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Organic-inorganic luminescent hybrid materials (HM) based on PbF2 inorganic matrices are promising for OLED application. One of the main task when synthesizing the above HM is preservation of a major content of organic molecules from destruction both at the melting synthesis technique and at coprecipitation from aqueous solutions of HF which is used as a fluorinating agent. In the present research we developed the soft synthesis technique of HM by the substitution of HF to ammonium bifluoride. As organic constituents we used highly efficient phosphors: beta-diketone complexes of Eu, 8-hydroxyquinoline complexes with metals I, II and III group of the Periodic Table. The effect of organic molecules or molecular fragments on size and morphology of obtained PbF2 nanoparticles, luminescence properties of HM both directly after precipitation, drying, and after calcination of powders were analyzed. The soft synthesis resulted in a capture of phosphor molecules by precipitating of PbF2 nanoc rystallites. The proceeding of the exchange reaction between a metal-organic complex and a matrix during the heat treatment of precipitated powders resulted to the formation of Pb-complexes of different coordination. By this way we have achieved controlled changes in HM photoluminescence parameters. This research was financially supported by the grant 17.1.18.0026.01 (10.4702.2017/BC).