ReCl5 • OPCl3; IR-Spektrum und Kristallstruktur / ReCl5 • OPCl3; IR Spectrum and Crystal Structure

Abstract

Single crystals of ReCl5 • OPCl3 were obtained by cooling a saturated solution of rheniumpentachloride in phosphorylchloride. It formes black needles, which are extremely sensitive to moisture. In the IR spectrum ν(PO) is shifted downwards by 140 cm-1 in comparison with liquid POCl3, indicating coordination via oxygen. The crystal structure was solved and refined from Xray diffraction data (space group Pnma, four formula units per unit cell, a = 1629, b = 790, c = 877 pm, 902 observed, independent reflexions, R = 0.040). The complex forms discrete molecules ReCl5 • OPCl3, with symmetry Cs(m). Bond lengths are Re -O - 214 pm and P-O = 146 pm, the angle Re -O -P is 143°