Synthesis and characterization of oxorhenium(V) complexes with an amine-amide-dithiol ligand. X-ray crystal structure of [N-(1-carboethoxy-2-thioethyl)-[N-(2-thioethyl)amino]acetimido]oxorhenium(V)

The preparation of N-(1-carboethoxy-2-thioethyl)[N-(2-thioethyl)amino]- acetamide (H4L) and its ligand-exchange reaction with ReO(PPh3)(2)Cl-3 are described. Two complexes, ReOHL and [Et3NH][ReOL], were formed depending on the extent of deprotonation of H4L during complexation. The structure of ReOHL was determined by single-crystal X-ray analysis. ReOHL crystallizes in the orthorhombic space group P2(1)2(1)2(1) with a = 10.4526(2) Angstrom, b = 11.5702(0) Angstrom, c = 12.0118(2) Angstrom, V = 1452.69(4) Angstrom(3), Z = 4, DC = 2.129 Mg/m(3), F(000) = 888 and R = 0.0216 for 2384 unique reflections. The coordination environment was approximately scquare-pyramidal with an amine N, a deprotonated amide N and two deprotonated thiol S atoms coordinated in the basal plane and the oxo ligand in the apical position.