@article {345, title = {Using switched angle spinning to simplify NMR spectra of strongly oriented samples}, journal = {Journal of the American Chemical Society}, volume = {125}, year = {2003}, note = {J Am Chem Soc695CXTimes Cited:13Cited References Count:38}, month = {Jul 2}, pages = {7998-8006}, abstract = {

This contribution describes a method that manipulates the alignment director of a liquid crystalline sample to obtain anisotropic magnetic interaction parameters, such as dipolar coupling, in an oriented liquid crystalline sample. By changing the axis of rotation with respect to the applied magnetic field in a spinning liquid crystalline sample, the dipolar couplings present in a normally complex strong coupling spectrum are scaled to a simple weak coupling spectrum. This simplified weak coupling spectrum is then correlated with the isotropic chemical shift in a switched angle spinning (SAS) two-dimensional (2D) experiment. This dipolar-isotropic 2D correlation was also observed for the case where the couplings are scaled to a degree where the spectrum approaches strong coupling. The SAS 2D correlation of C6F5Cl in the nematic liquid crystal I52 was obtained by first evolving at an angle close to the magic angle (54.7degrees) and then directly detecting at the magic angle. The SAS method provides a 2D correlation where the weak coupling pairs are revealed as cross-peaks in the indirect dimension separated by the isotropic chemical shifts in the direct dimension. Additionally, by using a more complex SAS method which involves three changes of the spinning axis, the solidlike spinning sideband patterns were correlated with the isotropic chemical shifts in a 2D experiment. These techniques are expected to enhance the interpretation and assignment of an isotropic. magnetic interactions including dipolar couplings for molecules dissolved in oriented liquid crystalline phases.

}, keywords = {solids}, isbn = {0002-7863}, doi = {Doi 10.1021/Ja0342244}, url = {://WOS:000183814500059}, author = {Havlin, R. H. and Park, G. H. J. and Mazur, T. and Pines, A.} } @article {350, title = {Theoretical studies of the spin dynamics of quadrupolar nuclei at rotational resonance conditions}, journal = {Journal of Chemical Physics}, volume = {116}, year = {2002}, note = {J Chem Phys503ECTimes Cited:12Cited References Count:20}, month = {Jan 1}, pages = {79-90}, abstract = {

A theory of the spin dynamics of I=3/2 quadrupolar nuclei in the sudden-passage limit is discussed in relation to the recently observed rotational resonance (RR) effects on the excitation and conversion of triple-quantum coherence in the FASTER multiple-quantum magic-angle spinning (MQMAS) experiments [T. Vosegaard, P. Florian, D. Massiot, and P. J. Grandinetti, J. Chem. Phys. 114, 4618 (2001)]. A novel interaction frame, which combines the quadrupolar interaction with the central transition radio frequency irradiation, is shown to be useful in understanding the complex spin dynamics at and away from RR conditions. Analytical expressions for the Hamiltonian obtained from bimodal Floquet theory are included in order to provide insight into the spin dynamics observed in the FASTER MQMAS experiments. Numerical simulations have been performed and were found to support the theoretical formalism. (C) 2002 American Institute of Physics.

}, keywords = {solids}, isbn = {0021-9606}, doi = {Doi 10.1063/1.1421613}, url = {://WOS:000172784700010}, author = {Walls, J. D. and Lim, K. H. and Pines, A.} } @article {391, title = {Scalar and anisotropic J interactions in undoped InP: A triple-resonance NMR study}, journal = {Physical Review B}, volume = {58}, year = {1998}, note = {Phys Rev B125HUTimes Cited:29Cited References Count:40}, month = {Oct 1}, pages = {8627-8633}, abstract = {

The heteronuclear J-coupling tensor between nearest neighbor P-31 and In-113 spins in undoped InP is investigated by means of In-113--\>P-31 polarization transfer under rapid magic angle spinning (MAS). The scalar contribution can be measured directly and is found to have the value \J(iso)(P-31-In-113,In-115)\ = (225+/-10) Hz. The principal value of the traceless anisotropic J-coupling tensor (pseudodipolar coupling) is determined to be J(aniso)(P-31-In-113,In-115)= 2/3[J(parallel to)(P-31-In-113,In-115)-J(perpendicular to)(P-31-In-113,In-115)] = (813+/-50) or (1733+/-50) Hz, assuming axial symmetry with the principal axis parallel to the In-P bond. Our values deviate from those reported previously [M. Engelsberg and R. E. Norberg, Phys. Rev. B 5, 3395 (1972)] [based on a moment analysis of the P-31 resonance \J(iso)(31P-In-113,In-115)\ = 350 Hz and J(aniso)(P-31-In-113,In-115) = 1273 Hz], but confirm the postulate that the nearest neighbor P-31-In-113,In-115 magnetic dipolar and pseudodipolar interactions are of the same order of magnitude and partially cancel each other.

}, keywords = {solids}, isbn = {0163-1829}, doi = {Doi 10.1103/Physrevb.58.8627}, url = {://WOS:000076232100075}, author = {Tomaselli, M. and deGraw, D. and Yarger, J. L. and Augustine, M. P. and Pines, A.} } @article {409, title = {Selective enhancement of NMR signals for alpha-cyclodextrin with laser-polarized xenon}, journal = {Angewandte Chemie-International Edition in English}, volume = {36}, year = {1997}, note = {Angew Chem Int EditYh944Times Cited:48Cited References Count:29}, month = {Nov 14}, pages = {2368-2370}, keywords = {solids}, isbn = {0570-0833}, doi = {Doi 10.1002/Anie.199723681}, url = {://WOS:A1997YH94400025}, author = {Song, Y. Q. and Goodson, B. M. and Taylor, R. E. and Laws, D. D. and Navon, G. and Pines, A.} } @article {419, title = {Surface-enhanced NMR using continuous-flow laser-polarized xenon}, journal = {Journal of the American Chemical Society}, volume = {119}, year = {1997}, note = {J Am Chem SocYk502Times Cited:66Cited References Count:16}, month = {Dec 3}, pages = {11711-11712}, keywords = {solids}, isbn = {0002-7863}, doi = {Doi 10.1021/Ja9713587}, url = {://WOS:A1997YK50200029}, author = {Haake, M. and Pines, A. and Reimer, J. A. and Seydoux, R.} } @article {432, title = {Measurement of carbon-proton dipolar couplings in liquid crystals by local dipolar field NMR spectroscopy}, journal = {Journal of Physical Chemistry}, volume = {100}, year = {1996}, note = {J Phys Chem-UsVv354Times Cited:54Cited References Count:31}, month = {Nov 28}, pages = {18696-18701}, abstract = {

The performance of several different two-dimensional NMR methods for the measurement of carbon-proton dipolar couplings in liquid crystalline phases is analyzed. Proton-detected local field spectroscopy allows the measurements of short range C-H couplings, which correspond to directly bond pairs, by direct inspection of the spectra. Off magic angle (OMAS) spinning techniques can be applied to anisotropic phases that can be oriented mechanically at an angle to the magnetic field, such as nematic phases. The consequent scaling of the chemical shift anisotropy and dipolar couplings can be used to resolve otherwise overlapping resonances, Moreover, an estimate of the accuracy of the technique can be achieved by performing a series of OMAS experiments with different sample orientations.

}, keywords = {solids}, isbn = {0022-3654}, doi = {Doi 10.1021/Jp962023z}, url = {://WOS:A1996VV35400008}, author = {Caldarelli, S. and Hong, M. and Emsley, L. and Pines, A.} } @article {458, title = {Nmr Measurement of Resolved Heteronuclear Dipole Couplings in Liquid-Crystals and Lipids}, journal = {Journal of Physical Chemistry}, volume = {98}, year = {1994}, note = {J Phys Chem-UsNw531Times Cited:68Cited References Count:25}, month = {Jul 7}, pages = {6668-6670}, abstract = {

Simplified nuclear magnetic resonance (NMR) spectra of heteronuclear dipolar couplings for molecules in an anisotropic environment, such as liquid crystals and lipids, are obtained by proton-detected local-field spectroscopy. The distance-dependent dipolar interactions between spins of magnetically active nuclei can be determined directly from the spectrum because many-body effects that complicate conventional dipolar NMR spectra are avoided by selectively probing local fields produced by rare spins at the location of abundant spins. We employ the technique to resolve the carbon-proton dipolar couplings of benzene dissolved in a nematic liquid crystal and to measure phosphorus-proton couplings in lecithin in the L(alpha) phase to obtain constraints on the phosphocholine headgroup structure.

}, keywords = {solids}, isbn = {0022-3654}, doi = {Doi 10.1021/J100078a002}, url = {://WOS:A1994NW53100002}, author = {Schmidt-Rohr, K. and Nanz, D. and Emsley, L. and Pines, A.} } @article {470, title = {Effects of Double Rotation on Homonuclear Spin Systems}, journal = {Journal of Magnetic Resonance Series A}, volume = {102}, year = {1993}, note = {J Magn Reson Ser AKz354Times Cited:3Cited References Count:13}, month = {Mar}, pages = {29-33}, keywords = {solids}, isbn = {1064-1858}, doi = {Doi 10.1006/Jmra.1993.1064}, url = {://WOS:A1993KZ35400005}, author = {Wu, Y. and Peng, Z. Y. and Olejniczak, Z. and Sun, B. Q. and Pines, A.} } @article {491, title = {Multiple-Quantum Nmr-Study of the Distribution of Benzene in Nay Zeolite}, journal = {Journal of Physical Chemistry}, volume = {96}, year = {1992}, note = {J Phys Chem-UsJu555Times Cited:26Cited References Count:24}, month = {Oct 15}, pages = {8517-8522}, abstract = {

We have used multiple-quantum NMR to measure the apparent spin network size as a function of excitation time of NaY zeolite samples containing varying amounts of benzene. Behavior observed at low concentrations of benzene was consistent with the presence of isolated clusters of benzene molecules in the supercages, with a statistical distribution of benzene molecules between supercages. Behavior observed at high concentrations of benzene was consistent with the presence of weakly coupled clusters of benzene molecules, with a uniform distribution of benzene molecules between supercages.

}, keywords = {solids}, isbn = {0022-3654}, doi = {Doi 10.1021/J100200a057}, url = {://WOS:A1992JU55500057}, author = {Pearson, J. G. and Chmelka, B. F. and Shykind, D. N. and Pines, A.} } @article {501, title = {High-Field Nmr of Adsorbed Xenon Polarized by Laser Pumping}, journal = {Physical Review Letters}, volume = {66}, year = {1991}, note = {Phys Rev LettEv897Times Cited:202Cited References Count:35}, month = {Feb 4}, pages = {584-587}, abstract = {

Optical pumping has been used to enhance the pulsed NMR signal of Xe-129, allowing the detection of low-pressure xenon gas and of xenon adsorbed on powdered solids. We observe an increase in sensitivity of more than 2 orders of magnitude over conventional NMR, the current limitation being the laser power. Adsorbed xenon is observed at 298 K on graphitized carbon (10 m2/g) and on powdered benzanthracene (approximately 0.5 m2/g) below 170 K. The increased sensitivity of this technique allows the study of a large class of amorphous materials with surface areas below 10 m2/g including semiconductors, polymers, metal oxides, and catalysts.

}, keywords = {solids}, isbn = {0031-9007}, doi = {Doi 10.1103/Physrevlett.66.584}, url = {://WOS:A1991EV89700017}, author = {Raftery, D. and Long, H. and Meersmann, T. and Grandinetti, P. J. and Reven, L. and Pines, A.} }