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. 2007;46(44):8380-3.
doi: 10.1002/anie.200702905.

Solid-state protein-structure determination with proton-detected triple-resonance 3D magic-angle-spinning NMR spectroscopy

Donghua H Zhou  1 , John J Shea, Andrew J Nieuwkoop, W Trent Franks, Benjamin J Wylie, Charles Mullen, Dennis Sandoz, Chad M Rienstra
Affiliations

Solid-state protein-structure determination with proton-detected triple-resonance 3D magic-angle-spinning NMR spectroscopy

Donghua H Zhou et al. Angew Chem Int Ed Engl. 2007.
No abstract available

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Figures

Figure 1
Figure 1
Solid-state 1H-detected 15N-1H 2D spectrum of uniformly-13C,15N,2H-labeled GB1, back-exchanged with H2O (750 MHz, 39 kHz MAS, 2 s recycle delay, 2 scans per row, t1max(15N) = 50 ms, t2max(1H) = 30 ms, total 30 min). No apodization or post-acquisition solvent suppression was applied. Assignments were derived from 3D experiments.
Figure 2
Figure 2
2D planes of (a) CON(H)H 3D (39 kHz MAS, 750 MHz, 2 s recycle delay, 2 scans per row, t1max(13C) = 18.8 ms, t2max(15N) = 30 ms, t3max(1H) = 30 ms, total 36 h) and (b) HN(H)H 3D (2 scans per row, t1max(1H) = 12 ms, t2max(15N) = 30 ms, t3max(1H) = 30 ms, total 36 h), with ω2 frequency indicated at the top. For both 2 ms RFDR[10] was used. Line broadening of 10, 10, 40 Hz was applied to 15N, 13C, and 1H dimensions, respectively. The backbone walk is traced by arrows.
Figure 3
Figure 3
N(H)H 2D spectrum of GB1 with 3 ms RFDR[10] (39 kHz MAS, 750 MHz, 2 s recycle delay, 8 scans per row, t1max(15N) = 50 ms, t2max(1H) = 30 ms, total 2 h). The 15N dimension was apodized by sine bell (shift=45°), and 1H by squared sine bell (shift=72°), −40 Hz Lorentzian, +80 Hz Gaussian functions. The inter-residue peaks are labeled with a suffix to indicate either 15N or 1H resonance frequency.
Figure 4
Figure 4
Ensemble of GB1 backbone structures calculated from SSNMR proton-proton distances and dihedral constraints, shown with two views for the ten lowest energy structures from 252 calculations. The backbone RMSD is 0.82±0.14 Å.
See this image and copyright information in PMC

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