Two new Cysteine and Methionine derivatives of aminophenol ligands (HLCys and HLMet) were synthesized by a convenient procedure. The ligands were characterized by 1H NMR, 13C NMR and IR spectroscopies, ESI-MS, elemental analysis and optical activity measurements. Iron(III) complexes (FeLCys and FeLMet) of these ligands were synthesized and characterized by spectroscopic, magnetic susceptibility studies and cyclic voltammetry techniques. The molecular structure of FeLCys and FeLMet determined by ESI-MS consist of two ligands coordinated to Fe(III) centers. The magnetic susceptibility measurement indicates the monomeric complexes with paramagnetic properties. Both complexes undergo metal-centred reduction, and ligand-centred oxidation. [ABSTRACT FROM AUTHOR]