent sublimation. The as-obtained bulk phase compound was shown to be pure by powder X-ray diffraction at 293 K and by IR and Raman spectroscopy. A single-crystal X-ray analysis was conducted at 100 K. In comparison to the previously reported structure model [Edwards (1964 ▸). pp. 3714-3718], the lattice parameters and fractional atom coordinates were determined to much higher precision and individual, anisotropic displacement parameters were refined for all atoms.