We describe solid-state NMR homonuclear recoupling experiments at high magic-angle spinning (MAS) frequencies using the radio frequency-driven recoupling (RFDR) scheme. The effect of heteronuclear decoupling interference during RFDR recoupling at high spinning frequencies is investigated experimentally and via numerical simulations, resulting in the identification of optimal decoupling conditions. The effects of MAS frequency, RF field amplitude, bandwidth, and chemical shift offsets are examined. Most significantly, it is shown that broadband homonuclear correlation spectra can be efficiently obtained using RFDR without decoupling during the mixing period in fully protonated samples, thus considerably reducing the rf power requirements for acquisition of correlation spectra. The utility of RFDR sans decoupling is demonstrated with broadband correlation spectra of a peptide and a model protein at high MAS frequencies and high magnetic field.
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7 February 2008
Research Article|
February 07 2008
Radio frequency-driven recoupling at high magic-angle spinning frequencies: Homonuclear recoupling sans heteronuclear decoupling
Marvin J. Bayro;
Marvin J. Bayro
Francis Bitter Magnet Laboratory and Department of Chemistry,
Massachusetts Institute of Technology
, Cambridge, Massachusetts 02139, USA
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Ramesh Ramachandran;
Ramesh Ramachandran
a)
Francis Bitter Magnet Laboratory and Department of Chemistry,
Massachusetts Institute of Technology
, Cambridge, Massachusetts 02139, USA
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Marc A. Caporini;
Marc A. Caporini
Francis Bitter Magnet Laboratory and Department of Chemistry,
Massachusetts Institute of Technology
, Cambridge, Massachusetts 02139, USA
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Matthew T. Eddy;
Matthew T. Eddy
Francis Bitter Magnet Laboratory and Department of Chemistry,
Massachusetts Institute of Technology
, Cambridge, Massachusetts 02139, USA
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Robert G. Griffin
Robert G. Griffin
b)
Francis Bitter Magnet Laboratory and Department of Chemistry,
Massachusetts Institute of Technology
, Cambridge, Massachusetts 02139, USA
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J. Chem. Phys. 128, 052321 (2008)
Article history
Received:
November 14 2007
Accepted:
December 19 2007
Citation
Marvin J. Bayro, Ramesh Ramachandran, Marc A. Caporini, Matthew T. Eddy, Robert G. Griffin; Radio frequency-driven recoupling at high magic-angle spinning frequencies: Homonuclear recoupling sans heteronuclear decoupling. J. Chem. Phys. 7 February 2008; 128 (5): 052321. https://doi.org/10.1063/1.2834736
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