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Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy
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Becker-Baldus, Johanna, Kemp, Thomas F., Past, Jaan, Reinhold, Andres, Samoson, Ago and Brown, Steven P. (2011) Longer-range distances by spinning-angle-encoding solid-state NMR spectroscopy. Physical Chemistry Chemical Physics, Vol.13 (No.10). pp. 4514-4518. doi:10.1039/c0cp02364g
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Official URL: http://dx.doi.org/10.1039/C0CP02364G
Abstract
A new spinning-angle-encoding spin-echo solid-state NMR approach is used to accurately determine the
dipolar coupling corresponding to a C-C distance over 4 Å in a fully labelled dipeptide. The dipolar coupling
dependent spin-echo modulation was recorded off magic angle, switching back to the magic angle for the
acquisition of the free-induction decay, so as to obtain optimum sensitivity. The retention of both ideal
resolution and long-range distance sensitivity was achieved by redesigning a 600MHz HXMAS NMR probe
to provide fast angle switching during the NMR experiment: For 1.8 mm rotors, angle changes of up to ~5
degrees in ~10 ms were achieved at 12 kHzMAS. A new experimental design that combines a reference and a
dipolar-modulated experiment and a master-curve approach to data interpretation is presented.
| Item Type: | Journal Article | ||||
|---|---|---|---|---|---|
| Subjects: | Q Science > QC Physics | ||||
| Divisions: | Faculty of Science > Physics | ||||
| Library of Congress Subject Headings (LCSH): | Nuclear magnetic resonance spectroscopy | ||||
| Journal or Publication Title: | Physical Chemistry Chemical Physics | ||||
| Publisher: | Royal Society of Chemistry | ||||
| ISSN: | 1463-9076 | ||||
| Official Date: | 2011 | ||||
| Dates: |
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| Volume: | Vol.13 | ||||
| Number: | No.10 | ||||
| Page Range: | pp. 4514-4518 | ||||
| DOI: | 10.1039/c0cp02364g | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access | ||||
| Funder: | Engineering and Physical Sciences Research Council (EPSRC) |
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