Hybridization of TEDOR and NCX MAS Solid-state NMR Experiments for Simultaneous Acquisition of Heteronuclear Correlation Spectra and Distance Measurements

Overview

Journal J Biomol NMR

Publisher Springer

Specialties Molecular Biology
Nuclear Medicine

Date 2019 Feb 27

PMID 30805819

Citations 5

Authors

T Gopinath

Songlin Wang

John Lee

Hideki Aihara

Gianluigi Veglia

Affiliations

Soon will be listed here.

Abstract

Magic angle spinning (MAS) solid-state NMR (ssNMR) spectroscopy is a major technique for the characterization of the structural dynamics of biopolymers at atomic resolution. However, the intrinsic low sensitivity of this technique poses significant limitations to its routine application in structural biology. Here we achieve substantial savings in experimental time using a new subclass of Polarization Optimized Experiments (POEs) that concatenate TEDOR and SPECIFIC-CP transfers into a single pulse sequence. Specifically, we designed new 2D and 3D experiments (2D TEDOR-NCX, 3D TEDOR-NCOCX, and 3D TEDOR-NCACX) to obtain distance measurements and heteronuclear chemical shift correlations for resonance assignments using only one experiment. We successfully tested these experiments on N-Acetyl-Val-Leu dipeptide, microcrystalline U-C,N ubiquitin, and single- and multi-span membrane proteins reconstituted in lipid membranes. These pulse sequences can be implemented on any ssNMR spectrometer equipped with standard solid-state hardware using only one receiver. Since these new POEs speed up data acquisition considerably, we anticipate their broad application to fibrillar, microcrystalline, and membrane-bound proteins.

Citing Articles

A kink in DWORF helical structure controls the activation of the sarcoplasmic reticulum Ca-ATPase.

Reddy U, Weber D, Wang S, Larsen E, Gopinath T, De Simone A Structure. 2021; 30(3):360-370.e6.

PMID: 34875216 PMC: 8897251. DOI: 10.1016/j.str.2021.11.003.

Solid-State NMR of Membrane Proteins in Lipid Bilayers: To Spin or Not To Spin?.

Gopinath T, Weber D, Wang S, Larsen E, Veglia G Acc Chem Res. 2021; 54(6):1430-1439.

PMID: 33655754 PMC: 11457538. DOI: 10.1021/acs.accounts.0c00670.

Multi-receiver solid-state NMR using polarization optimized experiments (POE) at ultrafast magic angle spinning.

Gopinath T, Weber D, Veglia G J Biomol NMR. 2020; 74(4-5):267-285.

PMID: 32333193 PMC: 7236978. DOI: 10.1007/s10858-020-00316-y.

Proton-detected polarization optimized experiments (POE) using ultrafast magic angle spinning solid-state NMR: Multi-acquisition of membrane protein spectra.

Gopinath T, Veglia G J Magn Reson. 2019; 310:106664.

PMID: 31837552 PMC: 7003683. DOI: 10.1016/j.jmr.2019.106664.

T* weighted Deconvolution of NMR Spectra: Application to 2D Homonuclear MAS Solid-State NMR of Membrane Proteins.

V S M, Gopinath T, Wang S, Veglia G Sci Rep. 2019; 9(1):8225.

PMID: 31160739 PMC: 6546711. DOI: 10.1038/s41598-019-44461-3.

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