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Impact of Group 13 Metals on Cp2TiCl2 Reduction and Structural Characterization of Resulting Compounds

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posted on 02.03.2017, 15:24 by Rafał Petrus, Józef Utko, Tadeusz Lis, Piotr Sobota
The aim of the current study was to examine the effects of group 13 metals on Cp2TiCl2 reduction in the presence of 2-methoxy­ethanol (MeO­Et­OH) or ethanol (EtOH) and the compositions of the resulting products. Direct reaction of Cp2TiCl2 and M [Al, Al (Fe contaminated), Ga, In] in toluene/​alcohol for 2 h gave a new family of uncommon homo- and heterometallic compounds: [Cp2­Ti2Al­(μ,η2-OEt­OMe)4­Cl2]­[Ti2­(μ,η2-OEt­OMe)3­(η2-OEt­OMe)2­Cl4] (1), [Cp2­Ti2Al­(μ,η2-OEt­OMe)4­Cl2]Cl (2), [Cp2­Ti2Al­(μ,η2-OEt­OMe)4­Cl2]­[Cp2Ti­(η2-HOEt­OMe)]­[FeCl4] (3), [Cp2Ti­(η2-HOEt­OMe)]­[Ga2Cl6]0.25­[Cl]0.5 (4), [Cp3Ti2­(μ-OEt)2­(OEt)]­[GaCl4] (5), [CpTi­(μ,η2-OEt­OMe)­Cl]2 (6), and [Cp3Ti2­(μ,η2-OEt­OMe)­(μ-OEt­OMe)­Cl] (7). The reaction with indium for 48 h resulted in isolation of [TiIn2­(μ,η2-OEt­OMe)4­(OEt­OMe)2­Cl4] (8), [In2­(μ-OEt­OMe)2­(HOEt­OMe)4­Cl4]2 (9), and [Ti­(OEt­OMe)4] (10). The complexes were characterized using elemental analysis, IR and NMR spectroscopies, and, for 19, single-crystal X-ray diffraction. The use of metallic gallium and indium to reduce Cp2­TiCl2 opens up a previously unexplored path that may provide access to novel and unique compounds.