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1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement

Miah, Habeeba K.; Cresswell, Rosalie; Iuga, Dinu; Titman, Jeremy J.

Authors

Habeeba K. Miah

Rosalie Cresswell

Dinu Iuga

Jeremy J. Titman



Abstract

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.

Journal Article Type Article
Journal Solid-State Nuclear Magnetic Resonance
Electronic ISSN 1527-3326
Publisher Elsevier
Peer Reviewed Peer Reviewed
APA6 Citation Miah, H. K., Cresswell, R., Iuga, D., & Titman, J. J. (in press). 1H CSA parameters by ultrafast MAS NMR: measurement and applications to structure refinement. Solid State Nuclear Magnetic Resonance, doi:10.1016/j.ssnmr.2017.02.002. ISSN 1527-3326
DOI https://doi.org/10.1016/j.ssnmr.2017.02.002
Publisher URL http://www.sciencedirect.com/science/article/pii/S0926204016301515
Copyright Statement Copyright information regarding this work can be found at the following address: http://creativecommons.org/licenses/by-nc-nd/4.0
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Copyright Statement
Copyright information regarding this work can be found at the following address: http://creativecommons.org/licenses/by-nc-nd/4.0





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