14N overtone transition in double rotation solid-state NMR
14N overtone transition in double rotation solid-state NMR
Solid-state NMR transitions involving outer energy levels of the spin-1 14N nucleus are immune, to first order in perturbation theory, to the broadening caused by the nuclear quadrupole interaction. The corresponding overtone spectra, when acquired in conjunction with magic-angle sample spinning, result in lines, which are just a few kHz wide, permitting the direct detection of nitrogen compounds without the need for labeling. Despite the success of this technique, “overtone” resonances are still broadened due to indirect, second order effects arising from the large quadrupolar interaction. Here we demonstrate that another order of magnitude in spectral resolution may be gained by using double rotation. This brings the width of the 14N solid-state NMR lines much closer to the region commonly associated with high-resolution solid-state NMR spectroscopy of 15N and demonstrates the improvements in resolution that may be possible through the development of pulsed methodologies to suppress these second order effects.
23748-23753
Haies, Ibraheem M.
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Jarvis, James A.
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Brown, Lynda J.
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Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Williamson, Philip T. F.
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Carravetta, Marina
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7 August 2015
Haies, Ibraheem M.
d14dce0d-4693-429a-8047-7770f3765d02
Jarvis, James A.
ff38f19b-7bfa-4361-b1ce-7cc7df510b92
Brown, Lynda J.
75aa95fa-5d27-46a7-9dbe-0f465a664f5b
Kuprov, Ilya
bb07f28a-5038-4524-8146-e3fc8344c065
Williamson, Philip T. F.
0b7715c6-b60e-4e95-a1b1-6afc8b9f372a
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Haies, Ibraheem M., Jarvis, James A., Brown, Lynda J., Kuprov, Ilya, Williamson, Philip T. F. and Carravetta, Marina
(2015)
14N overtone transition in double rotation solid-state NMR.
Physical Chemistry Chemical Physics, 17 (37), .
(doi:10.1039/C5CP03266K).
Abstract
Solid-state NMR transitions involving outer energy levels of the spin-1 14N nucleus are immune, to first order in perturbation theory, to the broadening caused by the nuclear quadrupole interaction. The corresponding overtone spectra, when acquired in conjunction with magic-angle sample spinning, result in lines, which are just a few kHz wide, permitting the direct detection of nitrogen compounds without the need for labeling. Despite the success of this technique, “overtone” resonances are still broadened due to indirect, second order effects arising from the large quadrupolar interaction. Here we demonstrate that another order of magnitude in spectral resolution may be gained by using double rotation. This brings the width of the 14N solid-state NMR lines much closer to the region commonly associated with high-resolution solid-state NMR spectroscopy of 15N and demonstrates the improvements in resolution that may be possible through the development of pulsed methodologies to suppress these second order effects.
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Accepted/In Press date: 4 August 2015
e-pub ahead of print date: 7 August 2015
Published date: 7 August 2015
Organisations:
Chemistry
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Local EPrints ID: 382234
URI: http://eprints.soton.ac.uk/id/eprint/382234
ISSN: 1463-9076
PURE UUID: 10bc3a66-7bd4-471c-a56b-388eca4474be
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Date deposited: 27 Oct 2015 13:32
Last modified: 15 Mar 2024 03:43
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Author:
Ibraheem M. Haies
Author:
James A. Jarvis
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