Structural, Thermal, and Vibrational Properties of N,N-Dimethylglycine-Chloranilic Acid-A New Co-Crystal Based on an Aliphatic Amino Acid
| Autor: | Wojciech Schilf, J. Nowicka-Scheibe, Joanna Hetmańczyk, Jan K. Maurin, Łukasz Hetmańczyk, Andrzej Pawlukojć |
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| Rok vydání: | 2021 |
| Předmět: |
temperature dependent IR spectroscopy
Technology Materials science Magic angle DFT calculation Protonation 02 engineering and technology Triclinic crystal system 010402 general chemistry 01 natural sciences Article chemistry.chemical_compound symbols.namesake N N-dimethylglycine–chloranilic acid (DMG+–CLA−) co-crystal General Materials Science Microscopy QC120-168.85 Hydrogen bond X-ray diffraction inelastic neutron scattering (INS) QH201-278.5 Nuclear magnetic resonance spectroscopy 021001 nanoscience & nanotechnology Engineering (General). Civil engineering (General) 0104 chemical sciences TK1-9971 Crystallography chemistry Descriptive and experimental mechanics Chloranilic acid X-ray crystallography symbols Electrical engineering. Electronics. Nuclear engineering TA1-2040 0210 nano-technology Raman spectroscopy |
| Zdroj: | Materials, Vol 14, Iss 3292, p 3292 (2021) Materials; Volume 14; Issue 12; Pages: 3292 Materials |
| ISSN: | 1996-1944 |
| Popis: | The new complex of N,N-Dimethylglycine (DMG) with chloranilic acid (CLA) was synthesized and examined for thermal, structural, and dynamical properties. The structure of the reaction product between DMG and CLA was investigated in a deuterated dimethyl sulfoxide (DMSO-d6) solution and in the solid state by Nuclear Magnetic Resonance (NMR) (Cross Polarization Magic Angle Spinning-CPMAS NMR). The formation of the 1:1 complex of CLA and DMG in the DMSO solution was also confirmed by diffusion measurement. X-ray single crystal diffraction results revealed that the N,N-dimethylglycine–chloranilic acid (DMG+–CLA−) complex crystallizes in the centrosymmetric triclinic P-1 space group. The X-ray diffraction and NMR spectroscopy show the presence of the protonated form of N,N-dimethylglycine and the deprotonated form of chloranilic acid molecules. The vibrational properties of the co-crystal were investigated by the use of neutron (INS), infrared (IR), and Raman (RS) spectroscopies, as well as the density functional theory (DFT) with periodic boundary conditions. From the band shape analysis of the N–CH3 bending vibration, we can conclude that the CH3 groups perform fast (τR ≈ 10−11 to 10‒13 s) reorientational motions down to a temperature of 140 K, with activation energy at ca. 6.7 kJ mol−1. X-ray diffraction and IR investigations confirm the presence of a strong N+–H···O− hydrogen bond in the studied co-crystal. |
| Databáze: | OpenAIRE |
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