Synthesis, spectroscopic studies and molecular structure of original halogeno-[S-methyl 3-(2-hydroxyphenylethylidene)dithiocarbazato]oxo-rhenium(V) complexes

摘要

A new neutral rhenium(V)-oxo complex with tridentate Schiff base (SNO-CH_3), derived from the condensation of 2-hydroxyacetophenone with dithiocarbazic acid methyl ester (H_2N-NH-C(=S)SCH_3) was prepared by a substitution reaction on the square pyramidal ionic complex [ReOCl_4][NBu_4]. Reacting the rhenium complex [Re~VO(SNO-CH_3)Cl] 1 with lithium iodide (LiI) allows the formation of the iodo homologous rhenium(V)-oxo complex [Re~VO(SNO-CH_3)I] 2. Compounds 1 and 2 were characterized by elemental analysis, IR, NMR spectra and mass spectrometry (FAB). The structure of [ReO(SNO-CH_3)I] 2 was determined by single X-ray diffraction methods. The coordination around rhenium is distorted square pyramidal with an apical double bonded oxo atom [Re = O: 1.660 A] and the basal ligands bend away from the oxo group.