Nuclear cross-relaxation induced by specimen rotation

Andrew, E.R.; Bradbury, A.; Eades, R. G.; Wynn, V. T.

doi:10.1016/0031-9163(63)90123-9

Cited by 145 publications

(74 citation statements)

References 5 publications

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“…If the spinning speed exceeds the chemical shift anisotropy only the highly resolved central band remains (Fig. 6A) (48). If the spinning speed is less than the chemical shift anisotropy the spectrum comprises several sidebands (Figs.…”

Section: Magic Angle Spinning Nmr Spectroscopy Of Oriented Bilayer Samentioning

confidence: 99%

Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Bechinger

Sizun

2003

Concepts Magnetic Resonance

111

148

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ABSTRACT:In contrast to solution NMR spectroscopy, where complete or almost complete averaging leads to isotropic values, the anisotropic character of nuclear interactions is apparent in solid-state NMR spectra. The orientation dependence of chemical shift and dipolar or quadrupolar interactions has been used to obtain dynamic as well as angular information from polypeptides that strongly interact with phospholipid bilayers. This article illustrates the advantageous characteristics of the anisotropic 15 N or 31 P chemical shift interactions that in a direct manner allow one to obtain information on the alignment of helical polypeptides or of phospholipid head groups with respect to the membrane normal.

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Section: Magic Angle Spinning Nmr Spectroscopy Of Oriented Bilayer Samentioning

confidence: 99%

Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Bechinger

Sizun

2003

Concepts Magnetic Resonance

111

148

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“…For example, Brouwer and Ripmeester [12] designed a recoupling sequence using symmetry principles [13,14], while Duma et al [15] used rotary resonance [16][17][18] to reintroduce the 1 H CSA. In common with all methods based on rotary resonance, the latter suffers from substantial sensitivity to rf inhomogeneity, while the sequence symmetry chosen in the former restricts the experiment to relatively slow MAS rates.…”

Section: Introductionmentioning

confidence: 99%

Measuring proton shift tensors with ultrafast MAS NMR

Miah

Bennett

Iuga

et al. 2013

Journal of Magnetic Resonance

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A new proton anisotropic-isotropic shift correlation experiment is described which operates with ultrafast MAS, resulting in good resolution of isotropic proton shifts in the detection dimension. The new experiment makes use of a recoupling sequence designed using symmetry principles which reintroduces the proton chemical shift anisotropy in the indirect dimension. The experiment has been used to measure the proton shift tensor parameters for the OH hydrogen-bonded protons in tyrosine.HCl and citric acid at Larmor frequencies of up to 850 MHz.

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“…This condition is summarized in the RR equation 14,15 When the RR condition is satisfied, the homonuclear dipolar interaction is reintroduced, and a pronounced broadening or splitting of the usual MAS peaks is observed. [14][15][16] Additionally, a rapid oscillatory exchange of Zeeman magnetization occurs between the two spins. Usually, it is the profile of this exchange as a function of time that is simulated to extract R DD .…”

Section: Introductionmentioning

confidence: 99%

Dipolar-Chemical Shift and Rotational Resonance¹³C NMR Studies of the Carboxyl−Methylene Carbon Spin Pair in Solid Phenylacetic Acid and Potassium Hydrogen Bisphenylacetate

Bryce

Wasylishen

2000

J. Phys. Chem. A

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The dipolar-chemical shift (CS) method has been applied to analyze the carboxyl-methylene carbon isolated spin pair in phenylacetic-13 C 2 acid and potassium hydrogen bisphenylacetate-13 C 2 . The span, Ω, of the CS tensor is decreased significantly for both carbon atoms in the potassium acid salt compared to the acid. The orientations of the carboxyl CS tensor and, more notably, the methylene CS tensor, have a marked dependence on the protonation state of the carboxyl group. Ab initio calculations [RHF/6-311G*, RHF/6-311++G(2d,-2p)] support the experimental findings. In addition to these studies, we demonstrate how rotational resonance (RR) NMR spectroscopy complements the dipolar-CS method in a study of the isolated 13 C spin pairs in phenylacetic-13 C 2 acid. In particular, the higher-order RR experiments provide a stringent check on the CS parameters and the dipolar coupling constant, R, derived from the dipolar-CS analysis. The dipolar-CS method, in combination with a two-dimensional spin-echo experiment, yields R ) 2150 ( 30 Hz for phenylacetic acid, whereas RR indicates that R ) 2100 ( 15 Hz. Although n ) 1 RR can be applied reliably to determine internuclear distances in the absence of CS tensor data, these data are critical for simulations of the n ) 2 RR effects. Specifically, longitudinal magnetization exchange curves are shown to be sensitive to slight rotations of the carboxyl carbon CS tensor about an axis perpendicular to the carboxyl plane, a phenomenon observed upon moving from the acid to the acid salt. Simulations indicate that altering the MAS rate by only a few tens of hertz can drastically alter the higher-order RR line shapes. The ab initio calculations of chemical shielding tensors provide data that are useful in the simulation of rotational resonance effects. We propose phenylacetic-13 C 2 acid as a setup sample for rotational resonance and other homonuclear dipolar recoupling experiments. IntroductionThe dipolar-chemical shift (CS) method is an effective NMR technique for studying isolated spin-1 / 2 pairs in stationary powdered solids. [1][2][3][4][5][6] Under favorable circumstances, when symmetry dictates the orientation of at least one component of one of the CS tensors, this method will yield the direct dipolar coupling constant (R DD ), the magnitudes of the principal components of the two CS tensors, the relative orientations of the CS tensors, and the orientations of these tensors with respect to the molecular axis system. 6 The fact that this orientational information is derived from a powdered sample makes the method particularly valuable when single crystals are not available. R DD is of interest because of its simple relationship with the distance, r 12 , between nucleus 1 and nucleus 2 (eq 1) where µ 0 is the permeability of free space and γ 1 and γ 2 are the magnetogyric ratios of the nuclei under consideration. It is important to recognize that r 12 is a motionally averaged distance. Complications in measuring very accurate values of r 12 using solid-state NMR will be di...

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Nuclear cross-relaxation induced by specimen rotation

Cited by 145 publications

References 5 publications

Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Measuring proton shift tensors with ultrafast MAS NMR

Dipolar-Chemical Shift and Rotational Resonance¹³C NMR Studies of the Carboxyl−Methylene Carbon Spin Pair in Solid Phenylacetic Acid and Potassium Hydrogen Bisphenylacetate

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Nuclear cross-relaxation induced by specimen rotation

Cited by 145 publications

References 5 publications

Alignment and structural analysis of membrane polypeptides by 15N and 31P solid‐state NMR spectroscopy

Alignment and structural analysis of membrane polypeptides by 15N and 31P solid‐state NMR spectroscopy

Measuring proton shift tensors with ultrafast MAS NMR

Dipolar-Chemical Shift and Rotational Resonance13C NMR Studies of the Carboxyl−Methylene Carbon Spin Pair in Solid Phenylacetic Acid and Potassium Hydrogen Bisphenylacetate

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Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Alignment and structural analysis of membrane polypeptides by ¹⁵N and ³¹P solid‐state NMR spectroscopy

Dipolar-Chemical Shift and Rotational Resonance¹³C NMR Studies of the Carboxyl−Methylene Carbon Spin Pair in Solid Phenylacetic Acid and Potassium Hydrogen Bisphenylacetate