The paper presents experimental studies and structural investigations of two new Fe(III) hydroxycarboxylate coordination compounds. The homopolynuclear complex combinations of Fe(III) glyoxylate and succinate type were obtained in the redox reaction between Fe(NO3)(3) and diols (1,2-ethanediol and 1,4-butanediol). The synthesized coordination compounds and the products formed during their thermal conversion were characterized by thermal analysis (in air and nitrogen), FT-IR and UV-VIS spectrometry, Mossbauer spectrometry, electron microscopy and XRD. By thermal decomposition of the complex combinations, at 300 degrees C, the well crystallized pure phase gamma-Fe2O3 as nanoparticles were formed. (C) 2011 Elsevier B.V. All rights reserved.