This article describes synthesis of the difference carboxylic acid derivatives of triphenylene and its complexation properties with Fe/Cr (III)-salophen. For this purpose, the carboxylic acid derivatives of 2,3,6,7,10,11-hexahydroxytriphenylene were synthesized and then reacted with four new Fe(III) and Cr(III) complexes involving tetradenta Schiff bases bis(salicylidene)-o-phenylenediamine-(salophenH2). The prepared compounds were characterized by means of elemental analysis carrying out infrared spectroscopy (IR), thermogravimetric analysis (TG), nuclear magnetic resonance (1H NMR), elemental analysis and magnetic susceptibility measurement. The complexes can also be characterized as low-spin distorted octahedral Fe(III) and Cr (III) bridged by carboxylic acids. © 2011 Elsevier B.V. All rights reserved.