The reaction between PCl3 and ReCl5 yielded at 200 degrees C the ionic tetr
achlorophosphonium dirhenium nonachloride, (PCl4)[Re2Cl9]. Single crystal X
-ray diffraction analysis revealed a monoclinic unit cell: a = 8.616(3) Ang
strom, b = 10.449(4) Angstrom, c = 9.397(3) Angstrom, beta = 99.72(3)degree
s, V = 833.9(5) Angstrom(3), Z = 2, sp. gr. P2(1)/m, wR(2) = 0.1083 and R-1
= 0.0527. The ionic compound is built from tetrahedra PCl4+ and face-shari
ng bioctahedra Re2Cl9-. The Re-Re distance, 2.724 Angstrom, indicates the p
resence of direct Re-Re interaction.