Abstract: | Formation and Vibrational Spectrum of the Pentachloro-oxo-niobate(V) Ion. Crystal Structure of As(C6H5)4]2NbOCl5 · 2 CH2Cl2 As(C6H5)4]2NbOCl5 is formed by reaction of NbOCl3 with As(C6H5)4]Cl in CH2Cl2; form the solution it crystallizes with two molecules of CH2Cl2. The i.r. and Raman spectrum is in accord with a NbOCl5 ion of symmetry 4mm. The crystals are triclinic (space group P1 ) with the lattice constants a = 1043, b = 1187, c = 2269 pm, α = 97.4, β = 106.3 and γ = 101.4°. The crystal structure was determined with X-ray diffraction data and refined to a residual index of R = 0.042. In the structure there are two of each crystallographic independent As(C6H5)4+ ions and CH2Cl2 molecules. The NbOCl5 ion has an octahedral shape with a Nb? O distance of 197 pm. |