Abstract

The first structurally characterised oxomolybdenum(V) complexes with thienyl carboxylate ligands were prepared by the reaction of [Mo 2O 3(C 5H 7O 2) 4] or (NH 4) 2[MoOCl 5] with the corresponding acid (2-thiophenecarboxylic, 5-methyl-2-thiophenecarboxylic or 3-(3-thienyl)acrylic acid). Complexes [Mo 2O 3(μ-OC 2H 5)(μ-O 2CR)(C 5H 7O 2) 2](R = –C 4H 3S ( 1), –C 4H 2S(CH 3) ( 2) or –CH CHC 4H 3S ( 3)) were obtained upon substitution of two acetylacetonate ligands from [Mo 2O 3(C 5H 7O 2) 4] with RCOO − in dry ethanol. Reactions of (NH 4) 2[MoOCl 5] with the corresponding thienyl carboxylic acid in the presence of γ-picoline (C 6H 7N) yielded complexes (C 6H 7NH)[Mo 2O 4(μ-O 2CR)Cl 2(C 6H 7N) 2] (R = –C 4H 3S ( 4), –C 4H 2S(CH 3) ( 5) or –CH CHC 4H 3S ( 6)). All of the six new complexes were characterised as dinuclear. The molecular structures of 1, 3, 4· 0. 5CH 3CN and 5 were determined by the single crystal X-ray diffraction method. In the complexes the two molybdenum atoms are doubly bridged either by one oxygen and one ethoxy-oxygen, or alternatively by two oxo-oxygens, and are additionally bridged by the thienyl carboxylate ion in a didentate bridging manner. All complexes were further characterised by means of chemical analysis, IR spectroscopy, TG and in some cases by the one and two-dimensional NMR method.

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