New Horizons for Magic-Angle Spinning NMR

Samoson, Ago; Tuherm, Tiit; Past, Jaan; Reinhold, Andres; Anupõld, Tiit; Heinmaa, Ivo

doi:10.1007/b98647

Cited by 122 publications

(96 citation statements)

References 3 publications

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“…For experiments at the spinning of 40 kHz, we used a 2.0-mm MAS double-resonance probe developed in Dr. Samoson's lab. [32][33][34] Unless otherwise mentioned, the signals were collected during an acquisition period of 20 ms at the spinning speed of 40,000 ± 10 Hz with cooling air at −5 °C supplied through the Varian VT stack at a flow rate of ∼140 scfh and cooled bearing air (1 °C ). The data were processed with Varian Spinsight software.…”

Section: Methodsmentioning

confidence: 99%

Sensitivity enhancement in 13C solid-state NMR of protein microcrystals by use of paramagnetic metal ions for optimizing 1H T1 relaxation

Wickramasinghe

Kotecha

Samoson

et al. 2007

Journal of Magnetic Resonance

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119

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We discuss a simple approach to enhance sensitivity for 13 C high-resolution solid-state NMR for proteins in microcrystals by reducing 1 H T 1 relaxation times with paramagnetic relaxation reagents. It was shown that 1 H T 1 values can be reduced from 0.4-0.8 s to 60-70 ms for ubiquitin and lysozyme in D 2 O in the presence of 10 mM Cu(II)Na 2 EDTA without substantial degradation of the resolution in 13 C CPMAS spectra. Faster signal accumulation using the shorter 1 H T 1 attained by paramagnetic doping provided sensitivity enhancements of 1.4-2.9 for these proteins, reducing the experimental time for a given signal-to-noise ratio by a factor of 2.0-8.4. This approach presented here is likely to be applicable to various other proteins in order to enhance sensitivity in 13 C high-resolution solidstate NMR spectroscopy.

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Section: Methodsmentioning

confidence: 99%

Sensitivity enhancement in 13C solid-state NMR of protein microcrystals by use of paramagnetic metal ions for optimizing 1H T1 relaxation

Wickramasinghe

Kotecha

Samoson

et al. 2007

Journal of Magnetic Resonance

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119

110

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“…Nevertheless, fast MAS brings a considerable improvement in resolution. While experimental results show that proton linewidths decrease only linearly with the rotor speed, the effect is more pronounced in 2D spectra where the 2 [11]. Fast MAS increasing the utility of proton NMR is more relevant to organic materials since in inorganic materials the proton density is usually low enough that even modest MAS rates (e.g.…”

Section: Hardwarementioning

confidence: 99%

“…Although 11 B is a very sensitive nucleus with a relatively high frequency and can readily distinguish BO 3 and BO 4 sites and even inequivalent sites within these groups, 10 B offers an alternative view. It is an I = 3 nucleus and spectra have been observed using a field stepping approach and spectra built up from 'slices' summed together ( Fig.…”

Section: Integer Spinsmentioning

confidence: 99%

Recent technique developments and applications of solid state NMR in characterising inorganic materials

Hanna

Smith

2010

Solid State Nuclear Magnetic Resonance

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A broad overview is given of some key recent developments in solid state NMR techniques that have driven enhanced applications to inorganic materials science. Reference is made to advances in hardware, pulse sequences and associated computational methods (e.g. first principles calculations, spectral simulation), along with their combination to provide more information about solid phases. The resulting methodology has allowed more nuclei to be observed and more structural information to be extracted. Cross referencing between experimental parameters and their calculation from the structure has seen an added dimension to NMR as a characterisation probe of materials. Emphasis is placed on the progress made in the last decade especially from those nuclei that were little studied previously. The general points about technique development and the increased range of nuclei observed are illustrated through a range of specific exemplars from inorganic materials science.

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[2] However, determination of the short-range intermolecular order often remains elusive.

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confidence: 99%

Study of Intermolecular Interactions in the Corrole Matrix by Solid‐State NMR under 100 kHz MAS and Theoretical Calculations

et al. 2013

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Recent progress in solid-state (SS)NMR spectroscopic methods based on fast magic angle spinning (MAS) [1] has enabled new opportunities for the structural study of small quantities (< 5 mg) of natural abundance samples. Utilizing throughspace and through-bond polarization transfer, indirect detection of low-g nuclei, and suitable homo-and heteronuclear decoupling, one-and two-dimensional (1D and 2D) spectra of such samples can be measured with excellent sensitivity and resolution.[2] However, determination of the short-range intermolecular order often remains elusive. Such analyses can be well-served by studying heteronuclear correlations that take advantage of the large chemical shift range of most low-g nuclei (for example, 13 C or 15 N). Indeed, heteronuclear correlation (HETCOR) NMR spectroscopy and measurements of internuclear distances, often in concert with theoretical calculations, have provided structural details of complex hydrogen-bonded systems in chemistry and biology, blended materials, and host-guest pairs.[3] Still, intermolecular polarization transfers to low-g nuclei are often hampered by low sensitivity. A promising solution to this challenge is offered by homonuclear 1 H-1 H 2D correlation methods, such as double-quantum (DQ)MAS [4] or spin-diffusion (NOESYlike) experiments, [5] provided that sufficient resolution is achieved in both dimensions. One of the possible approaches is the use of 1 H CRAMPS decoupling in concert with fast MAS to boost resolution in these experiments.[6] The recent development of ultrafast MAS (at 100 kHz and more [7] ) provides access to appropriate 1 H resolution without RF decoupling.Herein, we report the first application of 1 H 2D SSNMR measurements under MAS at 100 kHz, which are used in combination with indirectly detected 1 H{ 13 C} and 1 H{ 15 N} HETCOR experiments and theoretical calculations to scrutinize the interactions within a host-guest (HG) system consisting of 5,10,15-tris(pentafluorophenyl)corrole 1, and toluene (Scheme 1).Corroles are aromatic macrocycles composed of four pyrrolic rings connected by three meso carbons and bearing one direct pyrrole-pyrrole link. The first synthesis of these materials was a multi-step process with low overall yield.[8] As synthetic methods have improved, there has been increased interest in potential applications of corroles in catalysis, sensors, imaging, and medicinal chemistry.[9] The coordination chemistry of corroles has attracted particular attention, and new metal-corrole systems possessing intriguing properties are being continuously reported.[10] Studies of solid-state structures of corroles and their interactions with other aromatic compounds pose challenges for diffraction and spectroscopic methods. Owing to the difficulties involved in growing X-ray quality crystals of the corroles, which tend to form disordered host(corrole)-guest(solvent) systems, only a few X-ray structures of unsubstituted metal-free corrole have been published to date, including that of corrole 1.[11]Herein, we present the results ...

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New Horizons for Magic-Angle Spinning NMR

Cited by 122 publications

References 3 publications

Sensitivity enhancement in 13C solid-state NMR of protein microcrystals by use of paramagnetic metal ions for optimizing 1H T1 relaxation

Sensitivity enhancement in 13C solid-state NMR of protein microcrystals by use of paramagnetic metal ions for optimizing 1H T1 relaxation

Recent technique developments and applications of solid state NMR in characterising inorganic materials

Study of Intermolecular Interactions in the Corrole Matrix by Solid‐State NMR under 100 kHz MAS and Theoretical Calculations

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