Synthesis and Molecular Structure of 4-Methoxyphenyl-2'-pyrrolylthione and its Rhenium Complex
Svetlana, S.V., David Dolphin, van Lier, J.E., and Kudrevich, S.V.
Inorganica Chim. Acta.
A bidentate monoanionic N,S-ligand, 4-methoxyphenyl-2?-pyrrolylthione (1) was synthesised via an oxygen-to-sulphur exchange in the corresponding ketone and then fully characterised. A trinuclear complex (2) of rhenium with this compound was obtained in a reaction of KReO4 with 1 in the presence of a reducing agent in aqueous ethanol, followed by slow precipitation from chloroform–hexane. The structure of compound 2 corresponds to the formula [Re3O4(C12H10NOS)6]+1[ReO-1]•2CH3CH2OH. A single crystal X-ray diffraction study was performed for this complex. The following crystal data were obtained for 2: Mr=2262.556, monoclinic, space group C2/c, a=34.6651(2) Å, b=11.5694(1) Å, c=24.6839(2) Å, β=128.0350(4)o, V=7797.3(1) Å3, Z=4. The molecule contains a linear backbone [O=Re---O---Re---O---Re=O]7+ with six bidentate ligands 1 bonded by three rhenium coordination centres in equatorial planes. Such structures are uncommon for Re (V) complexes with heterocyclic bidentate nitrogen-containing ligands, which often exist as binuclear molecules.