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The first successful electrosynthesis of polycrystalline AgIIFBF4 and single crystalline AgIIF2 in both galvanostatic and potentiostatic conditions was achieved at the Boron‐Doped Diamond electrode in anhydrous hydrogen fluoride. Silver(I) oxidation and the F2 evolution reactions are well separated in the potential scale. Temperature of performing electrosynthesis as well as BF3 overpressure were...
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