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Irreversible Phase Transition of Bistetramethylammonium Hydrogencyclotriphosphate
Author(s) -
Mangstl Martin,
Celinski Vinicius R.,
Pritzel Christian,
Trettin Reinhard,
Schmedt auf der Günne Jörn
Publication year - 2017
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201700246
Subject(s) - orthorhombic crystal system , differential scanning calorimetry , crystallography , phase transition , powder diffraction , rietveld refinement , diffraction , crystal structure , nuclear magnetic resonance spectroscopy , chemistry , spectroscopy , materials science , x ray crystallography , space group , phase (matter) , stereochemistry , physics , condensed matter physics , organic chemistry , quantum mechanics , optics , thermodynamics
Crystalline α‐bistetramethylammonium hydrogencyclotriphosphate [N(CH 3 ) 4 ] 2 HP 3 O 9 ( Pcab ), which were synthesized via a low‐temperature route (<60 °C) shows an irreversible first‐order phase transition to β‐[N(CH 3 ) 4 ] 2 HP 3 O 9 ( P 2 1 2 1 2 1 ), 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 31 P, 1 H, and 13 C 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.