Band-selective 13C homonuclear 3D spectroscopy for solid proteins at high field with rotor-synchronized soft pulses.

Journal of Biomolecular NMR
Donghua H ZhouChad M Rienstra

Abstract

We demonstrate improved 3D 13C-13C-13C chemical shift correlation experiments for solid proteins, utilizing band-selective coherence transfer, scalar decoupling and homonuclear zero-quantum polarization transfer. Judicious use of selective pulses and a z-filter period suppress artifacts with a two-step phase cycle, allowing higher digital resolution in a fixed measurement time. The novel correlation of C(ali)-C(ali)-CX (C(ali) for aliphatic carbons, CX for any carbon) reduces measurement time by an order of magnitude without sacrificing digital resolution. The experiment retains intensity from side-chain carbon resonances whose chemical shift dispersion is critical to minimize spectral degeneracy for large proteins with a predominance of secondary structure, such as beta-sheet rich fibrillar proteins and alpha-helical membrane proteins. We demonstrate the experiment for the beta1 immunoglobulin binding domain of protein G (GB1) and fibrils of the A30P mutant of alpha-synuclein, which is implicated in Parkinson's disease. Selective pulses of duration comparable the rotor period give optimal performance, but must be synchronized with the spinning in non-trivial ways to minimize chemical shift anisotropy recoupling effects. Soft p...Continue Reading

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Citations

Sep 12, 2006·Journal of Biomolecular NMR·Heather L FrericksChad M Rienstra
Sep 28, 2007·Journal of Biomolecular NMR·Kathryn D KloepperChad M Rienstra
Sep 19, 2012·Journal of Biomolecular NMR·Donghua H ZhouChad M Rienstra
Nov 6, 2009·Journal of the American Chemical Society·Jakob J LopezClemens Glaubitz
Dec 7, 2007·The Journal of Physical Chemistry. B·Heather L Frericks SchmidtChad M Rienstra
Aug 5, 2009·Physical Chemistry Chemical Physics : PCCP·Ye TianLeonard J Mueller
Sep 29, 2007·Journal of Magnetic Resonance·Amir GoldbourtAnn E McDermott
Dec 25, 2007·Magnetic Resonance in Chemistry : MRC·Jun YangTatyana Polenova
Dec 25, 2007·Magnetic Resonance in Chemistry : MRC·Mrignayani KotechaYoshitaka Ishii
Dec 18, 2014·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Huawei Liu, Shanmin Zhang
Dec 18, 2021·Frontiers in Molecular Biosciences·Reza AmaniBenjamin J Wylie

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