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The dehydration process in the dl ‐phenylglycinium trifluoromethanesulfonate monohydrate crystal revealed by XRD, vibrational and DSC studies
Author(s) -
Wołoszyn Łukasz,
Ilczyszyn Maria M.,
Kinzhybalo Vasyl
Publication year - 2019
Publication title -
acta crystallographica section c
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.304
H-Index - 17
ISSN - 2053-2296
DOI - 10.1107/s2053229619014402
Subject(s) - dehydration , trifluoromethanesulfonate , chemistry , crystallography , polymer chemistry , organic chemistry , biochemistry , catalysis
Thermal analysis, X‐ray diffraction and temperature‐dependent IR spectroscopy were used to study the dehydration process of crystalline dl ‐phenylglycinium trifluoromethanesulfonate monohydrate (PGTFH), C 8 H 10 NO 2 + ·CF 3 SO 3 − ·H 2 O. PGTFH dehydrates in one step centred at 353 K and crystallizes in the monoclinic space group C 2/ c , whereas the anhydrous compound (PGTF) crystallizes in the triclinic space group P . The dehydration process in PGTFH is preceded by a weakening of both the noncovalent aromatic–aromatic interactions and the packing contacts. This process is accompanied by the breakage of medium‐strength O—H…O hydrogen bonds between ions inside layers and a reorganization of the ions within the layers. This reorganization results in the formation of two different ion pairs ( dl ‐phenylglycinium trifluoromethanesulfonate) and the formation of a new hydrogen‐bond network. The dehydration process does not destroy the nature of the crystal structure. Both crystals, i.e. hydrated and anhydrous, have a layered structure, although the layers of each crystal are arranged somewhat differently.