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KFe(H 2 P 2 O 7 ) 2 is synthesized at 443 K in molten polyphosphoric acids containing K and Fe ions, and its crystal structure is determined: triclinic unit cell with a = 4.9974(6) Å, b = 7.4766(9) Å, c = 7.8185(9) Å, α = 82.29(2) o , β = 83.37(2) o , γ = 74.13(2) o ; Z = 1, sp. gr. P . The structure is made up of infinite ribbons formed by corner-shared PO 4 tetrahedra and FeO 6 octahedra, with the K atoms in between. Neighboring ribbons are linked by hydrogen bonds. The proton conductivity of potassium iron(III) dihydrogen diphosphate is rather low.

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