Dynamic nuclear polarisation enhanced (14)N overtone MAS NMR spectroscopy.

Rossini,AJ, Emsley,L and O'Dell,LA 2014, Dynamic nuclear polarisation enhanced (14)N overtone MAS NMR spectroscopy., Physical Chemistry Chemical Physics, vol. 16, no. 25, pp. 12890-12899, doi: 10.1039/c4cp00590b.

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Title Dynamic nuclear polarisation enhanced (14)N overtone MAS NMR spectroscopy.
Author(s) Rossini,AJ
O'Dell,LAORCID iD for O'Dell,LA orcid.org/0000-0002-7760-5417
Journal name Physical Chemistry Chemical Physics
Volume number 16
Issue number 25
Start page 12890
End page 12899
Total pages 10
Publisher Royal Society of Chemistry
Place of publication Cambridge, United Kingdom
Publication date 2014
ISSN 1463-9084
Keyword(s) Science & Technology
Physical Sciences
Chemistry, Physical
Physics, Atomic, Molecular & Chemical
Summary Dynamic nuclear polarisation (DNP) has been used to obtain magic angle spinning (14)N(OT) (nitrogen-14 overtone) solid-state NMR spectra from several model amino acids, with both direct and indirect observation of the (14)N(OT) signal. The crystalline solids were impregnated with biradical solutions of organic liquids that do not dissolve the crystalline phase. The bulk phase was then polarized via(1)H spin diffusion from the highly-polarized surface (1)H nuclei, resulting in (1)H DNP signal enhancements of around two orders of magnitude. Cross polarisation from (1)H nuclei directly to the (14)N overtone transition is demonstrated under magic angle spinning, using a standard pulse sequence with a relatively short contact time (on the order of 100 μs). This method can be used to acquire (14)N overtone MAS powder patterns that match closely with simulated line shapes, allowing isotropic chemical shifts and quadrupolar parameters to be measured. DNP enhancement also allows the rapid acquisition of 2D (14)N(OT) heteronuclear correlation spectra from natural abundance powder samples. (1)H-(14)N(OT) HETCOR and (13)C-(14)N(OT) HMQC pulse sequences were used to observe all single-bond H-N and C-N correlations in histidine hydrochloride monohydrate, with the spectra obtained in a matter of hours. Due to the high natural abundance of the (14)N isotope (99.6%) and the advantages of observing the overtone transition, these methods provide an attractive route to the observation of C-N correlations from samples at natural isotopic abundance and enable the high resolution measurement of (14)N chemical shifts and quadrupolar interaction parameters.
Language eng
DOI 10.1039/c4cp00590b
Field of Research 020401 Condensed Matter Characterisation Technique Development
Socio Economic Objective 970102 Expanding Knowledge in the Physical Sciences
HERDC Research category C1 Refereed article in a scholarly journal
ERA Research output type C Journal article
Copyright notice ©2014, Royal Society of Chemistry
Persistent URL http://hdl.handle.net/10536/DRO/DU:30069930

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