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Determination of NMR interaction parameters from double rotation NMR

Hung, I. and Wong, A. and Howes, A. P. and Anupõld, Tiit and Past, J. and Samoson, A. and Mo, X. and Wu, G. and Smith, Mark E. and Brown, S. P. and Dupree, Ray (2007) Determination of NMR interaction parameters from double rotation NMR. Journal of Magnetic Resonance, 188 (2). pp. 246-259.

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Abstract

It is shown that the anisotropic NMR parameters for half-integer quadrupolar nuclei can be determined using double rotation (DOR) NMR at a single magnetic field with comparable accuracy to multi-field static and MAS experiments. The O-17 nuclei in isotopically enriched L-alanine and OPPh3 are used as illustrations. The anisotropic NMR parameters are obtained from spectral simulation of the DOR spinning sideband intensities using a computer program written with the GAMMA spin-simulation libraries. Contributions due to the quadrupolar interaction, chemical shift anisotropy, dipolar coupling and J coupling are included in the simulations. In L-alanine the oxygen chemical shift span is 455 ??- 20 ppm and 350 ??- 20 ppm for the O1 and O2 sites, respectively, and the Euler angles are determined to an accuracy of ??- 5-10 degrees. For cases where effects due to heteronuclear J and dipolar coupling are observed, it is possible to determine the angle between the internuclear vector and the principal axis of the electric field gradient (EFG). Thus, the orientation of the major components of both the EFG and chemical shift tensors (i.e., V-33 and delta(33)) in the molecular frame may be obtained from the relative intensity of the split DOR peaks. For OPPh3 the principal axis of the O-17 EFG is found to be close to the O-P bond, and the O-17-P-31 one-bond J coupling ((1)J(OP) = 161 ??- 2 Hz) is determined to a much higher accuracy than previously. (C) 2007 Elsevier Inc. All rights reserved.

Item Type: Article
Journal or Publication Title: Journal of Magnetic Resonance
Uncontrolled Keywords: solid-state NMR ; double rotation ; quadrupolar interaction ; chemical shift anisotropy ; J-coupling ; dipolar coupling ; oxygen-17
Subjects:
Departments: VC's Office
Faculty of Science and Technology > Lancaster Environment Centre
ID Code: 52874
Deposited By: ep_importer_pure
Deposited On: 27 Feb 2012 15:03
Refereed?: Yes
Published?: Published
Last Modified: 09 Apr 2014 23:10
Identification Number:
URI: http://eprints.lancs.ac.uk/id/eprint/52874

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