Skip to content Skip to navigation
University of Warwick
  • Study
  • |
  • Research
  • |
  • Business
  • |
  • Alumni
  • |
  • News
  • |
  • About

University of Warwick
Publications service & WRAP

Highlight your research

  • WRAP
    • Home
    • Search WRAP
    • Browse by Warwick Author
    • Browse WRAP by Year
    • Browse WRAP by Subject
    • Browse WRAP by Department
    • Browse WRAP by Funder
    • Browse Theses by Department
  • Publications Service
    • Home
    • Search Publications Service
    • Browse by Warwick Author
    • Browse Publications service by Year
    • Browse Publications service by Subject
    • Browse Publications service by Department
    • Browse Publications service by Funder
  • Help & Advice
University of Warwick

The Library

  • Login
  • Admin

Investigating discrepancies between experimental solid-state NMR and GIPAW calculation : N=C–N13C and OH⋯O1H chemical shifts in pyridinium fumarates and their cocrystals

Tools
- Tools
+ Tools

Corlett, Emily K., Blade, Helen, Hughes, Leslie P., Sidebottom, Philip J., Walker, David, Walton, Richard I. and Brown, Steven P. (2020) Investigating discrepancies between experimental solid-state NMR and GIPAW calculation : N=C–N13C and OH⋯O1H chemical shifts in pyridinium fumarates and their cocrystals. Solid State Nuclear Magnetic Resonance, 108 . 101662. doi:10.1016/j.ssnmr.2020.101662

[img]
Preview
PDF
WRAP-investigating-discrepancies-experimental-NMR-chemical-co-crystals-Brown-2020.pdf - Accepted Version - Requires a PDF viewer.
Available under License Creative Commons Attribution 4.0.

Download (1476Kb) | Preview
Official URL: https://doi.org/10.1016/j.ssnmr.2020.101662

Request Changes to record.

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: Journal Article
Subjects: Q Science > QD Chemistry
Divisions: Faculty of Science, Engineering and Medicine > Science > Chemistry
Faculty of Science, Engineering and Medicine > Science > Physics
Library of Congress Subject Headings (LCSH): Crystallography, Nuclear magnetic resonance spectroscopy
Journal or Publication Title: Solid State Nuclear Magnetic Resonance
Publisher: Academic Press
ISSN: 0926-2040
Official Date: August 2020
Dates:
DateEvent
August 2020Published
10 April 2020Available
25 March 2020Accepted
Volume: 108
Article Number: 101662
DOI: 10.1016/j.ssnmr.2020.101662
Status: Peer Reviewed
Publication Status: Published
Access rights to Published version: Open Access (Creative Commons)
Date of first compliant deposit: 26 March 2020
Date of first compliant Open Access: 5 May 2020
RIOXX Funder/Project Grant:
Project/Grant IDRIOXX Funder NameFunder ID
UNSPECIFIED[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
UNSPECIFIEDAstraZenecahttp://dx.doi.org/10.13039/100004325
UNSPECIFIEDSyngenta Internationalhttp://dx.doi.org/10.13039/501100010761
EP/L015307/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
639907 European Research Councilhttp://dx.doi.org/10.13039/501100000781
Related URLs:
  • Publisher
  • Related item in WRAP

Request changes or add full text files to a record

Repository staff actions (login required)

View Item View Item

Downloads

Downloads per month over past year

View more statistics

twitter

Email us: wrap@warwick.ac.uk
Contact Details
About Us