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Abstract. To obtain new effective precursors for single phase ceramic zirconia materials by the alkoxide route, three heterometallic iron-yttrium acetylacetonate complexes were synthesized by electrochemical anodic dissolution in acetylacetone. The structure and properties of the synthesized complex oxides were studied by XRD, EXAFS, magnetic susceptibility and M6ssbauer. It was shown that, for iron-containing gels and oxides, Fe 3+ ions--interchangeably with Y3+--participate in the oxide formation mechanism. The sets of interatomic distances found by EXAFS in the iron-yttrium precursor and in the zirconia gel are practically equal. The presence of structure fragments formed by these interactions--and especially by direct Fe--Y bonds in the precursors--allows single-phase triple ceramic oxides to form.