AbstractThe new niobium oxide fluorides MNbO2F4 [M = (Cr, Fe)], CrNb2O4F5, and Fe2Nb3O6F9 were prepared by treatment of chromium or iron nitrate with Nb-containing hydrofluoric acid solutions. Crystal structures were investigated by means of X-ray powder diffraction. All new compounds can be structurally refined in the cubic ReO3-type. The iron niobium oxide fluorides are reddish orange, and chromium containing phases exhibit a light green color. The niobium atoms are in the highest formal oxidation state.