A series of Al(III) compounds containing the C
6F
5-substituted
-diketiminate ligands LAlMeCl (
2), LAlMe
2 (
3), LAlMeI(
4), and LAlBr
2 (
5) (L = HC[(CMe)(NC
6F
5)]
2) were synthesized and characterized. The hydrolysis of
2 and
4 in thepresence of 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene as the hydrogen halide acceptor both lead to (LAlMe)
2(
-O) (
6), a methylalumoxane derivative, which is the first hydrolysis product with the general formula of (RAlMe)
nO.A comparison of the hydrolysis products of
2 and
4 with that of L'AlMeCl (L' = HC[(CMe)(NAr)]
2, Ar = 2,6-
iPr
2C
6H
3) shows that with the C
6F
5-substituted
-diketiminate ligand, it was not possible to generate LAlMe(OH).This is obviously due to the stronger Brönsted acidity of the proton and the smaller size of the C
6F
5 group in thiscompound compared to that of the corresponding 2,6-
iPr
2C
6H
3 derivative.