Two oxalate-bridged binuclear iron(III) complexes, [(FeL APMe ) 2 (μ-ox)] (1) and [(FeL APOMe ) 2 (μ-ox)] (2), in which H 2 L APMe and H 2 L APOMe are pyridine-based di-methyl and tert-butyl methoxy substituted aminophenol ligands respectively, were prepared. Both compounds have been characterized by X-ray crystallography, infrared spectroscopy, UV–Vis spectroscopic techniques, cyclic voltammetry analysis, and magnetic susceptibility studies. In both crystals, each iron(III) is coordinated by the oxygen atoms of an oxalate bridging ligand, two phenolate oxygen atoms, and amine nitrogens of ligands. The variable temperature magnetic susceptibility indicates antiferromagnetic coupling between iron centers in both complexes. Cyclic voltammograms of 2 in CH 2 Cl 2 at low temperature showed quasi-reversible peaks corresponding to ligand-centered oxidations.