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Differential Line Broadening in MAS Solid-State NMR due to Dynamic Interference

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Veniamin Chevelkov,^† Katja Faelber,^† Anna Schrey,^† Kristina Rehbein,^† Anne Diehl,^† and Bernd Reif*^†^‡

Contribution from the Leibniz-Forschungsinstitut fr Molekulare Pharmakologie (FMP), Robert-Rssle-Str. 10, D-13125 Berlin, Germany, and Charit Universittsmedizin, D-10115 Berlin, Germany

J. Am. Chem. Soc., 2007, 129 (33), pp 10195–10200

DOI: 10.1021/ja072024c

Publication Date (Web): July 31, 2007

†

Leibniz-Forschungsinstitut für Molekulare Pharmakologie (FMP).

In papers with more than one author, the asterisk indicates the name of the author to whom inquiries about the paper should be addressed.

‡

Charité Universitätsmedizin.

, reif@fmp-berlin.de

Abstract

Many MAS (magic angle spinning) solid-state NMR investigations of biologically relevant protein samples are hampered by poor resolution, particularly in the ¹⁵N chemical shift dimension. We show that dynamics in the nanosecond−microsecond time scale in solid-state samples can induce significant line broadening of ¹⁵N resonances in solid-state NMR experiments. Averaging of ¹⁵NH^α^/^β multiplet components due to ¹H decoupling induces effective relaxation of the ¹⁵N coherence in case the N−H spin pair undergoes significant motion. High resolution solid-state NMR spectra can then only be recorded by application of TROSY (Transverse Relaxation Optimized Spectroscopy) type techniques which select the narrow component of the multiplet pattern. We speculate that this effect has been the major obstacle to the NMR spectroscopic characterization of many membrane proteins and fibrillar aggregates so far. Only in very favorable cases, where dynamics are either absent or very fast (picosecond), high-resolution spectra were obtained. We expect that this approach which requires intense deuteration will have a significant impact on the quality and the rate at which solid-state NMR spectroscopic investigations will emerge in the future.

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Published In Issue August 22, 2007
Received March 22, 2007

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Article

Differential Line Broadening in MAS Solid-State NMR due to Dynamic Interference