Impact of Group 13 Metals on Cp2TiCl2 Reduction and Structural Characterization of Resulting Compounds
datasetposted 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 1–9, 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.