Abstract
The tritinate [Ti 3O](OPr i) 9(OMe) was isolated from the reaction of Ti(OPr i) 4 with water and methanol in isopropanol solution and characterized by elemental analysis, multinuclear NMR spectroscopy, and single-crystal X-ray diffraction ( a = 23.295(5), b = 19.560(4), c = 18.661(4) A ̊ , β = 108.39(3)°; Z = 8 ; space group P2 1/ c-C 2h 5). The [Ti 3O](OPr i) 9(OMe) molecule has a Ti 3 μ 3-O)( μ 3-OMe)( μ 2-OPr i) 3(OPr i) 6 structure in the solid state and in solution, but is unstable in solution at ambient temperature even in hydrocarbon solvents where it is in quasi-equilibrium with Ti(OPr i) 4− x (OMe) x , [Ti 3O](OPr i) 10, and more highly condensed polytitanates. The isostructural trititanate [Ti 3O](OPr i) 10 could not be isolated from isopropanol solutions of hydrolyzed Ti(OPr i) 4, but was identified as the sole hydrolysis product at low degrees of hydrolysis using 17O, 13C{ 1H} and 1H NMR spectroscopy.
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