Journal ArticleDOI
Heteronuclear decoupling in rotating solids
Andrew E. Bennett,Chad M. Rienstra,Michèle Auger,Michèle Auger,K. V. Lakshmi,K. V. Lakshmi,Robert G. Griffin +6 more
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TLDR
In this article, a simple two pulse phase modulation (TPPM) scheme was proposed to reduce the residual linewidths arising from insufficient proton decoupling power in double resonance magic angle spinning (MAS) experiments.Abstract:
A simple two pulse phase modulation (TPPM) scheme greatly reduces the residual linewidths arising from insufficient proton decoupling power in double resonance magic angle spinning (MAS) experiments. Optimization of pulse lengths and phases in the sequence produces substantial improvements in both the resolution and sensitivity of dilute spins (e.g., 13C) over a broad range of spinning speeds at high magnetic field. The theoretical complications introduced by large homo‐ and heteronuclear interactions among the spins, as well as the amplitude modulation imposed by MAS, are explored analytically and numerically. To our knowledge, this method is the first phase‐switched sequence to exhibit improvement over continuous‐wave (cw) decoupling in a strongly coupled homogeneous spin system undergoing sample spinning.read more
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Solid state NMR sequential resonance assignments and conformational analysis of the 2×10.4 kDa dimeric form of the Bacillus subtilis protein Crh
Anja Böckmann,Adam Lange,Anne Galinier,Sorin Luca,Nicolas Giraud,Michel Juy,Henrike Heise,Roland Montserret,François Penin,Marc Baldus +9 more
TL;DR: This study reports resonance assignments for the largest protein investigated by solid state NMR so far and describes the conformational dimeric variant of Crh with previously unknown chemical shifts.
Journal ArticleDOI
Pulse sequence symmetries in the nuclear magnetic resonance of spinning solids: Application to heteronuclear decoupling
Mattias Edén,Malcolm H. Levitt +1 more
TL;DR: In this paper, the average Hamiltonian theory of a class of symmetrical radio-frequency pulse sequences in the NMR of rotating solids was developed, and the results were applied to the problem of heteronuclear decoupling in the presence of rapid magic angle spinning.
Journal ArticleDOI
Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR.
Marvin J. Bayro,Galia T. Debelouchina,Matthew T. Eddy,Neil R. Birkett,Catherine E. MacPhee,Melanie Rosay,Werner Maas,Christopher M. Dobson,Robert G. Griffin +8 more
TL;DR: Acquisition of low temperature spectra addresses a problem that is frequently encountered in MAS spectra of proteins, and establishes that the PI3-SH3 protein strands are aligned in a parallel, in-register arrangement within the amyloid fibril.
Journal ArticleDOI
The aggregation-enhancing Huntingtin N-terminus is helical in amyloid fibrils
V. N. Sivanandam,Murali Jayaraman,Cody L. Hoop,Ravindra Kodali,Ronald Wetzel,Patrick C.A. van der Wel +5 more
TL;DR: On magic-angle-spinning solid-state NMR studies of the amyloid-like aggregates of an htt N-terminal fragment, it is found that the polyQ portion of this peptide exists in a rigid, dehydrated amyloids core that is structurally similar to simpler polyQ fibrils and may contain antiparallel β-sheets.
Journal ArticleDOI
Solid-state NMR measurement of Ψ in peptides: a NCCN 2Q-heteronuclear local field experiment
TL;DR: In this article, a solid-state NMR experiment is presented for measuring λ torsion angles in (15N−13Cα-13CO-15N)-labeled peptides.
References
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Journal ArticleDOI
Proton‐enhanced NMR of dilute spins in solids
TL;DR: In this article, the NMR signals of isotopically or chemically dilute nuclear spins S in solids can be enhanced by repeatedly transferring polarization from a more abundant species I of high abundance (usually protons) to which they are coupled.
Book
Principles of high-resolution NMR in solids
Abstract: 1 Introduction.- 2 Nuclear Spin Interactions in Solids.- 2.1 Basic Nuclear Spin Interactions in Solids.- 2.2 Spin Interactions in High Magnetic Fields.- 2.3 Transformation Properties of Spin Interactions in Real Space.- 2.4 Powder Spectrum Line Shape.- 2.5 The NMR Spectrum. Lineshapes and Moments.- 2.6 Magic Angle Spinning (MAS).- 2.7 Rapid Anisotropic Molecular Rotation.- 2.8 Line Shapes in the Presence of Molecular Reorientation.- 3 Multiple-Pulse NMR Experiments.- 3.1 Idealized Multiple-Pulse Sequences.- 3.2 The Four-Pulse Sequence (WHH-4).- 3.3 Coherent Averaging Theory.- 3.4 Application of Coherent Averaging Theory to Multiple-Pulse Sequences.- 3.5 Arbitrary Rotations and Finite Pulse Width in Multiple-Pulse Experiments.- 3.6 Second Averaging.- 3.7 The Influence of Pulse Imperfections on Multiple-Pulse Experiments.- 3.8 Resolution of Multiple-Pulse Experiments.- 3.9 Magic Angle Rotating Frame Line Narrowing Experiments.- 3.10 Modulation Induced Line Narrowing.- 3.11 Applications of Multiple-Pulse Experiments.- 4 Double Resonance Experiments.- 4.1 Basic Principles of Double Resonance Experiments.- 4.2 Cross-Polarization of Dilute Spins.- 4.3 Cross-Polarization Dynamics.- 4.4 Spin-Decoupling Dynamics.- 4.5 Application of Cross-Polarization Experiments.- 5 Two-Dimensional NMR Spectroscopy.- 5.1 Basic Principles of 2 D-Spectroscopy.- 5.2 2D-Spectroscopy of 13C-1H Interactions in Solids.- 5.3 Applications of 2D-Spectroscopy.- 6 Multiple-Quantum NMR Spectroscopy.- 6.1 Double-Quantum Decoupling.- 6.2 The Three-Level System Double Quantum Coherence.- 6.3 Multiple-Quantum Coherence.- 6.4 Selective Multiple-Quantum Coherence.- 6.5 Double-Quantum Cross-Polarization.- 7 Magnetic Shielding Tensor.- 7.1 Ramsey's Formula.- 7.2 Approximate Calculations of the Shielding Tensor.- 7.3 Proton Shielding Tensors.- 7.4 19F Shielding Tensors.- 7.5 13C Shielding Tensors.- 7.6 Other Shielding Tensors.- 8 Spin-Lattice Relaxation.- 8.1 Spin-Lattice Relaxation in the Weak Collision Limit.- 8.2 Spin-Lattice Relaxation in Multiple-Pulse Experiments.- 8.3 Application of Multiple-Pulse Experiments to the Investigation of Spin-Lattice Relaxation.- 8.4 Spin-Lattice Relaxation in Dilute Spin Systems.- 8.5 Selective Excitation and Spectral Diffusion.- 9 Appendix.- A Irreducible Tensor Representation of Spin Interactions.- B Rotations.- C General Line Shape Theory.- D Homogeneous, Inhomogeneous and Heterogeneous Lineshapes.- E Lineshape and Relaxation due to Fluctuating Chemical Shift Tensors.- F Time Evolution and Magnus Expansion.- G Coherent Versus Secular Averaging Theory.- H Applications of Average Hamiltonian Theory.- I Relaxation Theory.- 10 References.- 11 Subject Index.
Journal ArticleDOI
Nuclear Magnetic Resonance Spectra from a Crystal rotated at High Speed
TL;DR: In this article, it was shown that when these weak side-spectra are included the second moment does indeed remain invariant even though the second moments of the central portion, which is all that is observed experimentally, becomes smaller.
Journal ArticleDOI
Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle
Journal ArticleDOI
An improved sequence for broadband decoupling: WALTZ-16
TL;DR: In this paper, the effects of the proton irradiation sequence by means of a train of spin rotation operators, the overall effect at the end of the cycle being calculated by explicit matrix multiplication, the offset dependence of this proton response determined the residual splitting of the carbon-13 resonance and hence the effectiveness of the decoupling.