Synthese und Kristallstruktur von PPh4[ReF2Cl2(N2S2)] / Synthesis and Crystal Structure of PPh4[ReF2Cl2(N2S2)]

Abstract

PPh4[ReF2Cl2(N2S2)] has been prepared by the reaction of PPh4[ReCl4(NSCl)2] · CH2Cl2 with sodium fluoride in acetonitrile suspension. The compound forms black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 2525 observed unique reflexions, R = 0.053. Lattice dimensions at 20°C: a = 1277.4(3), b = 713.2(3), c = 2860.8(4) pm. β = 97.20(3)°. The compound consists of PPh4 + and [ReF2Cl2(N2S2)]- ions, in which the rhenium atom is surrounded octahedrally by two fluorine atoms, two chlorine atoms, and by the nitrogen atoms of a ReN2S2 five-membered ring, the fluorine ligands being in trans position to the N atoms. The bond lengths ReN (172; 177 pm) and NS (155; 160 pm) are in the range of double bonds, the S—S bond is relatively long (243 pm).