Vibrational, XRD and 13 C NMR studies of DL-phenylglycinium methanesulfonate crystal

Wołoszyn, Łukasz; Ilczyszyn, Marek; Haupa, Karolina Anna

doi:10.1016/j.saa.2016.05.046

Cited by 2 publications

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References 28 publications

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“…The wavenumbers of the bands observed in these spectra are summarized in Table 5. The band assignment presented in this table is based on the theoretical predictions of the internal vibrations of the PG + cation (Wołoszyn et al, 2016) and TF À anion (Gejji et al, 1993), and on a comparison of the assignments proposed for simple phenylglycine salts (Ilczyszyn et al, 2009a,b) and dl-phenylglycinium methanesulfonate (Wołoszyn et al, 2016). The notation of the benzene vibrations was used to name the internal vibrations of the phenylglycine phenyl group (Wojtkowiak & Chabanel, 1977;Varsá nyi, 1969).…”

Section: Vibrational Spectramentioning

confidence: 99%

The dehydration process in the DL-phenylglycinium trifluoromethanesulfonate monohydrate crystal revealed by XRD, vibrational and DSC studies

2019

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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 + ÁCF 3 -SO 3 À ÁH 2 O. PGTFH dehydrates in one step centred at 353 K and crystallizes in the monoclinic space group C2/c, whereas the anhydrous compound (PGTF) crystallizes in the triclinic space group P1. 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-HÁ Á ÁO 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.Note: (a) the values given before and after '/' are related to the cooling and heating processes, respectively.

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Section: Vibrational Spectramentioning

confidence: 99%