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Sequential backbone assignment based on dipolar amide-to-amide correlation experiments

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Abstract

Proton detection in solid-state NMR has seen a tremendous increase in popularity in the last years. New experimental techniques allow to exploit protons as an additional source of information on structure, dynamics, and protein interactions with their surroundings. In addition, sensitivity is mostly improved and ambiguity in assignment experiments reduced. We show here that, in the solid state, sequential amide-to-amide correlations turn out to be an excellent, complementary way to exploit amide shifts for unambiguous backbone assignment. For a general assessment, we compare amide-to-amide experiments with the more common 13C-shift-based methods. Exploiting efficient CP magnetization transfers rather than less efficient INEPT periods, our results suggest that the approach is very feasible for solid-state NMR.

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Acknowledgments

R.L. acknowledges support from the Max-Planck Gesellschaft and the Fonds der Chemischen Industrie (FCI) in terms of a Liebig junior group fellowship. R.L. and S.X. acknowledge funding from the DFG Collaborative Research Center 803 (Project A4).

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    1. Department for NMR-Based Structural Biology, Max Planck Institute for Biophysical Chemistry, Göttingen, Germany

      ShengQi Xiang, Kristof Grohe, Petra Rovó, Suresh Kumar Vasa, Karin Giller, Stefan Becker & Rasmus Linser

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    1. ShengQi Xiang
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    2. Kristof Grohe
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    3. Petra Rovó
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    4. Suresh Kumar Vasa
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    Correspondence to Rasmus Linser.

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    ShengQi Xiang and Kristof Grohe have contributed equally to this work.

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    Xiang, S., Grohe, K., Rovó, P. et al. Sequential backbone assignment based on dipolar amide-to-amide correlation experiments. J Biomol NMR 62, 303–311 (2015). https://doi.org/10.1007/s10858-015-9945-4

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