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.

journal_name

J Biomol NMR

authors

Jehle S,Hiller M,Rehbein K,Diehl A,Oschkinat H,van Rossum BJ

doi

10.1007/s10858-006-9078-x

subject

Has Abstract

pub_date

2006-11-01 00:00:00

pages

169-77

issue

3

eissn

0925-2738

issn

1573-5001

journal_volume

36

pub_type

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