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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. ISSN 1463-9076

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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
Volume:	Vol.13
Number:	No.10
Page Range:	pp. 4514-4518
Identification Number:	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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URI:	http://wrap.warwick.ac.uk/id/eprint/39118