A series of cyclohexane-1,2-diyl linked bis(ketiminato)aluminum complexes were synthesized. Reaction of a mixture of cis-and trans-diaminocyclohexane and 2,4-pentanedione gave a mixture of cis-and trans-cyclohexane-1,2-diyl linked bis(ketimine) ligands (cis-1 and trans-1), which can be separated by fractional recrystallization. Reactions of trans-1 with 1 and 2 equiv. AlMe 3 gave monoaluminum complex trans-C 6 H 10 [(NCMeCHCMeO)AlMe 2 ](NHCMeCHCMeO) (2) and dialuminum complex trans-C 6 H 10 [(NCMeCHCMeO)AlMe 2 ] 2 (3), respectively. Contrarily, when 1 equiv. or excess cis-1 reacted with AlMe 3 , only five-coordinate, linked bis(ketiminato)aluminum complex cis-C 6 H 10 [(NCMeCHCMeO) 2 AlMe]