H-1 and H-2 NMR spectroscopic studies at 203 K of the reaction of Br2FeIII(OEOP) in dichloromethane solution with phenylmagnesium bromide show that PhBrFeIII(OEOP) and BrFeII(OEOP) form, and that both are converted into a new paramagnetic complex, [Ph2Fe(OEOP)](n-), with two axial phenyl groups bound to iron.