Proton MAS NMR Spectra at High Magnetic Fields and High Spinning Frequencies: Spectral Simulations Using Floquet Theory

Ray, Siddharth S.; Vinogradov, Elena; Boender, Gert Jan; Vega, Shimon

doi:10.1006/jmre.1998.9998

Cited by 26 publications

(30 citation statements)

References 19 publications

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“…Hence the inhomogeneous broadenings for different NMR nuclei in a sample are expected to be approximately constant ͑when expressed in ppm͒. Table III shows estimates of the inhomogeneous linewidths for 13 C and 1 H NMRs of a pair of samples with substantial inhomogeneous broadenings ͑essentially due to ABMS effects͒. This confirms that inhomogeneous linewidths are essentially the same in ppm ͑or, equivalently, scale with the magnetogyric ratio if expressed in frequency units͒.…”

Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 53%

“…Other published attempts to calculate ab initio proton spectra under MAS have involved Floquet methods. 13 Unfortunately, these scale particularly badly with increasing spin system size, and so the limit in this case was about seven nuclear spins.…”

Section: Introductionmentioning

confidence: 93%

“…Table III shows estimates of the inhomogeneous linewidths for two samples where the difference between the spin-echo and natural linewidth is large enough to enable reasonable estimates of the inhomogeneous linewidth to be made. Even in these cases, the values are estimates due to the systematic errors in modeling the spin-echo decays from both 1 H and 13 C data as single exponentials; e.g., spin-echo decay rates from decoupled 13 C spectra have been shown to vary with the 1 H decoupling method. 34 For comparison, an estimated value of about 0.3 ppm was obtained in Ref.…”

Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 99%

“…Inhomogeneous contributions to dilute-spin linewidths have been studied in detail for 13 C MAS NMR, 32,33 and so it is not necessary to revisit this existing work, given that the inhomogeneous broadenings are seen to be the same on both rare and abundant spins. It should be noted, however, that a broadening of, say, 0.3 ppm due to susceptibility effects or sample disorder has a much smaller impact on 13 C NMR, with its large chemical shift range, in comparison to 1 H NMR.…”

Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 99%

“…This limitation can be overcome, at the expense of significantly increased complexity, using Floquet treatments. [11][12][13] In general, however, exact treatments rapidly become intractable once more than two spins are involved. The resulting expressions provide little insight into the factors that determine what the effective 1 H resolution will be for a given sample and set of experimental conditions.…”

Section: Introductionmentioning

confidence: 99%

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Origins of linewidth in H1 magic-angle spinning NMR

Zorin

Brown

Hodgkinson

2006

The Journal of Chemical Physics

128

116

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A detailed study of the factors determining the linewidth (and hence resolution) in H1 solid-state magic-angle spinning NMR is described. Although it has been known from the early days of magic-angle spinning (MAS) that resolution of spectra from abundant nuclear spins, such as H1, increases approximately linearly with increasing sample rotation rate, the difficulty of describing the dynamics of extended networks of coupled spins has made it difficult to predict a priori the resolution expected for a given sample. Using recently developed, highly efficient methods of numerical simulation, together with experimental measurements on a variety of test systems, we propose a comprehensive picture of H1 resolution under MAS. The “homogeneous” component of the linewidth is shown to depend primarily on the ratio between an effective local coupling strength and the spin rate, modified by geometrical factors which loosely correspond to the “dimensionality” of the coupling network. The remaining “inhomogeneous” component of the natural linewidth is confirmed to have the same properties as in dilute-spin NMR. Variations in the NMR frequency due to chemical shift effects are shown to have minimal impact on H1 resolution. The implications of these results for solid-state NMR experiments involving H1 and other abundant-spin nuclei are discussed.

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Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 53%

Section: Introductionmentioning

confidence: 93%

Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 99%

Section: Inhomogeneous Contributions To 1 H Linewidthsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Origins of linewidth in H1 magic-angle spinning NMR

Zorin

Brown

Hodgkinson

2006

The Journal of Chemical Physics

128

116

View full text Add to dashboard Cite

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Assignment of the Nonexchanging Protons of theα-Spectrin SH3 Domain by Two- and Three- Dimensional1H-13C Solid-State Magic-Angle Spinning NMR and Comparison of Solution and Solid-State Proton Chemical Shifts

et al. 2001

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The assignment of nonexchanging protons of a small microcrystalline protein, the alpha-spectrin SH3 domain (7.2 kDa, 62 residues), was achieved by means of three-dimensional (3D) heteronuclear (1H-13C-13C) magic-angle spinning (MAS) NMR dipolar correlation spectroscopy. With the favorable combination of a high B(0)-field, a moderately high spinning frequency, and frequency-switched Lee-Goldburg irradiation applied during 1H evolution, a proton linewidth < or =0.5 ppm at 17.6 Tesla was achieved for the particular protein preparation used. A comparison of the solid-state 1H chemical shifts with the shifts found in solution shows a remarkable similarity, which reflects the identical protein structures in solution and in the solid. Significant differences between the MAS solid- and liquid-state 1H chemical shifts are only observed for residues that are located at the surface of the protein and that exhibit contacts between different SH3 molecules. In two cases, aromatic residues of neighboring SH3 molecules induce pronounced upfield ring-current shifts for protons in the contact area.

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Recent Advances in Magic‐Angle Spinning Solid‐State NMR of Proteins

Ladizhansky¹

2014

Israel Journal of Chemistry

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Magic‐angle spinning (MAS) solid‐state NMR (SSNMR) spectroscopy is emerging as an important technique for the determination of three‐dimensional structures of biological molecules and for the characterization of their dynamics. While there is an established suite of MAS SSNMR experiments for protein structure determination in small‐ and medium‐sized proteins, these methods face many challenges in large systems. In this review, recent progress in MAS NMR spectroscopy is discussed, specifically focusing on the emerging developments aimed at improving the sensitivity and resolution of SSNMR that are likely to determine its future applications. These developments include sample preparation and isotopic labeling strategies, fast MAS, proton detection, and paramagnetic NMR spectroscopy.

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Proton MAS NMR Spectra at High Magnetic Fields and High Spinning Frequencies: Spectral Simulations Using Floquet Theory

Cited by 26 publications

References 19 publications

Origins of linewidth in H1 magic-angle spinning NMR

Origins of linewidth in H1 magic-angle spinning NMR

Assignment of the Nonexchanging Protons of theα-Spectrin SH3 Domain by Two- and Three- Dimensional1H-13C Solid-State Magic-Angle Spinning NMR and Comparison of Solution and Solid-State Proton Chemical Shifts

Recent Advances in Magic‐Angle Spinning Solid‐State NMR of Proteins

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