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Single crystals of Fe0.43Mo2.56SbO9.5 were obtained by hydrothermal techniques at 230 °C. The crystal structure was determined from single crystal X-ray diffraction data. The compound crystallizes in the non-centrosymmetric space group Pc with unit cell parameters a = 4.0003(2) A, b = 7.3355(3) A, c = 12.6985(6) A, β = 90°. The crystal structure comprises five crystallographically independent M atoms and one Sb3+ atom, M atoms are of two kinds of partially occupied sites Mo6+ and Fe3+. The building blocks consist of [SbO3O0.5O0.5E] octahedra (E = lone electron pair) and [(Mo/Fe)O6] octahedra. The M = (Mo, Fe) and O atoms are arranged in a distorted hexagonal 2D-net, not the Sb atoms. The distortion of the net and consequently the symmetry reduction results mainly from the location of the Sb atoms. Disorder manifests itself as a splitting of the metal sites and as a consequent shortening of the Mo–Fe distances. Six (Mo/Fe)O6 octahedra are connected to form a pseudohexagonal channel. The Sb3+ atom is displaced from the pseudo-six-fold axis.

Crystal Structure of the Disordered Non-Centrosymmetric Compound Fe0.43Mo2.56SbO9.5