Petrus Rafał, Utko Józef, Lis Tadeusz, Sobota Piotr
Faculty of Chemistry, University of Wrocław , 14 F. Joliot-Curie, 50-383 Wrocław, Poland.
Department of Chemistry, Wrocław University of Technology , 27 Wybrzeże Wyspiańskiego, 50-370 Wrocław, Poland.
Inorg Chem. 2017 Mar 20;56(6):3324-3334. doi: 10.1021/acs.inorgchem.6b02824. Epub 2017 Mar 2.
The aim of the current study was to examine the effects of group 13 metals on CpTiCl reduction in the presence of 2-methoxyethanol (MeOEtOH) or ethanol (EtOH) and the compositions of the resulting products. Direct reaction of CpTiCl and M [Al, Al (Fe contaminated), Ga, In] in toluene/alcohol for 2 h gave a new family of uncommon homo- and heterometallic compounds: [CpTiAl(μ,η-OEtOMe)Cl][Ti(μ,η-OEtOMe)(η-OEtOMe)Cl] (1), [CpTiAl(μ,η-OEtOMe)Cl]Cl (2), [CpTiAl(μ,η-OEtOMe)Cl][CpTi(η-HOEtOMe)][FeCl] (3), [CpTi(η-HOEtOMe)][GaCl][Cl] (4), [CpTi(μ-OEt)(OEt)][GaCl] (5), [CpTi(μ,η-OEtOMe)Cl] (6), and [CpTi(μ,η-OEtOMe)(μ-OEtOMe)Cl] (7). The reaction with indium for 48 h resulted in isolation of [TiIn(μ,η-OEtOMe)(OEtOMe)Cl] (8), [In(μ-OEtOMe)(HOEtOMe)Cl] (9), and [Ti(OEtOMe)] (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 CpTiCl opens up a previously unexplored path that may provide access to novel and unique compounds.
