Triazacyclononane (TACN) was coupled to glycine (L-Gly), alanine (L-Ala), and phenylalanine (L-Phe) via standard solution phase peptide coupling techniques. Copper(II) complexes of these new ligand-amino acid conjugates' [(CuLGly)(2)](ClO4)(4) (1), [(CuLAla)(2)Cl](ClO4)(3) (2), and [(Cu2LCl4)-Cl-Phe] (3), were synthesized and characterized. The X-ray crystal structures of 2 and 3 were determined. Complex 2 is a dimeric species where, L-Ala bridges between copper ions via its two TACN amine nitrogen atoms to one copper while the Ala terminal amine and carbonyl oxygen bind to the other copper. Complex 3 is bimetallic but only contains one L-Phe ligand that bridges between the copper ions.