We report the syntheses, structural, Mössbauer, magnetic, and redox characterization of a series of μ-oxido-bridged diiron(III) complexes in a set of 13-membered amide-based macrocyclic ligands that contain electron-donating and -withdrawing substituents (-H, -Cl, and -CH 3 ) on the ligand periphery. For all three complexes, the Mössbauer spectra indicate that two iron sites are indistinguishable, a fact that is well supported by X-ray crystallographic results. The three complexes exhibit almost identical isomer shifts but distinc-[a]