Efficient multispin homonuclear double-quantum recoupling for magic- angle spinning NMR: 13C-13C correlation spectroscopy of U-13C- erythromycin A

Chad M. Rienstra, Mary E. Hatcher, Leonard J. Mueller, Boqin Sun, Stephen W. Fesik, Robert G. Griffin

Research output: Contribution to journalArticlepeer-review

Abstract

We introduce a radio frequency (rf) pulse sequence for efficient homonuclear double-quantum dipolar recoupling under magic-angle spinning NMR. The sequence is optimized for two-dimensional double-quantum 13C-13C chemical shift correlation spectroscopy in multiple spin systems, such as the U-13C-labeled antibiotic erythromycin A. Spin systems such as this display a wide range of isotropic and anisotropic chemical shifts and, therefore, require a broadband dipolar recoupling sequence that minimizes the errors arising from the interaction of chemical shifts and rf inhomogeneity. The sequence should also preserve the theoretical efficiency over the powder average (~73%) provided by the C7 experiment of Levitt and co-workers (Lee, Y. K.; Kurur, N. D.; Helmle, M.; Johannessen, O. G.; Nielsen, N. C.; Levitt, M. H. Chem. Phys. Lett. 1995, 242, 304-309). We satisfy these criteria by combining the standard C7 (2π(φ)-2π{f+180)) elements with π-pulse permuted elements (π(φ)-2π(φ+180)-π(φ), in analogy to the MLEV decoupling scheme) to remove error terms over a ±10% range of rf amplitude. The new sequence, which we refer to as CMR7 (combined MLEV refocusing and C7), yields for two-spin systems broadband double-quantum filtering efficiencies greater than 70%. For multispin systems, the improved polarization transfer efficiency results in greater cross-peak intensities, facilitating assignment of U-13C-labeled molecules in the solid state.

Original languageEnglish (US)
Pages (from-to)10602-10612
Number of pages11
JournalJournal of the American Chemical Society
Volume120
Issue number41
DOIs
StatePublished - Oct 21 1998
Externally publishedYes

ASJC Scopus subject areas

  • Catalysis
  • Chemistry(all)
  • Biochemistry
  • Colloid and Surface Chemistry

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