Measurement of Heteronuclear Dipolar Coupling by Transferred-Echo Double-Resonance NMR

Hing, Andrew W.; Vega, Shimon; Schaefer, Jacob

doi:10.1006/jmra.1993.1146

Cited by 120 publications

(114 citation statements)

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“…Heteronuclear recoupling could also be done using simultaneous frequency and amplitude modulation (SFAM), which appears to be more robust than RE-DOR with respect to RF inhomogeneity and resonance offsets [43,44]. Transferred-echo double-resonance (TE-DOR) is another filtering method which has been applied to amino acids, peptides, and proteins with directly bonded 13 C-15 N pairs [45,46]. Reported TEDOR efficiencies are between 0.05 and 0.35 [46][47][48][49][50][51].…”

Section: Comparison With Other Filtering Methodsmentioning

confidence: 99%

“…Transferred-echo double-resonance (TE-DOR) is another filtering method which has been applied to amino acids, peptides, and proteins with directly bonded 13 C-15 N pairs [45,46]. Reported TEDOR efficiencies are between 0.05 and 0.35 [46][47][48][49][50][51]. Finally, filtering with 15 N-13 C cross-polarization between directly bonded pairs has been used for amino acids, peptides, and proteins and the reported efficiencies are between 0.40 and 0.70 [50][51][52][53][54][55][56].…”

Section: Comparison With Other Filtering Methodsmentioning

confidence: 99%

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Application of REDOR subtraction for filtered MAS observation of labeled backbone carbons of membrane-bound fusion peptides

Yang

Parkanzky

Bodner

et al. 2002

Journal of Magnetic Resonance

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Clean MAS observation of 13 C-labeled carbons in membrane-bound HIV-1 and influenza fusion peptides was made by using a rotational-echo double-resonance spectroscopy (REDOR) filter of directly bonded 13 C-15 N pairs. The clean filtering achieved with the REDOR approach is superior to filtering done with sample difference spectroscopy. In one labeling approach, the peptide had labels at a single 13 C carbonyl and its directly bonded 15 N. The resulting chemical shift distribution of the filtered signal is used to assess the distribution of local secondary structures at the labeled carbonyl. For the influenza peptide, the Leu-2 carbonyl chemical shift distribution is shown to vary markedly with lipid and detergent composition, as well as peptide:lipid ratio, suggesting that the local peptide structure also has a strong dependence on these factors. Because most carboxylic-and amino-labeled amino acids are commercially available, this REDOR approach should have broad applicability to chemically synthesized peptides as well as bacterially synthesized proteins. In a second labeling approach, the HIV-1 fusion peptide had U-13 C, 15 N labeling over three sequential residues. When a 1.6 ms REDOR dephasing time is used, only backbone 13 C signals are observed. The resulting spectra are used to determine spectral linewidths and to assess feasibility of assignment of uniformly labeled peptide.

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Section: Comparison With Other Filtering Methodsmentioning

confidence: 99%

Section: Comparison With Other Filtering Methodsmentioning

confidence: 99%

Application of REDOR subtraction for filtered MAS observation of labeled backbone carbons of membrane-bound fusion peptides

Yang

Parkanzky

Bodner

et al. 2002

Journal of Magnetic Resonance

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“…Obviously several alternatives exists, among which belong the Transfered-Echo-DoubleResonance (TEDOR) experiment [64,65] which here serves as another example illustrating the straightforward consideration of finite rf pulse irradiation in complex echotrain experiments in combination with extended reuse of propagators in two dipolar dephasing periods. The attractive feature of TEDOR as compared to REDOR is the elimination of background signals due to uncoupled spins.…”

Section: Typical Examples Of Simpson Simulationsmentioning

confidence: 99%

SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy

Bak

Rasmussen

Nielsen

2000

Journal of Magnetic Resonance

1,623

1,540

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“…[39]. The TEDOR pulse sequence is useful for transferring polarization from one type of nucleus to another type via relatively weak dipolar couplings [43,44]. The two-dimensional version, which has been developed and applied to polarization transfer from quadrupolar nuclei to spin-1/2 nuclei [45][46][47][48][49], yields a 2D spectrum showing correlated signal intensity from spatially-proximate nuclear spin pairs that are dipole-dipole coupled.…”

Section: Oretical Line From Eq(3) Similar Distributions Ofmentioning

confidence: 99%

Spatially correlated distributions of local metallic properties in bulk and nanocrystalline GaN

et al. 2017

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We compare local electronic structure at different atom types of a metallic semiconductor in bulk and nanocrystalline form. Multinuclear magic-angle-spinning nuclear magnetic resonance (MAS NMR) establishes that GaN synthesized as an intentionally-doped bulk powder or as annealed nanocrystalline particles exhibits metallic behavior and a wide distribution of differing electronic environments in both forms. Bulk polycrystalline wurtzite GaN doped with 0.13% Ge as a shallow donor exhibits a temperature-independent distribution of 71 Ga Knight shifts over the temperature range 123-473 K. Each Knight shift frequency in the inhomogeneously-broadened spectrum is characterized by a 71 Ga spin-lattice relaxation time T 1 that is in good agreement with the value predicted by the Knight-Korringa relation across the broad range of temperatures. The14 N spectrum shows a slightly smaller Knight shift distribution with spin-lattice relaxation time T 1 values at 295 K across the distribution also in good agreement with the Knight-Korringa relation. Similarly, annealed nanocrystalline wurtzite GaN (50-100 nm, and without Ge) exhibits a 71 Ga Knight shift distribution and T 1values (at 295 K) that follow the same Knight-Korringa behavior. Thus, both bulk and nanocrystalline forms of GaN are n-type and well above the metal-insulator transition (MIT), the nanocrystals most likely as a result of incorporation of shallow donor oxygen atoms during synthesis. Carriers in both forms of sample exhibit the near-ideal characteristics of a degenerate Fermi gas of non-interacting spins. The observation of NMR signals from both atom types, Ga and N, allows for the direct spatial correlation of the local electronic structure at the two sites in the lattice, specifically the s-orbital character of the electronic wavefunction of conduction band electrons at the Fermi edge. The relative values of these carrier wavefunction probabilities (nearly twice as great for the N atom as for the Ga) are in line with theoretical predictions. Analyses of 71 Ga, 14 N, and 15 N NMR results, including double-resonance 2D 15 N{ 71 Ga} measurements, reveal electronic disorder in the form of broad distributions of local metallic properties (Knight shifts) that are shown to be spatially correlated on a sub-nanometer scale.

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Measurement of Heteronuclear Dipolar Coupling by Transferred-Echo Double-Resonance NMR

Cited by 120 publications

References 0 publications

Application of REDOR subtraction for filtered MAS observation of labeled backbone carbons of membrane-bound fusion peptides

Application of REDOR subtraction for filtered MAS observation of labeled backbone carbons of membrane-bound fusion peptides

SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy

Spatially correlated distributions of local metallic properties in bulk and nanocrystalline GaN

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