3D 1H–13C–14N correlation solid-state NMR spectrum

Siegel, Renée; Trébosc, Julien; Amoureux, Jean‐Paul; Gan, Zhehong

doi:10.1016/j.jmr.2008.05.013

Cited by 21 publications

(31 citation statements)

References 35 publications

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“…The selectivity with which 1 H-13 C cross-peaks are observed can be controlled by a selective (differing) 1 H-13 C cross-polarization step. It must be noted that this experiment does not require a very large magnetic field, a perfectly adjusted magic angle or a perfectly stabilized spinning speed, as with previous 1 H- 14 N and 13 C-14 N HMQC experiments [9][10][11][12][13][14]. Indeed, the different 14 N magnetizations are utilized, instead of being observed as previously.…”

Section: Resultsmentioning

confidence: 89%

“…Spectra (b and c) are acquired using a pulse sequence that selects pure SQ 14 close proximity to nitrogen-14 nuclei. The selectivity with which 1 H-13 C cross-peaks are observed can be controlled by a selective (differing) 1 H-13 C cross-polarization step.…”

Section: Resultsmentioning

confidence: 99%

“…Thus, nitrogen NMR has been mostly limited to the less abundant isotope 15 N, hence requiring isotopic enrichment. The main difficulty in observing 14 N arises from the large quadrupole interaction, which results in broad NMR spectra of molecules in both liquid and solid states. In solutions, the broadening comes from very fast quadrupolar relaxation mechanisms.…”

Section: Introductionmentioning

confidence: 99%

“…As the dipolar coupling is much larger than both the J-coupling and RDS, Gan et al obtained a 2D 1 H-14 N correlation NMR spectrum in just a few minutes using the rotary resonance recoupling (R 3 ) D-HMQC experiment [13]. Recently, it has been shown on a 13 C enriched L-histidine.HClÁH 2 O sample that a 3D 1 H-13 C-14 N correlation spectrum could also be obtained using the through-space dipolar interaction [14]. The efficiency of 13 C-14 N-13 C transfer was very weak (4-5%) and the experiment lasted 85 h on a 18.8 T spectrometer.…”

Section: Introductionmentioning

confidence: 99%

“…The SPIDER experiment is mainly suitable for slow spinning rates (m R % 5 kHz), which are not sufficient to cancel the 13 C chemical shift anisotropy (CSA) on high-field spectrometers. We propose here a new magic angle spinning (MAS) 14 N-edited method for 1 H-13 C through-space HETCOR spectra to obtain high-resolution in both dimensions. We combine latest hetero-recoupling (Simultaneous Frequency and Amplitude Modulation: SFAM 2 ) [16,17] and homo-decoupling (Smooth Amplitude Modulation: SAM 3 ) [18] techniques along with a filter based on 13 C-14 N D-HMQC experiment.…”

Section: Introductionmentioning

confidence: 99%

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High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids

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Section: Resultsmentioning

confidence: 89%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids

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Trébosc²,

Hu³

et al. 2008

Journal of Magnetic Resonance

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Nitrogen-14 NMR Studies of Biological Systems

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Solid‐State NMR Spectroscopy: Introduction for Solid‐State Chemists

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Handbook of Solid State Chemistry

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Solid‐state nuclear magnetic resonance spectroscopy ( ssNMR ) is a powerful and flexible tool for deriving structural and dynamical information for a broad variety of material classes ranging from metals, intermetallics, and ceramics over organic, inorganic, and metal–organic frameworks to molecular crystals and polymers. The combination of relaxation experiments, lineshape analyses, and 2 D exchange techniques spans a dynamical window of about 14 decades with correlation times ranging from 10 −12 s for fast ion conduction and up to 100 s for the relaxation close to the glass transition. ssNMR is element selective and thus able to identify chemical building units and simultaneously probes their homo‐ and heteronuclear through‐bond and through‐space connectivities, orientation correlations, as well as distances up to a few nanometers. Thus, ssNMR is ideally suited and often used to complement diffraction studies and quantum chemical calculations. It does not suffer from a loss of long‐range order and may equally be applied to crystalline, disordered, and amorphous materials to make progress on the structure elucidation of complex compounds. This chapter provides an overview of fundamental aspects of ssNMR , including the most important nuclear spin interactions and their typical spectral lineshapes for both wideline and high‐resolution experiments. Based on this, we describe the development and application of various 1 D and 2 D NMR techniques, for both structural and dynamical aspects, on selected examples taken from the recent literature. In particular, we focus on strengths, weaknesses, and the expressiveness of the individual methods.

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3D 1H–13C–14N correlation solid-state NMR spectrum

Cited by 21 publications

References 35 publications

High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids

High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids

Nitrogen-14 NMR Studies of Biological Systems

Solid‐State NMR Spectroscopy: Introduction for Solid‐State Chemists

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