title: Spectral editing: selection of methyl groups in multidimensional solid-state magic-angle spinning NMR.
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.
authors.affiliation: Leibniz-Institut für Molekulare Pharmakologie, Robert-Rössle-Strasse 10, D-13125, Berlin, Germany.
authors.forename: Stefan
authors.initials: S
authors.lastname: Jehle
authors.forename: Matthias
authors.initials: M
authors.lastname: Hiller
authors.forename: Kristina
authors.initials: K
authors.lastname: Rehbein
authors.forename: Anne
authors.initials: A
authors.lastname: Diehl
authors.forename: Hartmut
authors.initials: H
authors.lastname: Oschkinat
authors.forename: Barth-Jan
authors.initials: BJ
authors.lastname: van Rossum
mesh_terms: D000577:Amides / Q000737:chemistry; D000596:Amino Acids / Q000737:chemistry*; D001425:Bacterial Outer Membrane Proteins / Q000737:chemistry; D002247:Carbon Isotopes; D007930:Leucine / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008280:Magnetics; D008697:Methane / Q000737:chemistry; D009587:Nitrogen Isotopes
chemical_list: D000577:Amides; D000596:Amino Acids; D001425:Bacterial Outer Membrane Proteins; D002247:Carbon Isotopes; D009587:Nitrogen Isotopes; D007930:Leucine; D008697:Methane