Windowless dipolar recoupling: the detection of weak dipolar couplings between spin 12 nuclei with large chemical shift anisotropies

Gregory, David; Mitchell, Dan J.; Stringer, John A.; Kiihne, Suzanne; Shiels, Jerome C.; Callahan, John J.; Mehta, Manish; Drobny, Gary P.

doi:10.1016/0009-2614(95)01166-3

Cited by 149 publications

(150 citation statements)

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“…The three dipolar recoupling pulse sequences that will be discussed in the context of structural studies of proteins adsorbed at biomaterial interfaces are the heteronuclear recoupling experiment REDOR (Rotational Echo Double Resonance) [31], and the homonuclear recoupling experiments DRAWS (Dipolar Recoupling with a Windowless Sequence) [32] and SEDRA (Simple Excitation for Dephasing of Rotational-echo Amplitudes) [33,34]. REDOR, developed by Schaefer and coworkers is commonly used to measure the distance between heteroatoms [35].…”

Section: Nmr Methods For the Study Of Protein Structure At Biomateriamentioning

confidence: 99%

Solid state NMR studies of molecular recognition at protein–mineral interfaces

Goobes

Stayton

Drobny

2007

Progress in Nuclear Magnetic Resonance Spectroscopy

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Section: Nmr Methods For the Study Of Protein Structure At Biomateriamentioning

confidence: 99%

Solid state NMR studies of molecular recognition at protein–mineral interfaces

Goobes

Stayton

Drobny

2007

Progress in Nuclear Magnetic Resonance Spectroscopy

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“…The Hamiltonian is often truncated after the first, zeroth-order term, although higher order terms may be included for more accurate results. For DRAWS, the zeroth-order average dipolar Hamiltonian has been calculated as 7 In this expression, d ij is the static dipolar coupling between the two resonances, and the coefficients c xx-yy and c zz depend only on the Euler angles orienting the dipolar tensor in the rotor frame. 9 For RFDR, the zeroth-order average Hamiltonian expression for the dipolar Hamiltonian has been calculated as in which the coefficient, d h ij , depends on the static dipolar coupling, the dipolar angles, the rotor speed, and the isotropic chemical shift difference between the two resonances.…”

Section: Cpmas Datamentioning

confidence: 99%

“…[1][2][3][4][5][6][7] Multidimensional dipolar recoupling NMR techniques, developed by extension of existing onedimensional experiments into two or more dimensions, 3,6,[8][9][10] make possible the simultaneous measurement of many distances in uniformly isotopically labeled samples. Simulations have shown that multidimensional dipolar recoupling experiments may have sufficient resolution to allow the assignment of relatively large spin systems.…”

Section: Introductionmentioning

confidence: 99%

“…To compare pulse sequence effects, cross-peak buildup curves are obtained with two dipolar recoupling methods: dipolar recoupling with a windowless sequence (DRAWS) 7 and radio frequency driven dipolar recoupling (RFDR). 2 These two techniques have different coherence transfer mechanisms, which lead to significantly different results in two-dimensional experiments.…”

Section: Introductionmentioning

confidence: 99%

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Distance Measurements in Multiply Labeled Crystalline Cytidines by Dipolar Recoupling Solid State NMR

et al. 1999

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To systematically explore the effects of spin system size and geometry on the precision and accuracy of two-dimensional solid state NMR distance measurements, we have applied two homonuclear dipolar recoupling experiments, 2D DRAWS and 2D RFDR, to five polycrystalline samples of uniformly or selectively 13 Clabeled cytidine. Distance information has been obtained from the intensities and time behavior of crosspeaks observed in the resulting two-dimensional spectra. The experimental cross-peak buildup curves obtained from these crystalline cytidine samples have been analyzed by comparison with simulations. In uniformly 13 C-labeled cytidine, indirect coherence transfer mechanisms lead to low-precision distance measurements not unlike those measured in solution state NOESY experiments. In the selectively labeled cytidines, the distance measurements are considerably more precise, allowing the possibility of very accurate structure determinations from selectively or randomly labeled spin systems. Of the two techniques, the 2D DRAWS method allows identification of indirect coherence transfer mechanisms that hinder accurate distance measurement.

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“…1 In particular, a large number of heteronuclear and homonuclear recoupling pulse sequences are now available and applicable to a variety of experimental conditions. [2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][21] Most of the recoupling sequences generate in a zeroth-order approximation an effective dipolar-coupling Hamiltonian that contains zeroquantum ͑ZQ͒ or double-quantum ͑DQ͒ two-spin operators. In this publication we focus primarily on zeroth-order sequences.…”

Section: Introductionmentioning

confidence: 99%

Dipolar truncation in magic-angle spinning NMR recoupling experiments

Bayro¹,

Huber²,

Ramachandran³

et al. 2009

The Journal of Chemical Physics

169

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Quantitative solid-state NMR distance measurements in strongly coupled spin systems are often complicated due to the simultaneous presence of multiple noncommuting spin interactions. In the case of zeroth-order homonuclear dipolar recoupling experiments, the recoupled dipolar interaction between distant spins is attenuated by the presence of stronger couplings to nearby spins, an effect known as dipolar truncation. In this article, we quantitatively investigate the effect of dipolar truncation on the polarization-transfer efficiency of various homonuclear recoupling experiments with analytical theory, numerical simulations, and experiments. In particular, using selectively 13 C-labeled tripeptides, we compare the extent of dipolar truncation in model three-spin systems encountered in protein samples produced with uniform and alternating labeling. Our observations indicate that while the extent of dipolar truncation decreases in the absence of directly bonded nuclei, two-bond dipolar couplings can generate significant dipolar truncation of small, long-range couplings. Therefore, while alternating labeling alleviates the effects of dipolar truncation, and thus facilitates the application of recoupling experiments to large spin systems, it does not represent a complete solution to this outstanding problem.

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Windowless dipolar recoupling: the detection of weak dipolar couplings between spin 12 nuclei with large chemical shift anisotropies

Cited by 149 publications

References 30 publications

Solid state NMR studies of molecular recognition at protein–mineral interfaces

Solid state NMR studies of molecular recognition at protein–mineral interfaces

Distance Measurements in Multiply Labeled Crystalline Cytidines by Dipolar Recoupling Solid State NMR

Dipolar truncation in magic-angle spinning NMR recoupling experiments

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