In this study, the influence of initial reagents on the phase composition and morphology of magnesium ferrite obtained by combustion of glycine-nitrate gel was investigated. The local environment of iron ions in the gel-precursor was studied in detail using FT-IR, XANES-and EXAFS-spectroscopy. It has been established that in the gel-precursor obtained by dissolving metals (Mg, Fe) in dilute nitric acid, binuclear Fe(III) complexes are formed, while in a similar gel-precursor obtained from crystalline hydrates of nitrates of the corresponding metals, trinuclear Fe(III) complexes predominate. Combustion of a gel consisting of binuclear Fe(III) complexes leads to the formation of nanocrystalline magnesium ferrite powder, characterized by a unimodal particle size distribution. KEYWORDS gel combustion, glycine, spinel, nanopowders, MgFe 2 O 4 ACKNOWLEDGEMENTS This research was supported by the Russian Science Foundation (project No. 22-73-00185). The measurements were performed using the equipment of the Joint Research Centre (JRC PMR) IGIC RAS.FOR CITATION Smirnova M.N., Nikiforova G.E., Kondrat'eva O.N. Synthesis of magnesium ferrite by combustion of glycine-nitrate gel: the influence of reagents on the gel-precursor and the microstructure of nanopowders.