Symmetry‐Based Pulse Sequences in Magic‐Angle Spinning Solid‐State NMR

Levitt, Malcolm H.

doi:10.1002/chin.200338276

Cited by 71 publications

(186 citation statements)

References 54 publications

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“…16,17 In the last decades a series of homonuclear and heteronuclear recoupling experiments have been developed that combine a 2D approach with fast MAS and dipolar multiple-quantum NMR spectroscopy. In this way, the chemical shift resolution of different chemical environments allows sites of interest to be distinguished and fully identified, and then it is possible to obtain structural information since dipole-dipole couplings are sensitive to the distances between the coupled nuclei as well as to the orientation of the internuclear vector.…”

Section: Solid-state Nmr Techniquesmentioning

confidence: 99%

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Solid‐State NMR Studies on Supramolecular Chemistry

Chierotti

Gobetto

2012

Supramolecular Chemistry

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Solid‐state NMR (SSNMR) methods provide new insights in the investigation of the structure and dynamics of condensed phases. Advances in commercial solid‐state hardware and the developments of new pulse sequences have been of paramount importance for overcoming the earlier resolution problems and yield spectra sensitive to intra‐ and intermolecular hydrogen‐bonding and π–π interactions. This chapter aims to provide an overview of the recent development of the technique for the study of the structure and dynamics of supramolecular systems paying particular attention to the role of the weak interactions such as hydrogen bonds through NMR chemical shift as well as the through‐space dipolar coupling SSNMR investigations.

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Section: Solid-state Nmr Techniquesmentioning

confidence: 99%

“…Under MAS conditions the excitation of DQ coherences requires the use of a recoupling pulse sequence. 16,17 The most used is the BABA scheme, 18 whose acronym comes from the presence of very closely spaced pulses (back-to-back) in the time domain.…”

Section: Solid-state Nmr Techniquesmentioning

confidence: 99%

Solid‐State NMR Studies on Supramolecular Chemistry

Chierotti

Gobetto

2012

Supramolecular Chemistry

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“…The symmetry-based RN n ν recoupling sequences, possible supercycles, and the theory of these schemes in first-and secondorder average Hamiltonians have been discussed in great detail before. 30,31,47,[57][58][59][60][61] Here we will briefly summarize the main results in view of our application. For simplicity consider a spin system consisting of a single half-integer quadrupolar S-spin and several spin-1 / 2 I-spins.…”

Section: Symmetry-based Heteronuclear Longitudinal Two-spin-order Dipmentioning

confidence: 99%

“…30 Pulse sequences denoted R18 1 7 and R18 2 5 have been described, which are applied to the I-spins and accomplish single-quantum recoupling of the heteronuclear dipolar interactions while suppressing the I-spin homonuclear dipolar couplings. [47][48][49] These sequences lead to strong dipolar oscillations in powdered samples and have been successfully used to detect perturbations of 15 N-1 H bond lengths caused by intermolecular hydrogen bonds.…”

Section: Introductionmentioning

confidence: 99%

“…These sequences achieve heteronuclear longitudinal two-spin-order (I z S z ) recoupling, hence not suffering from dipolar truncation, while decoupling the I-spin homonuclear dipolar couplings. 31,30 The heteronuclear longitudinal two-spin-order recoupling sequences are demonstrated by numerical simulations and by experimentally estimating the 17 In this contribution we combine the approaches described above to develop a comprehensive methodology to study hydrogen bonding in biological systems through 17 O and 17 O-1 H NMR.…”

Section: Introductionmentioning

confidence: 99%

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Sensitivity Enhancement and Heteronuclear Distance Measurements in Biological ¹⁷O Solid-State NMR

Brinkmann

Kentgens

2006

J. Phys. Chem. B

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In this contribution we present a comprehensive approach to study hydrogen bonding in biological and biomimetic systems through 17 O and 17 O-1 H solid-state NMR combined with density functional theory calculations of 17 O and 1 H NMR parameters. We explore the signal enhancement of 17 O in L-tyrosine‚HCl using repetitive double-frequency swept radio frequency pulses in solid-state NMR. The technique is compatible with high magnetic fields and fast magic-angle spinning of the sample. A maximum enhancement by a factor of 4.3 is obtained in the signal-to-noise ratio of the selectively excited 17 O central transition in a powdered sample of 17 O η -L-tyrosine‚HCl at an external field of 14.1 T and a spinning frequency of 25 kHz. As little as 128 transients lead to meaningful 17 O spectra of the same sample at an external field of 18.8 T and a spinning frequency of 50 kHz. Furthermore we employed supercycled symmetry-based pulse sequences on the protons to achieve heteronuclear longitudinal two-spin-order (I z S z ) recoupling to determine 17 O-1 H distances. These sequences recouple the heteronuclear dipolar 17 O-1 H couplings, where dipolar truncation is absent, while decoupling the homonuclear proton dipolar interactions. They can be applied at fast magic-angle-spinning frequencies up and beyond 50 kHz and are very robust with respect to 17 O quadrupolar couplings and both 17O and 1 H chemical shift anisotropies, which makes them suitable for the use at high external magnetic fields. The method is demonstrated by determining the 17 O η -1 H distance in L-tyrosine‚HCl at a spinning frequency of 50 kHz and an external field of 18.8 T.

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Methodological development of solid‐state NMR for characterization of membrane proteins

Bjerring

Vosegaard

Malmendal

et al. 2003

Concepts Magnetic Resonance

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Solid-state NMR is a promising method for structural analysis of membrane proteins. The method is capable of providing atomic-resolution structure information without the need for crystals or fast molecular motion as is required for X-ray diffraction and liquid-state NMR, respectively. However, it is clear that solid-state NMR still needs substantial methodological development before it can provide the desired detailed information about large structures or be applied routinely for structure-function relationship studies. Here, we address some important considerations and elements in the solid-state NMR methodology relevant for characterization of membrane proteins. These are relevant for establishing the appropriate technology and may serve as an inspiration for future developments in synthesis, isotope labeling, and physical preparation of samples for solid-state NMR characterization

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Symmetry‐Based Pulse Sequences in Magic‐Angle Spinning Solid‐State NMR

Abstract: For Abstract see ChemInform Abstract in Full Text.

Cited by 71 publications

References 54 publications

Solid‐State NMR Studies on Supramolecular Chemistry

Solid‐State NMR Studies on Supramolecular Chemistry

Sensitivity Enhancement and Heteronuclear Distance Measurements in Biological ¹⁷O Solid-State NMR

Methodological development of solid‐state NMR for characterization of membrane proteins

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Symmetry‐Based Pulse Sequences in Magic‐Angle Spinning Solid‐State NMR

Abstract: For Abstract see ChemInform Abstract in Full Text.

Cited by 71 publications

References 54 publications

Solid‐State NMR Studies on Supramolecular Chemistry

Solid‐State NMR Studies on Supramolecular Chemistry

Sensitivity Enhancement and Heteronuclear Distance Measurements in Biological 17O Solid-State NMR

Methodological development of solid‐state NMR for characterization of membrane proteins

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Sensitivity Enhancement and Heteronuclear Distance Measurements in Biological ¹⁷O Solid-State NMR