NMR Studies of Dynamic Processes in Organic Solids

Reichert, Detlef

doi:10.1016/s0066-4103(04)55003-2

Cited by 38 publications

(18 citation statements)

References 616 publications

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“…Notably, several early studies demonstrated that motions of organic compounds on a time scale similar to that of the pulse nutation frequency reduces the efficiency of pulse decoupling [33–36]. Currently, the pulse nutation frequency in most OS solid-state NMR experiments is similar to the rotational diffusion frequency of membrane proteins at approximately 10 5 Hz [37], and therefore interference effects may be present.…”

Section: Discussionmentioning

confidence: 99%

Improved 1H amide resonance line narrowing in oriented sample solid-state NMR of membrane proteins in phospholipid bilayers

Park

Opella

2012

Journal of Magnetic Resonance

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We demonstrate 1H amide resonance line widths <300 Hz in 1H/15N heteronuclear correlation (HETCOR) spectra of membrane proteins in aligned phospholipid bilayers. This represents a substantial improvement over typically observed line widths of ~1 kHz. Furthermore, in a proton detected local field (PDLF) version of the experiment that measures heteronuclear dipolar couplings, line widths <130 Hz are observed. This dramatic line narrowing of 1H amide resonances enables many more individual signals to be resolved and assigned from uniformly 15N labeled membrane proteins in phospholipid bilayers under physiological conditions of temperature and pH. Finding that the decrease in line widths occurs only for membrane proteins that undergo fast rotational diffusion around the bilayer normal, but not immobile molecules, such as peptide single crystals, identifies a potential new direction for pulse sequence development that includes overall molecular dynamics in their design.

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Section: Discussionmentioning

confidence: 99%

Improved 1H amide resonance line narrowing in oriented sample solid-state NMR of membrane proteins in phospholipid bilayers

Park

Opella

2012

Journal of Magnetic Resonance

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“…By slowing down the dynamic process by decreasing the temperature, one can reach the so-called intermediate-motion regime, at which the time constant of the dynamic process is similar to the inverse coupling constant of the anisotropic interaction. 12 This scenario, which is mathematically very similar to the treatment of exchange NMR experiments, 13 is well known in liquid-state NMR where the exchange of different isotropic frequencies leads to a loss of phase coherence and to a broadening of the spectra. The same approach is applicable for static solid-state spectra, where the exchange occurs between different anisotropic frequencies, i.e., between nuclei belonging to molecules with different orientations with respect to the external magnetic field.…”

Section: Introductionmentioning

confidence: 87%

Intermediate motions as studied by solid-state separated local field NMR experiments

deAzevedo

Saalwächter

Pascui

et al. 2008

The Journal of Chemical Physics

126

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Second-order dipolar order in magic-angle spinning nuclear magnetic resonance J. Chem. Phys. 135, 154507 (2011) Single crystal nuclear magnetic resonance in spinning powders J. Chem. Phys. 135, 144201 (2011) Resistive detection of optically pumped nuclear polarization with spin phase transition peak at Landau level filling factor 2/3 Appl. Phys. Lett. 99, 112106 (2011) High-resolution 13C nuclear magnetic resonance evidence of phase transition of Rb,Cs-intercalated singlewalled nanotubes J. Appl. Phys. 110, 054306 (2011) Introduction of the Floquet-Magnus expansion in solid-state nuclear magnetic resonance spectroscopy J. Chem. Phys. 135, 044109 (2011) Additional information on J. Chem. Phys. In this report, the application of a class of separated local field NMR experiments named dipolar chemical shift correlation ͑DIPSHIFT͒ for probing motions in the intermediate regime is discussed. Simple analytical procedures based on the Anderson-Weiss ͑AW͒ approximation are presented. In order to establish limits of validity of the AW based formulas, a comparison with spin dynamics simulations based on the solution of the stochastic Liouville-von-Neumann equation is presented. It is shown that at short evolution times ͑less than 30% of the rotor period͒, the AW based formulas are suitable for fitting the DIPSHIFT curves and extracting kinetic parameters even in the case of jumplike motions. However, full spin dynamics simulations provide a more reliable treatment and extend the frequency range of the molecular motions accessible by DIPSHIFT experiments. As an experimental test, molecular jumps of imidazol methyl sulfonate and trimethylsulfoxonium iodide, as well as the side-chain motions in the photoluminescent polymer poly͓2-methoxy-5-͑2Ј-ethylhexyloxy͒-1,4-phenylenevinylene͔, were characterized. Possible extensions are also discussed.

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“…In this regard, we have investigated the dynamic properties of the phenyl rings in TPM via solidstate 2 H NMR studies of the deuterated material (C 6 D 5 ) 3 COH (TPM-d 15 ). Solid-state 2 H NMR spectroscopy is a powerful technique for investigating molecular motion in solids [4][5][6][7][8][9][10][11][12]. When the rate of motion is in the range 10 3 -10 8 s À1 (the intermediate motion regime), analysis of the 2 H NMR lineshape provides detailed information on the rate, geometry and mechanism of the motion.…”

mentioning

confidence: 99%

Solid triphenylmethanol: A molecular material that undergoes multiple internal reorientational processes on different timescales

Kitchin

Serrano-González

et al. 2006

Journal of Solid State Chemistry

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NMR Studies of Dynamic Processes in Organic Solids

Cited by 38 publications

References 616 publications

Improved 1H amide resonance line narrowing in oriented sample solid-state NMR of membrane proteins in phospholipid bilayers

Improved 1H amide resonance line narrowing in oriented sample solid-state NMR of membrane proteins in phospholipid bilayers

Intermediate motions as studied by solid-state separated local field NMR experiments

Solid triphenylmethanol: A molecular material that undergoes multiple internal reorientational processes on different timescales

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