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Data for Investigating discrepancies between experimental solid-state NMR and GIPAW calculation : N=C–N13C and OH⋯O1H chemical shifts in pyridinium fumarates and their cocrystals
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Corlett, Emily K., Blade, Helen, Hughes, Leslie P., Sidebottom, Philip J., Walker, David, Walton, Richard I. and Brown, Steven P. (2020) Data for Investigating discrepancies between experimental solid-state NMR and GIPAW calculation : N=C–N13C and OH⋯O1H chemical shifts in pyridinium fumarates and their cocrystals. [Dataset]
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Plain Text (Readme file)
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Abstract
An NMR crystallography analysis is presented for four solid-state structures of pyridine fumarates and their cocrystals, using crystal structures deposited in the Cambridge Crystallographic Data Centre, CCDC. Experimental one-dimensional, one-pulse 1H and 13C cross-polarisation (CP) magic-angle spinning (MAS) nuclear magnetic resonance (NMR) and two-dimensional 14N–1H heteronuclear multiple-quantum coherence MAS NMR spectra are compared with gauge-including projector augmented wave (GIPAW) calculations of the 1H and 13C chemical shifts and the 14N shifts that additionally depend on the quadrupolar interaction. Considering the high ppm (>10 ppm) 1H resonances, while there is good agreement (within 0.4 ppm) between experiment and GIPAW calculation for the hydrogen-bonded NH moieties, the hydrogen-bonded fumaric acid OH resonances are 1.2–1.9 ppm higher in GIPAW calculation as compared to experiment. For the cocrystals of a salt and a salt formed by 2-amino-5-methylpyridinium and 2-amino-6-methylpyridinium ions, a large discrepancy of 4.2 and 5.9 ppm between experiment and GIPAW calculation is observed for the quaternary ring carbon 13C resonance that is directly bonded to two nitrogens (in the ring and in the amino group). By comparison, there is excellent agreement (within 0.2 ppm) for the quaternary ring carbon 13C resonance directly bonded to the ring nitrogen for the salt and cocrystal of a salt formed by 2,6-lutidinium and 2,5-lutidine, respectively.
Item Type: | Dataset | ||||||||||||||||||
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Subjects: | Q Science > QD Chemistry | ||||||||||||||||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry Faculty of Science, Engineering and Medicine > Science > Physics |
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Type of Data: | Experimental data | ||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Crystallography, Nuclear magnetic resonance spectroscopy | ||||||||||||||||||
Publisher: | University of Warwick, Department of Physics | ||||||||||||||||||
Official Date: | 27 April 2020 | ||||||||||||||||||
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Status: | Not Peer Reviewed | ||||||||||||||||||
Publication Status: | Published | ||||||||||||||||||
Media of Output (format): | .txt .xy .magres .cif .info .par .temp .png .ased .docx | ||||||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | ||||||||||||||||||
Copyright Holders: | University of Warwick | ||||||||||||||||||
Description: | Data record consists of a zip archive, organised by sub-folders containing the raw data files, named and organised according to the nature of the calculation or experiments. Sub-folders consist of: |
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Date of first compliant deposit: | 27 April 2020 | ||||||||||||||||||
Date of first compliant Open Access: | 27 April 2020 | ||||||||||||||||||
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