New Schiff base (HL) ligand is prepared via condensation of isatins and amino acids in 1:1 molar ratio. Metal complexes are prepared and characterized by elemental analysis, molar conductance, electronic, infrared, and multinuclear magnetic resonance ( 1 H NMR, 13 C NMR, and 119 Sn NMR). The analytical data showed that the ligand acts as bidentate toward metal ions via azomethine nitrogen and carboxylate oxygen by a stoichiometric reaction of metal : ligand (1 : 2) to from metal complexes (Pb(II)(L) 2 and Bu 2 Sn(L) 2 , where L is the Schiff base ligands of histidine and methionine). The conductivity values between 15 and 25 Ω −1 cm 2 mol −1 in DMF imply the presence of nonelectrolyte species. On the basis of the above spectral studies, distorted octahedral and tetrahedral geometry have been proposed for the resulting organotin(IV) and lead(II) complexes.