Redetermination of the crystal structure of NbF4

Abstract

Single crystals of NbF4, niobium(IV) tetrafluoride, were synthesized by disproportionation of Nb2F5 at 1273K in a sealed niobium tube, extracted and studied by single-crystal X-ray diffraction. Previous reports on the crystal structure of NbF4 were based on X-ray powder diffraction data and the observed isotypicity to SnF4 [Gortsema & Didchenko (1965). Inorg. Chem. 4, 182-186; Schäfer et al. (1965). J. Less Common Met. 9, 95-104]. The data obtained from a single-crystal X-ray diffraction study meant the atomic coordinates could now be refined as well as their anisotropic displacement parameters, leading to a significant improvement of the structural model of NbF4. In the structure, the Nb atom is octahedron-like surrounded by six F atoms of which four are bridging to other NbF6 octahedra, leading to a layer structure extending parallel to the ab plane.