Dipolar recoupling in fast-MAS solid-state NMR spectroscopy

Schnell, Ingo

doi:10.1016/j.pnmrs.2004.06.003

Cited by 124 publications

(45 citation statements)

References 145 publications

(286 reference statements)

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“…One is that the homonuclear interaction is greatly reduced by the sample rotation. This can be understood if we consider the part of the spin Hamiltonian that describes the spin physics of the I = 1/2 nuclei: (6) where δ Fig. 1) do not modify the homonuclear term in the interaction representation of the RF, this term is not "recoupled" by the pulses, so that to first order the homonuclear interaction is reduced to its vanishing average under MAS.…”

Section: Theoretical Backgroundmentioning

confidence: 99%

“…5 Therefore, development of NMR methods that recouple the dipolar interaction yet retain the high resolution under MAS conditions, has become an active area of research. 3,[5][6][7][8][9][10] The recoupling is often achieved by the application of rotor synchronized RF pulses. 5 Over the past eighteen years a variety of recoupling sequences under MAS have been developed to recover the dipolar couplings in isolated spin pairs.…”

Section: Introductionmentioning

confidence: 99%

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Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

et al. 2007

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We report the first results establishing REAPDOR experiments for distance measurements between a spin-1/2 ( 31 P) and spin-7/2 ( 51 V) pair in a series of vanadium-substituted polyoxoanionic solids from the Keggin and Wells-Dawson families. We have quantitatively measured 31 P-51 V distances in mono-vanadium substituted K 4 PVW 11 O 40 , 1-K 7 P 2 VW 17 O 62 , and 4-K 7 P 2 VW 17 O 62 . Numerical simulations of the experimental data yield very good agreement with the averaged P-W/P-V distances determined from the X-ray diffraction measurements in the same or related compounds. REAPDOR is therefore a very sensitive P-V distance probe anticipated to be especially useful in the absence of long-range order. Our results suggest that REAPDOR spectroscopy could be broadly applicable for interatomic distance measurements in other spin-7/2-spin-1/2 nuclear pairs.

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Section: Theoretical Backgroundmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

et al. 2007

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“…. ½ : [10] This is reasonable since both r.f. frequencies are in the MHz regime so that even several integer multiples of the r.f.…”

Section: Average Hamiltonian In the Rotating Framementioning

confidence: 90%

“…Although CP encompasses a very large family of experiments such as those noted above, it is also a member of a ''super family'' of experiments that perform dipolar recoupling among spins (9)(10)(11).…”

Section: Introductionmentioning

confidence: 99%

Tutorial on analytic theory for cross‐polarization in solid state NMR

Rovnyak

2008

Concepts Magnetic Resonance

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This tutorial aims to be a self-contained and explicit analysis of the basic cross polarization (CP) solid-state NMR experiment (SSNMR) in the isolated spin-pair approximation using standard quantum mechanical arguments. The general result of obtaining coherence transfer between two dipolar coupled spin-active nuclei while applying radio frequency fields to both nuclei is described, with emphasis on the origin of the well known Hartmann-Hahn matching conditions. No new theory is presented; rather several common analytical methods in SSNMR are demonstrated in the context of cross-polarization under static and magic-angle spinning (MAS) conditions. A background in NMR and quantum mechanics is assumed, however this work attempts to minimize the need for excursions into the literature. This article was written to aid a reader in advancing into more detailed descriptions of CP and dipolar recoupling in general.

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“…Several NMR techniques have been developed to recouple the dipolar interactions under MAS (19,20). In most of the numerous recent applications, molecular dynamics is considered as a complication to be avoided.…”

Section: Introductionmentioning

confidence: 99%

A simple analytical model to describe dynamic magic‐angle spinning experiments

Hirschinger

2006

Concepts Magnetic Resonance

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A simple analytical method based on the memory-function approach and the Anderson-Weiss theory is presented for studying in a uniform way the spin dynamics in several NMR experiments performed under the conditions of magic-angle spinning (MAS). A series of 1 H MAS spectra of adamantane serve as an example for a sample with homogeneous line broadening. A good agreement between experimental and calculated integral spinning sideband intensities for a spinning frequency ranging from 5 to 33 kHz is obtained using a sixth-order approximation of the theory. Moreover, this model, which is able to describe the NMR spectra in the presence of a rotationally diffusive isotropic and anisotropic Gaussian-Markoff process, allows the treatment of the combined effects of sample spinning and molecular motion. Finally, the application of MAS recoupling methods in the intermediate motional regime is examined by using the concept of refocusing pulses. It is shown that recoupling experiments such as rotational-echo double-resonance (REDOR) can still be applied in the presence of anisotropic molecular motion.

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Dipolar recoupling in fast-MAS solid-state NMR spectroscopy

Cited by 124 publications

References 145 publications

Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

Tutorial on analytic theory for cross‐polarization in solid state NMR

A simple analytical model to describe dynamic magic‐angle spinning experiments

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Dipolar recoupling in fast-MAS solid-state NMR spectroscopy

Cited by 124 publications

References 145 publications

Internuclear 31P−51V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

Internuclear 31P−51V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

Tutorial on analytic theory for cross‐polarization in solid state NMR

A simple analytical model to describe dynamic magic‐angle spinning experiments

Contact Info

Product

Resources

About

Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy

Internuclear ³¹P−⁵¹V Distance Measurements in Polyoxoanionic Solids Using Rotational Echo Adiabatic Passage Double Resonance NMR Spectroscopy