A robust pulse sequence for the determination of small homonuclear dipolar couplings in magic-angle spinning NMR
A robust pulse sequence for the determination of small homonuclear dipolar couplings in magic-angle spinning NMR
We present a new solid-state NMR pulse sequence that accomplishes efficient broad-band dipolar recoupling in systems with small dipolar couplings and large chemical shift anisotropies. The method involves a supercycled symmetry-based recoupling sequence incorporated in a constant-interval data acquisition strategy. The supercycle removes destructive higher-order average Hamiltonian terms, and makes the method more robust at long time intervals. We demonstrate 38.4% double-quantum filtering efficiency on diammonium [1,4-13C2]-fumarate in which the internuclear distance, as estimated by X-ray diffraction, is 387.8 pm. The estimated 13C-13C dipolar coupling was -136.5±5.1 Hz, corresponding to an internuclear distance of 382.5±4 pm.
1-7
Kristiansen, Peter Eugen
3d73fca2-0139-41a6-9a36-1a097ed506ef
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Lai, Wai Cheu
29df4026-12c5-4a02-a271-8e7d19c10ec0
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
21 May 2004
Kristiansen, Peter Eugen
3d73fca2-0139-41a6-9a36-1a097ed506ef
Carravetta, Marina
1b12fa96-4a6a-4689-ab3b-ccc68f1d7691
Lai, Wai Cheu
29df4026-12c5-4a02-a271-8e7d19c10ec0
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
Kristiansen, Peter Eugen, Carravetta, Marina, Lai, Wai Cheu and Levitt, Malcolm H.
(2004)
A robust pulse sequence for the determination of small homonuclear dipolar couplings in magic-angle spinning NMR.
Chemical Physics Letters, 390 (1-3), .
(doi:10.1016/j.cplett.2004.03.075).
Abstract
We present a new solid-state NMR pulse sequence that accomplishes efficient broad-band dipolar recoupling in systems with small dipolar couplings and large chemical shift anisotropies. The method involves a supercycled symmetry-based recoupling sequence incorporated in a constant-interval data acquisition strategy. The supercycle removes destructive higher-order average Hamiltonian terms, and makes the method more robust at long time intervals. We demonstrate 38.4% double-quantum filtering efficiency on diammonium [1,4-13C2]-fumarate in which the internuclear distance, as estimated by X-ray diffraction, is 387.8 pm. The estimated 13C-13C dipolar coupling was -136.5±5.1 Hz, corresponding to an internuclear distance of 382.5±4 pm.
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Published date: 21 May 2004
Organisations:
Chemistry
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Local EPrints ID: 146481
URI: http://eprints.soton.ac.uk/id/eprint/146481
ISSN: 0009-2614
PURE UUID: 7ad9f6f5-a798-4e47-8144-6c02dc724035
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Date deposited: 21 Apr 2010 14:12
Last modified: 14 Mar 2024 02:47
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Author:
Peter Eugen Kristiansen
Author:
Wai Cheu Lai
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