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  4. The refocused INADEQUATE MAS NMR experiment in multiple spin-systems: Interpreting observed correlation peaks and optimising lineshapes
 
research article

The refocused INADEQUATE MAS NMR experiment in multiple spin-systems: Interpreting observed correlation peaks and optimising lineshapes

Cadars, Sylvian
•
Sein, Julien
•
Duma, Luminita
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2007
Journal of Magnetic Resonance

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.

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Type
research article
DOI
10.1016/j.jmr.2007.05.016
Web of Science ID

WOS:000249750800003

Author(s)
Cadars, Sylvian
Sein, Julien
Duma, Luminita
Lesage, Anne
Pham, Tran N.
Baltisberger, Jay H.
Brown, Steven P.
Emsley, Lyndon  
Date Issued

2007

Publisher

Academic Press Inc - Elsevier Science

Published in
Journal of Magnetic Resonance
Volume

188

Issue

1

Start page

24

End page

34

Subjects

solid-state NMR

•

zero-quantum coherences

•

z-filter

•

multispin systems

•

INADEQUATE

•

solid-state

•

magic angle spinning

•

scalar coupling

•

through-bond spectroscopy

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/110063
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