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The refocused INADEQUATE MAS NMR experiment in multiple spin-systems: interpreting observed correlation peaks and optimising lineshapes
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Cadars, Sylvian, Sein, Julien, Duma, Luminita, Lesage, Anne, Pham, Tran N., Baltisberger, Jay H., Brown, Steven P. and Emsley, Lyndon (2007) The refocused INADEQUATE MAS NMR experiment in multiple spin-systems: interpreting observed correlation peaks and optimising lineshapes. Journal of Magnetic Resonance, Vol.188 (No.1). pp. 24-34. doi:10.1016/j.jmr.2007.05.016 ISSN 1090-7807.
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Official URL: http://dx.doi.org/10.1016/j.jmr.2007.05.016
Abstract
The robustness of the refocused INADEQUATE MAS NMR pulse sequence for probing through-bond connectivities has been demonstrated in a large range of solid-state applications. This pulse sequence nevertheless suffers from artifacts when applied to multispin systems, e.g. uniformly labeled C-13 solids, which distort the lineshapes and can potentially result in misleading correlation peaks. In this paper, we present a detailed account that combines product-operator analysis, numerical simulations and experiments of the behavior of a three-spin system during the refocused INADEQUATE pulse sequence. The origin of undesired anti-phase contributions to the spectral lineshapes are described, and we show that they do not interfere with the observation of long-range correlations (e.g. two-bond C-13-C-13 correlations). The suppression of undesired contributions to the refocused INADEQUATE spectra is shown to require the removal of zero-quantum coherences within a z-filter. A method is proposed to eliminate zero-quantum coherences through dephasing by heteronuclear dipolar couplings, which leads to pure in-phase spectra. (C) 2007 Elsevier Inc. All rights reserved.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry Q Science > QC Physics |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
Journal or Publication Title: | Journal of Magnetic Resonance | ||||
Publisher: | Academic Press | ||||
ISSN: | 1090-7807 | ||||
Official Date: | September 2007 | ||||
Dates: |
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Volume: | Vol.188 | ||||
Number: | No.1 | ||||
Number of Pages: | 11 | ||||
Page Range: | pp. 24-34 | ||||
DOI: | 10.1016/j.jmr.2007.05.016 | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Access rights to Published version: | Restricted or Subscription Access |
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