DNP Enhanced Frequency-Selective TEDOR Experiments in Bacteriorhodopsin
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Author(s) • • • •
Bajaj, Vikram S.
Mak-Jurkauskas, Melody L.
Belenky, Marina
Herzfeld, Judith
Griffin, Robert Guy
Date Issued
September 2009
Journal
Journal of Magnetic Resonance
Publisher
Elsevier
Version
Author's final manuscript
Abstract
We describe a new approach to multiple [superscript 13]C–[superscript 15]N distance measurements in uniformly labeled solids, frequency-selective (FS) TEDOR. The method shares features with FS-REDOR and ZF- and BASE-TEDOR, which also provide quantitative [superscript 15]N–[superscript 13]C spectral assignments and distance measurements in U-[[superscript 13]C,[superscript 15]N] samples. To demonstrate the validity of the FS-TEDOR sequence, we measured distances in [U-[superscript 13]C,15N]-asparagine which are in good agreement with other methods. In addition, we integrate high frequency dynamic nuclear polarization (DNP) into the experimental protocol and use FS-TEDOR to record a resolved correlation spectrum of the Arg-[superscript 13]Cγ–[superscript 15]Nε region in [U-[superscript 13]C,15N]-bacteriorhodopsin. We resolve six of the seven cross-peaks expected based on the primary sequence of this membrane protein.
MIT Department
Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)
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DOI of Published Version
https://doi.org/10.1016/j.jmr.2009.09.005