Journal
JOURNAL OF MAGNETIC RESONANCE
Volume 212, Issue 2, Pages 320-329Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2011.07.011
Keywords
Solid-state NMR; Indirect homo-nuclear correlation; Bio-molecules; Ultra-fast MAS; Very-high magnetic field
Funding
- Region Nord/Pas de Calais
- Europe (FEDER)
- CNRS
- French Minister of Science
- USTL
- ENSCL
- CortecNet
- Bruker BIOSPIN
- TGIR RMN THC [FR-3050]
- Fundamental Research Funds for the Central Universities
- Shanghai Leading Talent Training Program [2007CB925200]
- [ANR-2010-jcjc-0811-01]
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We propose a new broadband second-order proton-assisted C-13-C-13 correlation experiment, SHANGHAI. The C-13-C-13 magnetization transfer is promoted by H-1 irradiation with interspersed four phases super-cycling. This through-space homo-nuclear sequence only irradiates on the proton channel during the mixing time. SHANGHAI benefits from a large number of modulation sidebands, hence leading to a large robustness with respect to chemical shift differences, which permits its use in a broad MAS frequency range. At ultra-fast MAS nu(R) >= 60 kHz), SHANGHAI is only efficient when the amplitude of H-1 recoupling rf-field is close to half the spinning speed (nu(1) approximate to nu(R)/2). However, at moderate to fast MAS (nu(R) = 20-35 kHz), SHANGHAI is efficient at any rf-power level larger than nu(1) approximate to 10 kHz, which simultaneously permits avoiding excessive heating of bio-molecules, and using large sample volumes. We show that SHANGHAI can be employed at the very high magnetic field of 23.5 T and then allows the observation of correlation between C-13 nuclei, even if their resonance frequencies differ by more than 38 kHz. (C) 2011 Elsevier Inc. All rights reserved.
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