Fast-MAS total through-bond correlation spectroscopy using adiabatic pulses

Hardy, Edme H.; Detken, Andreas; Meier, Beat H.

doi:10.1016/j.jmr.2003.08.003

Cited by 55 publications

(51 citation statements)

References 30 publications

(41 reference statements)

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“…The UC2QF COSY experiment, however, appears to be fairly robust with respect to MAS, and we see no theoretical incompatibility with even higher MAS rates. Recently, Meier [9,10] introduced an adiabatic-pulse version of the TOBSY experiment that also shows excellent correlation spectroscopy at 30 kHz.…”

Section: Resultsmentioning

confidence: 99%

“…Still, scalar couplings are present in the solid state and provide a mechanism for magnetization transfer and correlation spectroscopy. There has recently been significant interest in scalar-coupling-driven correlation in solids as a tool for establishing through-bond connectivity, for facilitating spectral assignment, and as a complementary method to dipolar-driven correlation spectroscopy [1][2][3][4][5][6][7][8][9][10][11][12]. Indeed, scalar coupling-driven correlation in solids complements the more popular dipolardriven methods in two ways.…”

Section: Introductionmentioning

confidence: 99%

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Uniform-sign cross-peak double-quantum-filtered correlation spectroscopy

Mueller

Elliott

Leskowitz

et al. 2004

Journal of Magnetic Resonance

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We detail the uniform-sign cross-peak double-quantum-filtered correlation spectroscopy (UC2QF COSY) experiment, a new through-bond correlation method for disordered solids. This experiment is a refocused version of the popular double-quantumfiltered correlation spectroscopy experiment in liquids. Its key feature is that it provides in-phase and doubly absorptive line shapes, which renders it robust for chemical shift correlation in solids. Both theory and experiment point to distinct advantages of this protocol, which are illustrated by several experiments under challenging conditions, including fast magic-angle spinning (30 kHz), anisotropic molecular motion, and 13 C correlation spectroscopy at the natural abundance isotope level.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Uniform-sign cross-peak double-quantum-filtered correlation spectroscopy

Mueller

Elliott

Leskowitz

et al. 2004

Journal of Magnetic Resonance

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“…The pure J-modulated component s 0 vanishes. The spin-echo modulation is therefore given by Equation (58).…”

Section: Very Fast Masmentioning

confidence: 99%

Principles of Spin‐Echo Modulation by J‐Couplings in Magic‐Angle‐Spinning Solid‐State NMR

et al. 2004

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In magic-angle-spinning solid-state NMR, the homonuclear J-couplings between pairs of spin-1/2 nuclei may be determined by studying the modulation of the spin echo induced by a pi-pulse, as a function of the echo duration. We present the theory of J-induced spin-echo modulation in magic-angle-spinning solids, and derive a set of modulation regimes which apply under different experimental conditions. In most cases, the dominant spin-echo modulation frequency is exactly equal to the J-coupling. Somewhat surprisingly, the chemical shift anisotropies and dipole-dipole couplings tend to stabilise--rather than abscure--the J-modulation. The theoretical conclusions are supported by numerical simulations and experimental results obtained for three representative samples containing 13C spin pairs.

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“…Recent advances in solid-state NMR [5], based on symmetry principles and average Hamiltonian theory (AHT), allow the design of pulse sequences that cancel the 1st order average Hamiltonian and minimize the higher orders contributions from CSA, D and offset terms, maintaining only the isotropic J-coupling. These sequences, known as TOBSY (TOtal through Bond correlation SpectroscopY), were originally developed for 13 C spectroscopy [6,7] and have been demonstrated in immobilized systems [6][7][8][9], or more recently were successfully used to study dynamics and structure of membrane proteins [10] in lipid bilayers or protein fibrils [11]. A few HRMAS 1 H NMR studies on polymers and other organic compounds [12,13] have used TOBSY sequences, albeit without the use of adiabatic pulses and their superior performance.…”

Section: Introductionmentioning

confidence: 99%