The reaction of Cp*TiX 3 [X = Cl ( 1a ), F ( 1b ), Cp* = η 5 -C 5 Me 5 ] with an excess of AlMe 3 afforded the methylated products Cp*TiCl 2 Me ( 2a ) and (Cp*TiF 2 Me)(AlMe 2 F) ( 2b ), respectively, whereas under thermal conditions the reduced titanium species Cp* 2 Ti 2 (μ-Cl) 6 Al 2 Me 4 ( 3 ) and Cp* 2 Ti 2 (μ-F) 8 Al 4 Me 8 ( 4 ) were obtained in moderate yields. The reduction of Ti(IV) to Ti(III) is observed when Cp‘ 2 TiF 2 (Cp‘ = η 5 -C 5 H 5, η 5 -C 5 H 4 Me, Cp*) and Cp*TiF 3 are treated with AlEt 3, leading to [Cp‘ 2 Ti(μ-F) 2 AlEt 2 ] 2 [Cp‘ = η 5 -C 5 H 5 ( 5 ), η 5 -C 5 H 4 Me ( 6 ), Cp* ( 7 )] and Cp* 2 Ti 2 (μ-F) 8 Al 4 Et 8 ( 8 ), respectively. The crystal structures of complexes 3, 4, and 6 have been determined by X-ray single-crystal structure analyses. The core of structure 3 is described as a chair conformation. The environments of the Al and Ti atoms in 3 are distorted tetrahedral and pseudo square pyramidal, respectively. The single-crystal structure analysis of 4 shows an octahedral metal core for Al 4 Ti 2 with the Ti atoms occupying trans positions. The core of complex 6 is a nonplanar eight-membered ring consisting of two titanium atoms, two aluminum atoms, and four bridging fluorine atoms.
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Yu et al. (1999) studied this question.
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