@article {316, title = {Isotropic proton-detected local-field nuclear magnetic resonance in solids}, journal = {Journal of Chemical Physics}, volume = {122}, year = {2005}, note = {J Chem Phys899JFTimes Cited:1Cited References Count:31}, month = {Feb 15}, abstract = {

A nuclear magnetic resonance method is presented which produces linear, isotropic proton-detected local-field spectra for INS spin systems in powdered samples. The method, heteronuclear isotropic evolution (HETIE), refocuses the anisotropic portion of the heteronuclear dipolar coupling frequencies by evolving the system under a series of specially designed Hamiltonians and evolution pathways. The theory behind HETIE is presented along with experimental studies conducted on a powdered sample of ferrocene, demonstrating the methodology outlined in this paper. Applications of HETIE for use in structure determination in the solid state are discussed. (C) 2005 American Institute of Physics.

}, keywords = {spectra}, isbn = {0021-9606}, doi = {Doi 10.1063/1.1844296}, url = {://WOS:000227140000043}, author = {Havlin, R. H. and Walls, J. D. and Pines, A.} } @article {306, title = {NMR spectroscopy in inhomogeneous B-0 and B-1 fields with non-linear correlation}, journal = {Journal of Magnetic Resonance}, volume = {175}, year = {2005}, note = {J Magn Reson939CPTimes Cited:8Cited References Count:38}, month = {Jul}, pages = {1-10}, abstract = {

Resolved NMR spectra from samples in inhomogeneous B-0 and B-1 fields can be obtained with the so-called \"ex situ\" methodology, employing a train of composite or adiabatic z-rotation RF pulses to periodically refocus the inhomogeneous broadening during the detection of the time-domain signal. Earlier schemes relied on a linear correlation between the inhomogeneous B0 and B, fields. Here the pulse length, bandwidth, and amplitude of the adiabatic pulses of the hyperbolic secant type are adjusted to improve the refocusing for a setup with non-linear correlation. The field correlation is measured using a two-dimensional nutation experiment augmented with a third dimension with varying RF carrier frequency accounting for off-resonance effects. The pulse optimization is performed with a computer algorithm using the experimentally determined field correlation and a standard adiabatic z-rotation pulse as a starting point for the iterative optimization procedure. The shape of the z-rotation RF pulse is manipulated to provide refocusing for the conditions given by the sample-, magnet-, and RF-coil geometry. (c) 2005 Elsevier Inc. All rights reserved.

}, keywords = {spectra}, isbn = {1090-7807}, doi = {Doi 10.1016/J.Jmr.2005.03.006}, url = {://WOS:000230050200001}, author = {Topgaard, D. and Sakellariou, D. and Pines, A.} } @article {449, title = {C-13 Chemical-Shift Tensor Correlation Via Spin-Diffusion in Solid Tropolone Using Switched-Angle Spinning Spectroscopy}, journal = {Journal of Chemical Physics}, volume = {103}, year = {1995}, note = {J Chem PhysTh657Times Cited:7Cited References Count:42}, month = {Dec 8}, pages = {9844-9854}, abstract = {

In switched-angle spinning spectroscopy (SAS) a sample is spun about different angles, beta, relative to the magnetic field, during various periods of the experiment. In the present work, SAS is combined with two-dimensional exchange spectroscopy in order to correlate carbon-13 chemical shift tensors of the carbonyl (1) and hydroxyl (2) carbons of tropolone. Experiments were performed on a sample enriched to 25 at. \% in each of these sites (at different molecules). At this level of enrichment the dominant exchange mechanism between the two sites involves spin diffusion, The experiment consists of a preparation period during which the sample spins at the magic angle and the magnetization of one of the sites is quenched by means of a selective pulse sequence. During the rest of the experiment the sample spins with its axis away from the magic angle except for a short period just before the detection where the axis is switched to the magic angle in order to select the magnetization to be detected. Experiments were performed for all four possible combinations of the initial and final magnetizations, thus providing chemical shift correlations between carbons 1,1\&$\#$39;,2, and 2\&$\#$39; in the two magnetically inequivalent (but symmetry related) molecules in the unit cell. Combining these results with the known crystal structure of tropolone (neglecting a small tilt between the perpendicular to the molecular plane and the crystallographic c-axis) provides information on the orientation and magnitude of the chemical shift tensors of the two types of carbons, The principal values (in ppm) are sigma(xx)(1)=65, sigma(yy)(1)=33, sigma(zz)(1)=-98, sigma(xx)(2)=77, sigma(yy)(2)=17, and sigma(zz)(2)=-94. Assuming sigma(zz) to be perpendicular to the molecular plane, the orientations of the sigma(yy) s\&$\#$39; are 12 degrees off the C-1=0 bond (toward the hydroxyl carbon) for carbon 1 and 10 degrees off the C-3=C-2 bond (away from the carbonyl carbon) for carbon 2. (C) 1995 American Institute of Physics.

}, keywords = {spectra}, isbn = {0021-9606}, doi = {Doi 10.1063/1.469951}, url = {://WOS:A1995TH65700040}, author = {Larsen, R. G. and Lee, Y. K. and He, B. and Yang, J. O. and Luz, Z. and Zimmermann, H. and Pines, A.} } @article {504, title = {High-Resolution O-17 Nmr of Solid Silicates}, journal = {Journal of the American Chemical Society}, volume = {113}, year = {1991}, note = {J Am Chem SocEr082Times Cited:90Cited References Count:39}, month = {Jan 2}, pages = {32-38}, abstract = {

Several O-17-enriched silicates were studied by use of dynamic angle spinning (DAS) and double rotation (DOR) nuclear magnetic resonance spectroscopy. These methods average away second-order quadrupolar interactions by reorienting a sample about a time-dependent axis, thereby yielding high-resolution spectra of oxygen-17 nuclei. A narrow spectral line is observed for each distinct oxygen site at the sum of the isotropic chemical shift and the field-dependent isotropic second-order quadrupolar shift. Resolution is increased by up to 2 orders of magnitude compared to conventional magic angle spinning (MAS) spectra. Crystallographically inequivalent oxygens are now observable as distinct resonances in spectra of polycrystalline silicates such as diopside (CaMgSi2(17)O6), wollastonite (CaSi17O3), clinoenstatite (MgSi17O3), larnite (Ca2Si17O4),and forsterite (Mg2Si17O4).

}, keywords = {spectra}, isbn = {0002-7863}, doi = {Doi 10.1021/Ja00001a006}, url = {://WOS:A1991ER08200006}, author = {Mueller, K. T. and Wu, Y. and Chmelka, B. F. and Stebbins, J. and Pines, A.} }