A synthetic and structural study of oxorhenium(v) complexes with mixed didentate (o, o)‐terdentate(o, n, n) ligands

Abstract The reaction of cis-[ReOCl2(L3)] (L3− = terdentate O, N, N-donor ligand 2-[[{2-(2-pyr-idinyl)ethyl}amino]methyl]phenolate) with ethylene glycol (H2eg) in acetonitrile led to the isolation of [ReO(L3)(eg)]. The analogous complexes [ReO(L3)(cat)] (H2cat = 1, 2-dihydroxybenzene) and [ReO(L3)(ox)] (H2ox = oxalic acid) could not be prepared by this method. [ReO(L3)(cat)] was synthesized by the one-pot reaction of [ReOCl4 −] with a twofold molar excess of HL3 and H2cat in ethanol, and [ReO(L3)(ox)] was isolated from the reaction of [ReO(L3)(eg)] and H2ox in acetonitrile. All complexes were characterized by various physical techniques, including IR and NMR. The X-ray crystal structure of [ReO(L3)(cat)l/2EtOH] was determined. Crystals are triclinic, P, a = 8.920(2), b = 11.209(5), c = 11.735(5)A, α = 78.00(4), β = 68.93(3), γ = 86.49(3)°, Z = 2. The structure was solved by the Patterson method and refined by full-matrix least-squares procedures to R = 0.047 (Rw = 0.066) for 2321 reflections with F 0 > 3[...