Abstract
Crystalline α‐bistetramethylammonium hydrogencyclotriphosphate [N(CH3)4]2HP3O9 (Pcab), which were synthesized via a low‐temperature route (<60 °C) shows an irreversible first‐order phase transition to β‐[N(CH3)4]2HP3O9 (P212121), which was investigated by differential scanning calorimetry, X‐ray powder diffraction, and solid state nuclear magnetic resonance spectroscopy. The crystal structure of β‐bistetramethylammonium hydrogencyclotriphosphate was solved and refined from X‐ray powder diffraction data by the Rietveld method using constraints obtained by 31P, 1H, and 13C NMR spectroscopy. The new compound crystallizes in an orthorhombic space group with a = 9.3828(1), b = 11.8196(1) and c = 16.0396(2) Å.
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