Eight neutral mononuclear complexes constructed from transition metals (M = Co(Ⅱ), Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ)) and ligands N-(2-pyridylmethyl)-L-phenylalanine (L-Hpmpa) and N-(2-pyridylmethyl)-L-tyrosine (L-Hpmtyr) have been synthesized by both hydrothermal and conventional room temperature reactions. Four of them have been structurally characterized by single-crystal X-ray diffractions. They are: [Co(L-pmpa)2·2H2O] 1, [Ni(L-pmpa)2·2H2O] 2, [Cu(L-pmpa)2·2H2O] 3 and [Cu(L-pmtyr)2·2H2O] 4. Single-crystal X-ray analysis, IR and elemental analysis revealed that complexes 1, 2 and 3 are isostructural. Powder X-ray diffraction, IR and elemental analysis revealed that complexes 4, 5 (Zn[L-pmtyr]2·2H2O), 6 (Cd[L-pmtyr]2·2H2O), 7 (Co[L-pmtyr]2·2H2O) and 8 (Ni[L-pmtyr]2·2H2O) are isostructural. The photoluminescence properties of L-Hpmtyr ligand, compounds 5 and 6 were also investigated.