1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement
A 1H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν1 and ultrafast MAS to resolve 1H sites in ν2 is described. This experiment is used to measure 1H shift parameters for L-ascorbic acid,...
| Main Authors: | , , , |
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| Format: | Article |
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Elsevier
2017
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| Online Access: | https://eprints.nottingham.ac.uk/40628/ |
| _version_ | 1848796102509199360 |
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| author | Miah, Habeeba K. Cresswell, Rosalie Iuga, Dinu Titman, Jeremy J. |
| author_facet | Miah, Habeeba K. Cresswell, Rosalie Iuga, Dinu Titman, Jeremy J. |
| author_sort | Miah, Habeeba K. |
| building | Nottingham Research Data Repository |
| collection | Online Access |
| description | A 1H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν1 and ultrafast MAS to resolve 1H sites in ν2 is described. This experiment is used to measure 1H shift parameters for L-ascorbic acid, a compound with a relatively complex hydrogen-bonding network in the solid. The 1H CSAs of hydrogen-bonded sites with resolved isotropic shifts can be extracted directly from the recoupled lineshapes. In combination with DFT calculations, hydrogen positions in crystal structures obtained from X-ray and neutron diffraction are refined by comparison with simulations of the full two-dimensional NMR spectrum. The improved resolution afforded by the second dimension allows even unresolved hydrogen-bonded sites 1H to be assigned and their shift parameters to be obtained. |
| first_indexed | 2025-11-14T19:42:39Z |
| format | Article |
| id | nottingham-40628 |
| institution | University of Nottingham Malaysia Campus |
| institution_category | Local University |
| last_indexed | 2025-11-14T19:42:39Z |
| publishDate | 2017 |
| publisher | Elsevier |
| recordtype | eprints |
| repository_type | Digital Repository |
| spelling | nottingham-406282020-05-04T18:34:58Z https://eprints.nottingham.ac.uk/40628/ 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement Miah, Habeeba K. Cresswell, Rosalie Iuga, Dinu Titman, Jeremy J. A 1H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν1 and ultrafast MAS to resolve 1H sites in ν2 is described. This experiment is used to measure 1H shift parameters for L-ascorbic acid, a compound with a relatively complex hydrogen-bonding network in the solid. The 1H CSAs of hydrogen-bonded sites with resolved isotropic shifts can be extracted directly from the recoupled lineshapes. In combination with DFT calculations, hydrogen positions in crystal structures obtained from X-ray and neutron diffraction are refined by comparison with simulations of the full two-dimensional NMR spectrum. The improved resolution afforded by the second dimension allows even unresolved hydrogen-bonded sites 1H to be assigned and their shift parameters to be obtained. Elsevier 2017-02-13 Article PeerReviewed Miah, Habeeba K., Cresswell, Rosalie, Iuga, Dinu and Titman, Jeremy J. (2017) 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement. Solid-State Nuclear Magnetic Resonance . ISSN 1527-3326 (In Press) http://www.sciencedirect.com/science/article/pii/S0926204016301515 doi:10.1016/j.ssnmr.2017.02.002 doi:10.1016/j.ssnmr.2017.02.002 |
| spellingShingle | Miah, Habeeba K. Cresswell, Rosalie Iuga, Dinu Titman, Jeremy J. 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title | 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title_full | 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title_fullStr | 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title_full_unstemmed | 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title_short | 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement |
| title_sort | 1h csa parameters by ultrafast mas nmr: measurement and applications to structure refinement |
| url | https://eprints.nottingham.ac.uk/40628/ https://eprints.nottingham.ac.uk/40628/ https://eprints.nottingham.ac.uk/40628/ |