Fe-, Y-Fe-Al- and Y-Ce-Fe- citrates were synthesized in ethylene glycol (EG) medium under conditions similar to those used in the polymerized complex method. Their elemental composition, IR, 13C and 1H NMR, X-ray photoelectron and Mossbauer spectra were studied, and formulae describing their composition were proposed. The complexes contained EG bonded as adduct and ester with citric acid ligand and did not contain ligands with deprotonated alcoholic groups. The complexes consisted of agglomerated spheres, 0.7-3μm in diameter. The local composition of the products was established by energy dispersive X-ray microanalysis. The comparison of the number of the ligands, their average electrical charge and the esterification degree of mono-, di- and trimetallic complexes proved the mixed-metal nature of the species studied. The thermal decomposition of the complexes was studied and a general scheme of the processes taking place was proposed. Highly crystalline, phase homogeneous Y3Fe4AlO12 was produced after heating the respective complex at 1000℃. Ce-doped yttrium-iron garnet, similarly prepared, contained traces of CeO2.