Low-Power High-Resolution Solid-State NMR of Peptides and Proteins

Ernst, Matthias; Meier, Marcel A.; Tuherm, Tiit; Samoson, Ago; Meier, Beat H.

doi:10.1021/ja0494510

Cited by 88 publications

(85 citation statements)

References 19 publications

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“…It operates, however, in a parameter range where the pulses are considerably longer than in TPPM sequences. At very high spinning frequencies, low-power decoupling schemes become possible [24][25][26][27] or the use of rotor-synchronized pulses in the rotor-synchronized Hahn-echo pulse train experiment. 28 Analyzing the efficiency of a decoupling method in solid-state NMR under MAS requires the analysis of all terms contributing to the observed linewidth in the spectrum.…”

Section: Introductionmentioning

confidence: 99%

Understanding two-pulse phase-modulated decoupling in solid-state NMR

Scholz

Hodgkinson

Meier

et al. 2009

The Journal of Chemical Physics

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A theoretical description of the two-pulse phase-modulated (TPPM) decoupling sequence in magic-angle spinning NMR is presented using a triple-mode Floquet approach. The description is formulated in the radio-frequency interaction-frame representation and is valid over the entire range of possible parameters leading to the well-known results of continuous-wave (cw) decoupling and XiX decoupling in the limit of a phase change of 0° and 180°, respectively. The treatment results in analytical expressions for the heteronuclear residual coupling terms and the homonuclear spin-diffusion terms. It also allows the characterization of all resonance conditions that can contribute in a constructive or a destructive way to the residual linewidth. Some of the important resonance conditions are described for the first time since they are not accessible in previous treatments. The combination of the contributions from the residual couplings and the resonance conditions to the effective Hamiltonian, as obtained in a Floquet description, is shown to be required to describe the decoupling behavior over the full range of parameters. It is shown that for typical spin system and experimental parameters a C13 linewidth of approximately 12Hz can be obtained for TPPM decoupling in an organic solid or a protein. This is a major contribution to the experimentally observed linewidths of around 20Hz and indicates that decoupling techniques are still one of the limiting factors in the achievable linewidths.

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Section: Introductionmentioning

confidence: 99%

Understanding two-pulse phase-modulated decoupling in solid-state NMR

Scholz

Hodgkinson

Meier

et al. 2009

The Journal of Chemical Physics

Self Cite

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“…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%

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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“…In recent years, high-speed (35-60 kHz) MAS instrumentation has become available. [7][8][9] However, even at these high spinning rates, fully protonated samples still have homogeneously broadened lines (> 500 Hz).…”

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confidence: 99%