Journal of the Chemical Society, Dalton Transactions p. 2843 - 2849 (1996)
Update date:2022-08-05
Topics: Characterization X-ray crystallography Purification Publication Reaction
Hart, Suzanne L.
Duncalf, David J.
Hastings, Jeremy J.
McCamley, Andrew
Taylor, Paul C.
New, selective and high-yielding preparations of the mixed-ring complexes [Ti(η5-C5H5)(η5-C 9H7)Cl2] and [Ti(η5-C5H5)(η5-C 5H4But)Cl2] are reported. These have been used to prepare a range of mono- and di-substituted titanium(IV) alkyl and benzenethiolate complexes of the form [Ti(η5-C5H5)(η 5-ring)(CH2SiMe3)Cl] and [Ti(η5-C5H5)(η5-ring)R 2] (ring = indenyl or C5H4But; R = Me, CH2Ph, CH2SiMe3 or SPh). While the indenyl ligand in the racemic, chiral-at-metal complex [Ti(η5-C5H5)(η5-C 9H7)(CH2SiMe3)Cl] is bound in an η5 fashion, X-ray structural data clearly indicate that there is some 'η3 ring-slip' character to the bonding. The NMR and nuclear Overhauser effect experiments conducted on [Ti(η5-C5H5)(η5-C 5H4But)(CH2SiMe3)Cl] demonstrate hindered rotation around the Ti-C5H4But bond and show the geometry to be fixed such that the But and SiMe3 groups are remote.
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