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  4. Combination of DQ and ZQ Coherences for Sensitive Through-Bond NMR Correlation Experiments in Biosolids under Ultra-Fast MAS
 
research article

Combination of DQ and ZQ Coherences for Sensitive Through-Bond NMR Correlation Experiments in Biosolids under Ultra-Fast MAS

Webber, Amy L.
•
Pell, Andrew J.
•
Barbet-Massin, Emeline
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2012
CHEMPHYSCHEM

A double-zero quantum (DZQ)-refocused INADEQUATE experiment is introduced for J-based NMR correlations under ultra-fast (60 kHz) magic angle spinning (MAS). The experiment records two spectra in the same dataset, a double quantumsingle quantum (DQ-SQ) and zero quantumsingle quantum (ZQ-SQ) spectrum, whereby the corresponding signals appear at different chemical shifts in ?1. Furthermore, the spin-state selective excitation (S3E) J-decoupling block is incorporated in place of the second refocusing echo of the INADEQUATE scheme, providing an additional gain in sensitivity and resolution. The two sub-spectra acquired in this way can be treated separately by a shearing transformation, producing two diagonal-free single quantum (SQ-SQ)-type spectra, which are subsequently recombined to give an additional sensitivity enhancement, thus offering an improvement greater than a factor of two as compared to the original refocused INADEQUATE experiment. The combined DZQ scheme retains transverse magnetization on the initially polarized (I) spin, which typically exhibits a longer transverse dephasing time (T2') than its through-bond neighbour (S). By doing so, less magnetization is lost during the refocusing periods in the sequence to give even further gains in sensitivity for the J correlations. The experiment is demonstrated for the correlation between the carbonyl (CO) and alpha (CA) carbons in a microcrystalline sample of fully protonated, [15N,13C]-labelled CuII,?ZnII superoxide dismutase, and its efficiency is discussed with respect to other J-based schemes.

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Type
research article
DOI
10.1002/cphc.201200099
Web of Science ID

WOS:000305131000024

Author(s)
Webber, Amy L.
Pell, Andrew J.
Barbet-Massin, Emeline
Knight, Michael J.
Bertini, Ivano
Felli, Isabella C.
Pierattelli, Roberta
Emsley, Lyndon  
Lesage, Anne
Pintacuda, Guido
Date Issued

2012

Publisher

WILEY-V C H VERLAG GMBH

Published in
CHEMPHYSCHEM
Volume

13

Issue

9

Start page

2405

End page

2411

Subjects

double and zero quantum coherences

•

magic angle spinning

•

NMR spectroscopy

•

solid state

•

through-bond interactions

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/20.500.14299/109988
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