Recoupling of heteronuclear dipolar interactions in solid-state NMR using symmetry-based pulse sequences

Zhao, Xin; Edén, Mattias; Levitt, Malcolm H.

doi:10.1016/s0009-2614(01)00593-0

Cited by 142 publications

(198 citation statements)

References 27 publications

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“…The symmetry-based theory 33,34,36,41,42 introduced and developed by Levitt and co-workers provides a general principle for designing rotor-synchronized rf pulse sequences to selectively recouple and/or decouple various anisotropic spin interactions in MAS NMR spectroscopy. The symmetry-based approaches are classified as CN n v and RN n v schemes, depending on whether a "Cycle" or "Reverse" operation is applied on the irradiated spins by a basic pulse element.…”

Section: Resultsmentioning

confidence: 99%

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Hou

Byeon

Ahn

et al. 2012

The Journal of Chemical Physics

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C and15 N chemical shift (CS) interaction is a sensitive probe of structure and dynamics in a wide variety of biological and inorganic systems, and in the recent years several magic angle spinning NMR approaches have emerged for residue-specific measurements of chemical shift anisotropy (CSA) tensors in uniformly and sparsely enriched proteins. All of the currently existing methods are applicable to slow and moderate magic angle spinning (MAS) regime, i.e., MAS frequencies below 20 kHz. With the advent of fast and ultrafast MAS probes capable of spinning frequencies of 40-100 kHz, and with the superior resolution and sensitivity attained at such high frequencies, development of CSA recoupling techniques working under such conditions is necessary. In this work, we present a family of R-symmetry based pulse sequences for recoupling of 13 C/ 15 N CSA interactions that work well in both natural abundance and isotopically enriched systems. We demonstrate that efficient recoupling of either first-rank (σ 1 ) or second-rank (σ 2 ) spatial components of CSA interaction is attained with appropriately chosen γ -encoded RN n v symmetry sequences. The advantage of these γ -encoded RN n v -symmetry based CSA (RNCSA) recoupling schemes is that they are suitable for CSA recoupling under a wide range of MAS frequencies, including fast MAS regime. Comprehensive analysis of the recoupling properties of these RN n v symmetry sequences reveals that the σ 1 -CSA recoupling symmetry sequences exhibit large scaling factors; however, the partial homonuclear dipolar Hamiltonian components are symmetry allowed, which makes this family of sequences suitable for CSA measurements in systems with weak homonuclear dipolar interactions. On the other hand, the γ -encoded symmetry sequences for σ 2 -CSA recoupling have smaller scaling factors but they efficiently suppress the homonuclear dipole-dipole interactions. Therefore, the latter family of sequences is applicable for measurements of CSA parameters in systems with strong homonuclear dipolar couplings, such as uniformly-13 C labeled biological solids. We demonstrate RNCSA NMR experiments and numerical simulations establishing the utility of this approach to the measurements of 13

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Section: Resultsmentioning

confidence: 99%

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Hou

Byeon

Ahn

et al. 2012

The Journal of Chemical Physics

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“…The R18 5 2 sequence has been employed to recouple the heteronuclear 15 N-1 H dipolar couplings while decoupling the homonuclear proton dipolar interactions. 21,22 The experimental 2D spectrum shown in Fig. 10(a) Fig.…”

Section: Two-dimensional Homonuclear Correlation Spectroscopymentioning

confidence: 99%

“…11(d). 21,22 Ramped cross-polarization creates enhanced 15 N transverse magnetization that is subjected to a Hahn echo sequence of total duration T and a 180°pulse as refocusing pulse in the center of the evolution time interval. For a time t 1 , the 15 N transverse magnetization evolves in the presence of the R18 5 2 heteronuclear recoupling sequence on the protons.…”

Section: N-1 H Distance Measurementsmentioning

confidence: 99%

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Environmentally friendly flame retardants. A detailed solid-state NMR study of melamine orthophosphate

2007

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We used solid-state NMR spectroscopy to gain detailed information about the proton positions, proximities and the hydrogen-bonding network in the environmentally friendly flame retardant melamine orthophosphate (MP). High-resolution proton one- and two-dimensional solid-state NMR spectra were obtained at high external magnetic field in combination with fast magic angle spinning of the sample. Furthermore, we recorded homo- and heteronuclear correlation spectra of types (15)N–(15)N, (1)H–(13)C, (1)H–(15)N and (1)H–(31)P. In addition, we determined the geometry of the NH and NH(2) groups in MP by (15)N–(1)H heteronuclear recoupling experiments.We were able to completely assign the different isotropic chemical shifts in MP. Furthermore, we could identify the protonation of the melamine and orthophosphate moieties. The experimental results are discussed in connection with the structural model obtained by powder X-ray diffraction together with a combined molecular modeling-Rietveld refinement approach (De Ridder et al. Helv. Chim. Acta 2004; 87: 1894). We show that the geometry of the NH2 groups can only be successfully estimated by solid-state NMR.

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“…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. 49 50 However, in the case of single-quantum heteronuclear recoupling, the recoupled heteronuclear dipolar interactions do not commute for different spin pairs.…”

Section: Introductionmentioning

confidence: 99%

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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Recoupling of heteronuclear dipolar interactions in solid-state NMR using symmetry-based pulse sequences

Cited by 142 publications

References 27 publications

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Environmentally friendly flame retardants. A detailed solid-state NMR study of melamine orthophosphate

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

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Recoupling of heteronuclear dipolar interactions in solid-state NMR using symmetry-based pulse sequences

Cited by 142 publications

References 27 publications

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

Environmentally friendly flame retardants. A detailed solid-state NMR study of melamine orthophosphate

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

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