196940-98-4Relevant academic research and scientific papers
Preparation and characterization of (C5Me4Ph)TiCl3, the oxochloride complexes [(C5Me4Ph)TiCl2]2( μ-O) and [(C5Me4Ph)TiCl( μ-O)]3 and the oxo-complex [(C5Me4Ph)Ti]4( μ-O)6
Bjoergvinsson, Mar,Halldorsson, Snorri,Arnason, Ingvar,Magull, Joerg,Fenske, Dieter
, p. 207 - 215 (1997)
The titanium compound (C5Me4Ph)TiCl3 (1) can be prepared by the reaction of (C5Me4Ph)SiMe3 with TiCl4. Hydrolysis of 1 in the presence of HNEt2 or Ag2O has allowed for the isolation of the oxochloride complexes [(C5Me4Ph)TiCl2]2( μ-O) (2) and [(C5Me4Ph)TiCl( μ-O)]3 (3), respectively. The NMR spectra of 3 are consistent with a nearly flat Ti3O3 ring having down-up-up or E-Z-Z arrangement of (C5Me4Ph)-ligands around the ring. The X-ray crystal structure of 2 (monoclinic, space group C2/c, a = 19.847(12), b = 9.089(5), c = 20.405(13) A, β = 124.06(5)°) consists of trans [(C5Me4Ph)TiCl2]2( μ-O) molecules of C2 symmetry with nearly linear Ti-O-Ti units (169.3(2)°). Reaction of 1 with an excess of H2O/HNEt2 results in the formation of the oxo-complex [(C5Me4Ph)Ti]4( μ-O)6 (4). The X-ray crystal structure of 4 (triclinic, space group P1, a = 11.861(5), b = 12.706(5), c = 18.218(8) A, α = 87.58(3)°, β = 89.00(3)°, γ = 86.60(3)°) reveals that the molecules of 4 have an adamantane-like Ti4O6 cage of nearly Td symmetry. The NMR spectra and molecular structures of 1, 2, 3 and 4 are discussed.
