Spectral editing: selection of methyl groups in multidimensional solid-state magic-angle spinning NMR.
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.
Jehle
Stefan
S
Leibniz-Institut für Molekulare Pharmakologie, Robert-Rössle-Strasse 10, D-13125, Berlin, Germany.
Hiller
Matthias
M
Rehbein
Kristina
K
Diehl
Anne
A
Oschkinat
Hartmut
H
van Rossum
Barth-Jan
BJ
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
D000577:Amides; D000596:Amino Acids; D001425:Bacterial Outer Membrane Proteins; D002247:Carbon Isotopes; D009587:Nitrogen Isotopes; D007930:Leucine; D008697:Methane