Synthesis and crystal structure of a new layered zirconium phosphate compound, Zr(PO4)F(OSMe2)

Abstract

The crystal structure of a layered zirconium phosphate compound Zr(PO₄)F(OSMe₂) was solved ab initio by using X-ray powder diffraction data and refined by the Rietveld method. It crystallizes in the tetragonal space group P4/n with a= 6.6093(2), c= 9.2371(3)Å and Z= 2. The positions of the metal and the phosphorus atoms were derived from a three-dimensional Patterson map computed using 50 unambiguously indexed powder diffraction intensities. The remaining atoms were located from Fourier-difference maps. The final agreement factors are Rwp= 0.109, Rp= 0.082 and R_F= 0.059. The structure is layered in which the metal atoms and the phosphate groups are located nearly in a plane. All the oxygen atoms of the phosphate group are involved in metal co-ordination. The axial sites of the metal octahedra are occupied by the charge-neutralizing fluoride ion and the oxygen atom of a dimethyl sulfoxide molecule.