In the present study, we discussed to synthesis of a new Schiff base with nitro groups and its complexation properties with Fe/Cr(III) salen/salophen capped complexes. For this, 1,3,5-tris (formylphenoxymethyl)benzene (1, TRIPOD) involving aldehyde groups was converted to the Schiff base derivative (2, TNPIM-TRIPOD) using 4-nitroaniline. The synthesized compound 2 were reacted with four new trinuclear Fe(III) and Cr(III) complexes involving tetradenta Schiff bases N,N-bis(salicylidene)ethylenediamine-(salenH2) or bis(salicylidene)-o-phenylenediamine-(salophenH2). Characterization of all compounds was made with elemental analysis, infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), nuclear magnetic resonance (1H-NMR), and magnetic susceptibility measurement. The complexes can also be characterized as low-spin distorted octahedral Fe(III) and Cr(III) bridged by nitro groups. © Springer Science+Business Media B.V. 2009.