Studies on peroxomolybdates XVII. Synthesis and structure of tri(ammonium) fluoride difluorooxodiperoxomolybdate(VI), (NH 4) 3F[MoF 2O(O 2) 2

Abstract

The crystal structure of tri(ammonium) fluoride difluorooxodiperoxomolybdate(VI), (NH 4) 3F[MoF 2O(O 2) 2], was determined using single-crystal X-ray diffraction methods. The yellow compound crystallizes in the orthorhombic space group P2 12 12 1 with a = 6.745(3) A ̊ , b = 8.718(3) A ̊ , c = 15.427(5) A ̊ and Z = 4 . Reflection intensities were recorded at room temperature on a Syntex P2 1 diffractometer using Mo Kα radiation. Full-matrix least-squares refinement yielded a final R value of 0.026 for 1474 observed ( I > 3 σ( I)) reflections. In the complex anion the coordination geometry is pentagonal bipyramidal. Bond distances are as follows: Mo = O apical 1.679(3) Å, MoO peroxo 1.915(4)-1.969(3) Å, MoF equatorial 1.960(3) Å, MoF apical 2.150(2) Å and (OO) peroxo 1.471(6)-1.481(5) Å. The powder photograph of the title compound was recorded at room temperature and was indexed.