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New coordination polymers with 2D network structures with fluorine directly coordinated to the metal ion were prepared both via mechanochemical synthesis and fluorolytic sol–gel synthesis. Depending on the synthesis route, the samples show different particle sizes, according to SEM imaging. The crystal structures of barium acetate fluoride, strontium acetate fluoride, and lead acetate fluoride (BaF(CH3COO), SrF(CH3COO) and PbF(CH3COO)) were solved from X-ray powder diffraction data. The structure solution is backed by the results from 19 F MAS NMR, FT IR data, and thermal analysis. The calculated chemical shifts of the 19 F MAS NMR spectra coincide well with the measured ones. It turns out that the grinding conditions have a remarkable influence on the mechanochemical synthesis and its products. Our systematic study also indicates a strong influence of the atomic radii of Ca, Sr, Ba, and Pb on the success of the syntheses. [ABSTRACT FROM AUTHOR]