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Crystal data for the series of piperazinium bis(n-alkanoates) of the type 2[CxH2x - 1O2-] [C4H12N22+] for x = 1 to 16 are presented. Most of these compounds have triclinic unit cells whose dimensions, obtained from single-crystal work, have been used to index their powder diagrams. The a ( = 5.718 Å) and b ( = 7.481 Å) cell dimensions remain nearly constant while the c dimension and the volume of the unit cell increase linearly with x, the number of carbon atoms in the alkanoate anion. Presumably the aliphatic sequence in the alkanoate anion adopts the fully extended conformation and lies in the bc plane and nearly along the c direction.