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Single crystals of ReCl 5  • OPCl 3  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 POCl 3 , 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 ReCl 5  • OPCl 3 , with symmetry C s (m). Bond lengths are Re -O - 214 pm and P-O = 146 pm, the angle Re -O -P is 143°

ReCl 5 • OPCl 3 ; IR-Spektrum und Kristallstruktur / ReCl 5 • OPCl 3 ; IR Spectrum and Crystal Structure