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Hybrid organo-inorganic materials were synthesized by co-precipitation from aqueous solutions with stable phosphors — 8-hydroxyquinolates and β-diketonates of metals with ammonium fluoride. The photoluminescence spectra of the obtained hybrid materials were studied. A comparison is made with the spectral-luminescent properties of hybrid materials obtained by the melt method with low-melting lead oxyfluoride glasses.