Tribromohydroxyphosphonium hexafluorometalate: synthesis, spectroscopic characterization, and crystal structure of Br(3)POH(+)AsF(6)(-)

The reaction of tribromophosphine oxide in the superacidic systems XF/MF(5) (X = H, D; M = As, Sb) leads to tribromohydroxyphosphonium hexafluorometalates. The structure was successfully elucidated in the case of tribromohydroxyphosphonium hexafluoroarsenate. Br(3)POH(+)AsF(6)(-) crystallizes in the orthorhombic space group Pnma (No. 53 with a = 1292.5(1) pm, b = 871.6(1) pm, and c = 845.0(1) pm) with four formula units per cell. The Raman, IR, (1)H NMR, and (31)P NMR spectra of Br(3)POX(+)MF(6)(-) (X = H, D; M = As, Sb) are reported.