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Tetracyclic bisaminals formed by condensation of tetraazamacrocycles and glyoxal have rarely been utilized as ligands for transition metal ions. Five novel Cu2+ complexes are presented to expand this set. Glyoxal derivatives of pyruvic aldehyde and butanedione were expected to further rigidify the bisaminal skeleton because of the steric requirements of the methyl groups, while the previously unutilized...