Yttrium, titanium, and yttrium‐titanium citrate complexes are synthesized in ethylene glycol medium at conditions similar to those used when the polymerized complex method (a version of the sol‐gel technology) is applied. The composition and IR, 1H and 13C NMR spectral characteristics of the isolated solid state complexes are studied. Proofs of the mixed metal nature of the bimetallic complexes are reported. The conditions of deprotonation of the alcoholic OH group of the citrate ligands are considered.