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Redetermination of hydronium perchlorate at 193 and 293 K.

A sample of hydronium perchlorate, H(3)O(+) x ClO(4)(-), crystallized from ethanol at ambient temperature, was found to be orthorhombic (space group Pnma) at both 193 and 293 K, with no phase transition observed in this temperature range. This contrasts with the earlier observation [Nordman (1962). Acta Cryst. 15, 18-23] of a monoclinic phase (space group P2(1)/n) at 193 K for crystals grown at that temperature from perchloric acid. The hydronium and perchlorate ions lie across a mirror plane but it is not possible to define at either temperature a simple description of the H-atom positions due to the three-dimensional tumbling of the hydronium cation.