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Chemical preparation, crystal structure, NMR spectroscopy and thermal investigations of the 4-dimethylaminopyridinium dihydrogenmonophosphate (C 7 H 11 N 2 ) H 2 PO 4 are studied. This compound crystallizes in the triclinic system, with the space group P 1 À and the following parameters: a = 7.8046 (3) Å , b = 8.0826(3) Å , c = 8.42 62(3) Å , a = 98.497(3)°, b = 104.689(3)°, c = 99.428(3)°, V = 497.14(3) Å 3 , Z = 2.The structural arrangement can be described as inorganic chains, ½H 2 PO 4 nÀ n , parallel to the a-direction, the organic cations are linked to these chains by hydrogen bonds N-HÁÁÁO to form a three-dimensional infinite network.