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Spin dynamics in the modulation frame: Application to homonuclear recoupling in magic angle spinning solid-state NMR

J. Chem. Phys. 128, 124503 (2008); doi:10.1063/1.2834732

Published 24 March 2008

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Gaël De Paëpe, Józef R. Lewandowski, and Robert G. Griffin
Francis Bitter Magnet Laboratory and Department of Chemistry, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139, USA
We introduce a family of solid-state NMR pulse sequences that generalizes the concept of second averaging in the modulation frame and therefore provides a new approach to perform magic angle spinning dipolar recoupling experiments. Here, we focus on two particular recoupling mechanisms—cosine modulated rotary resonance (CMpRR) and cosine modulated recoupling with isotropic chemical shift reintroduction (COMICS). The first technique, CMpRR, is based on a cosine modulation of the rf phase and yields broadband double-quantum (DQ) 13C recoupling using >70  kHz omega1,C/2pi rf field for the spinning frequency omegar/2=10–30  kHz and 1H Larmor frequency omega0,H/2pi up to 900  MHz. Importantly, for p>=5, CMpRR recouples efficiently in the absence of 1H decoupling. Extension to lower p values (3.5<=p<5) and higher spinning frequencies is possible using low power 1H irradiation (<0.25omegar/2pi). This phenomenon is explained through higher order cross terms including a homonuclear third spin assisted recoupling mechanism among protons. CMpRR mitigates the heating effects of simultaneous high power 13C recoupling and 1H decoupling. The second technique, COMICS, involves low power 13C irradiation that induces simultaneous recoupling of the 13C DQ dipolar and isotropic chemical shift terms. In contrast to CMpRR, where the DQ bandwidth (~30  kHz at omega0,H/2pi=750  MHz) covers the entire 13C spectral width, COMICS recoupling, through the reintroduction of the isotropic chemical shift, is selective with respect to the carrier frequency, having a typical bandwidth of ~100  Hz. This approach is intended as a general frequency selective method circumventing dipolar truncation (supplementary to R2 experiments). These new gamma-encoded sequences with attenuated rf requirements extend the applicability of homonuclear recoupling techniques to new regimes—high spinning and Larmor frequencies—and therefore should be of major interest for high resolution biomolecular studies. ©2008 American Institute of Physics
History: Received 4 December 2007; accepted 19 December 2007; published 24 March 2008
Permalink: http://link.aip.org/link/?JCPSA6/128/124503/1
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Supplemental Material

KEYWORDS and PACS

Keywords
PACS
  • 76.60.Lz
    Spin echoes (condensed matter NMR)
  • 76.60.Cq
    Chemical and Knight shifts (condensed matter NMR)
  • YEAR: 2008

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0021-9606 (print)   1089-7690 (online)
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  67. See EPAPS Document No. E-JCPSA6-128-032891 for details. This document contains 6 appendices and 1 table: Appendix A: Cosine and Sine expansion; Appendix B: Irreducible spherical tensor, ZQ and DQ operators; Appendix C: Scaling factor; Appendix D: Time dependent expression for the dipolar interaction; Appendix E: Euler angles and generalized CM-based interaction frame; Appendix F: Generalized CM-based interaction frame: Evaluation of the second order cross-terms; Table I: Theoretical phase modulation settings for CMpRR (sine). This document can be reached through a direct link in the online article's HTML reference section or via the EPAPS homepage (http://www.aip.org/pubservs/epaps.html). [EPAPS]

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