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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

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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:
DateEvent
2011Published
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)

Data sourced from Thomson Reuters' Web of Knowledge

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