Journal ArticleDOI
Two- and Three-Dimensional 13C-17O Heteronuclear Correlation NMR Spectroscopy for Studying Organic and Biological Solids.
Ivan Hung,Zhehong Gan,Gang Wu +2 more
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TLDR
In this paper, two-and three-dimensional (2D and 3D) 13C-17O heteronuclear correlation solid-state NMR experiments under magic-angle spinning (MAS) conditions were reported.Abstract:
We report two- and three-dimensional (2D and 3D) 13C-17O heteronuclear correlation solid-state NMR experiments under magic-angle spinning (MAS) conditions. These experiments utilize the D-RINEPT (Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer) scheme with symmetry-based SR412 recoupling blocks for coherence transfer between 13C and 17O nuclei. First, a 2D 17O → 13C correlation experiment was performed for the [1-13C,17O]-Gly/Gly·HCl cocrystal and [U-13C, 1-17O]-α/β-d-glucose samples. Second, a 2D 17O → 13C MQ-D-RINEPT correlation experiment where the indirect dimension incorporates the multiple-quantum MAS (MQMAS) scheme was tested for obtaining isotropic 17O resolution with [U-13C, 1-17O]-α/β-d-glucose. Third, a new 3D 17O → 13C → 13C correlation experiment was demonstrated where 17O → 13C and 13C → 13C correlations are achieved by D-RINEPT and DARR (Dipolar Assisted Rotational Resonance) sequences, respectively (thus termed as a 3D D-RINEPT/DARR OCC experiment). This new 3D 17O NMR experiment is implemented with the aim for site-resolved solid-state 17O NMR studies.read more
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Journal ArticleDOI
Solid-state 17O NMR study of α-d-glucose: exploring new frontiers in isotopic labeling, sensitivity enhancement, and NMR crystallography
Jiahui Shen,Victor V. Terskikh,Jochem Struppe,Alia Hassan,Martine Monette,Ivan Hung,Zhehong Gan,Andreas Brinkmann,Gang Wu +8 more
TL;DR: In this paper , the authors report synthesis and solid-state 17O NMR characterization of α-d-glucose for which all six oxygen atoms are site-specifically 17O-labeled.
Journal ArticleDOI
Residue-Specific High-Resolution 17O Solid-State Nuclear Magnetic Resonance of Peptides: Multidimensional Indirect 1H Detection and Magic-Angle Spinning.
TL;DR: In this paper , the use of 17O for initial polarization is found to provide better sensitivity per unit time compared to 1H, and the potential to determine sequential assignments and long-range distance restraints is demonstrated by using 3D 1H/13C/17O experiments, suggesting that such methods can become an essential tool for biomolecular structure determination.
Journal ArticleDOI
A combined solid-state NMR and quantum chemical calculation study of hydrogen bonding in two forms of α-d-glucose.
TL;DR: In this article , a detailed solid-state 1H NMR investigation of the model compounds α-d-glucose and α-dragon sulfate monohydrate was carried out using a combination of fast magic-angle spinning (MAS), combined rotation and multiple pulse spectroscopy (CRAMPS), and two-dimensional correlation experiments carried out at ultrahigh magnetic fields.
Journal ArticleDOI
Modeling the Structure of Crystalline Alamethicin and Its NMR Chemical Shift Tensors.
Jiří Czernek,Jiří Brus +1 more
TL;DR: In this paper, the plane-wave density-functional theory (PW DFT) was used to obtain the structure of desolvated crystalline alamethicin and predict the NMR chemical shift tensors (CSTs) of its nuclei.
Book ChapterDOI
Solid-state NMR of quadrupolar nuclei: Selected new methods and applications
TL;DR: New methods for solid-state NMR of quadrupolar nuclei are surveyed in this paper , with the focus largely on new or improved pulse sequences, and covers the past few years of literature up to early 2022.
References
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Journal ArticleDOI
A two-dimensional nuclear overhauser experiment with pure absorption phase in four quadrants☆
TL;DR: In this article, a method for obtaining pure absorption phase spectra in four quadrants in a two-dimensional nuclear magnetic resonance spin exchange experiment is described, which results in a substantial increase in resolution and discrimination while maintaining a signal-to-noise ratio comparable to that of the usual magnitude spectrum.
Journal ArticleDOI
Isotropic Spectra of Half-Integer Quadrupolar Spins from Bidimensional Magic-Angle Spinning NMR
Lucio Frydman,John S. Harwood +1 more
TL;DR: In contrast to what happens in spin-'/2 spectroscopy, no single-axis spinning techniques are available for canceling the effects of these second-order anisotropies as discussed by the authors.
Journal ArticleDOI
dipolar-assisted rotational resonance in magic-angle spinning NMR
TL;DR: In this article, a new 13 C -13 C recoupling mechanism was proposed for band-selective recouplings between carbonyl/aromatic carbons and aliphatic carbons under magic-angle spinning.
Journal ArticleDOI
Multiple-Quantum Magic-Angle Spinning NMR: A New Method for the Study of Quadrupolar Nuclei in Solids
TL;DR: In this paper, the authors have shown that the combined use of fast magic-angle spinning and bidimensional multiple-quantum (MQ) spectroscopy can refocus these anisotropies.
PatentDOI
Adiabatic pulses for wideband inversion and broadband decoupling
TL;DR: In this article, an inversion pulse for wideband application is obtained from a simple nonlinear amplitude modulation wherein the amplitude is modulated in accord with A(t)=A 0 {1-| sin βt| n } and the entire pulse is frequency modulated such that the phase varies as φ(t) =φ 0 + 1/2 kt 2