Spectral editing: selection of methyl groups in multidimensional solid-state magic-angle spinning NMR

J Biomol NMR. 2006 Nov;36(3):169-77. doi: 10.1007/s10858-006-9078-x. Epub 2006 Sep 22.

Abstract

A simple spectroscopic filtering technique is presented that may aid the assignment of (13)C and (15)N resonances of methyl-containing amino-acids in solid-state magic-angle spinning (MAS) NMR. A filtering block that selects methyl resonances is introduced in two-dimensional (2D) (13)C-homonuclear and (15)N-(13)C heteronuclear correlation experiments. The 2D (13)C-(13)C correlation spectra are recorded with the methyl filter implemented prior to a (13)C-(13)C mixing step. It is shown that these methyl-filtered (13)C-homonuclear correlation spectra are instrumental in the assignment of C(delta) resonances of leucines by suppression of C(gamma)-C(delta) cross peaks. Further, a methyl filter is implemented prior to a (15)N-(13)C transferred-echo double resonance (TEDOR) exchange scheme to obtain 2D (15)N-(13)C heteronuclear correlation spectra. These experiments provide correlations between methyl groups and backbone amides. Some of the observed sequential (15)N-(13)C correlations form the basis for initial sequence-specific assignments of backbone signals of the outer-membrane protein G.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Amides / chemistry
  • Amino Acids / chemistry*
  • Bacterial Outer Membrane Proteins / chemistry
  • Carbon Isotopes
  • Leucine / chemistry
  • Magnetic Resonance Spectroscopy / methods*
  • Magnetics
  • Methane / chemistry
  • Nitrogen Isotopes

Substances

  • Amides
  • Amino Acids
  • Bacterial Outer Membrane Proteins
  • Carbon Isotopes
  • Nitrogen Isotopes
  • Leucine
  • Methane