Annual Reports on NMR Spectroscopy, Vol. 23 by G. A. Webb

By G. A. Webb

This e-book is a part of a chain on spectroscopy, and covers NMR reviews of remoted spin-pairs within the reliable nation, the oxidation nation dependence of transition steel shieldings, the Cinderella nuclei, nuclear spin leisure in natural platforms, strategies of macromolecules and aggregates and the NMR of coals and coal items. similar titlesare volumes 20, 21 and 22 within the sequence. summary: This e-book is a part of a sequence on spectroscopy, and covers NMR reviews of remoted spin-pairs within the sturdy country, the oxidation nation dependence of transition steel shieldings, the Cinderella nuclei, nuclear spin rest in natural structures, options of macromolecules and aggregates and the NMR of coals and coal items. comparable titlesare volumes 20, 21 and 22 within the sequence

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The dipolar coupling is only on the order of 50Hz in this case, indicating the potential of this technique for observing such small interactions, and, hence, large spin-spin separations. 4. 1 One-dimensional NMR studies of single-crystal and powder samples The first rigorous treatment of NMR powder patterns due to isolated heteronuclear spin pairs was detailed by VanderHart and Gutowsky' 26 in 1968. They proposed both moment and full line-shape methods of analysis to determine chemical shift, dipolar coupling and indirect coupling information from rigid-lattice NMR line shapes.

12)), where the angles 8 and I$ orient the magnetic-field vector in the principal-axis system of the chemical-shift tensor. Equation (18) is now substituted into (17) in order to describe properly the effect of dipolar coupling. The experimental line shape is analysed, usually by fitting to spectra calculated using (17), in order to obtain R , a and fl for that particular system, as well as the chemical-shift-tensor components. The value of R can be used to derive internuclear separations from polycrystalline samples.

Previous 'H chemical-shift tensor assignments for malonic acid68 were confirmed in this manner. ^' The orientation dependence of each of these interactions provided the spatial orientation of the phenyl ring plane, carboxyl group plane and the long axis of the molecule within the unit cell, in excellent agreement with neutron-diffraction results. Homonuclear and heteronuclear decoupling techniques were required to eliminate 'H-'H, 'H-19F and 19F-19Fdipolar broadening of the various abundant spin spectra.

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