14N overtone NMR spectra under magic angle spinning : experiments and numerically exact simulations

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DOIResolve DOI: http://doi.org/10.1063/1.4775592
AuthorSearch for: ; Search for:
TypeArticle
Journal titleThe Journal of Chemical Physics
Volume138
Issue6
Pages064201-1064201-10; # of pages: 10
AbstractIt was recently shown that high resolution 14N overtone NMR spectra can be obtained directly under magic angle spinning (MAS) conditions [L. A. O’Dell and C. I. Ratcliffe, Chem. Phys. Lett. 514, 168 (2011)]10.1016/j.cplett.2011.08.030. Preliminary experimental results showed narrowed powder pattern widths, a frequency shift that is dependent on the MAS rate, and an apparent absence of spinning sidebands, observations which appeared to be inconsistent with previous theoretical treatments. Herein, we reproduce these effects using numerically exact simulations that take into account the full nuclear spin Hamiltonian. Under sample spinning, the 14N overtone signal is split into five (0, ±1, ±2) overtone sidebands separated by the spinning frequency. For a powder sample spinning at the magic angle, the +2ωr sideband is dominant while the others show significantly lower signal intensities. The resultant MAS powder patterns show characteristic quadrupolar lineshapes from which the 14N quadrupolar parameters and isotropic chemical shift can be determined. Spinning the sample at other angles is shown to alter both the shapes and relative intensities of the five overtone sidebands, with MAS providing the benefit of averaging dipolar couplings and shielding anisotropy. To demonstrate the advantages of this experimental approach, we present the 14N overtone MAS spectrum obtained from L-histidine, in which powder patterns from all three nitrogen sites are clearly resolved.
Publication date
PublisherAIP Publishing
LanguageEnglish
AffiliationMeasurement Science and Standards; National Research Council Canada
Peer reviewedYes
NRC numberA12-10-0052
NPARC number21268120
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Record identifiera417f055-9223-4cbc-83e5-9de05409b249
Record created2013-04-16
Record modified2016-05-09
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