By G. A. Webb
This e-book is a part of a chain on spectroscopy, and covers NMR reports of remoted spin-pairs within the reliable country, the oxidation nation dependence of transition steel shieldings, the Cinderella nuclei, nuclear spin leisure in natural structures, 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 publication is a part of a sequence on spectroscopy, and covers NMR stories of remoted spin-pairs within the stable kingdom, the oxidation country dependence of transition steel shieldings, the Cinderella nuclei, nuclear spin rest in natural structures, ideas 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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Extra info for Annual Reports on NMR Spectroscopy, Vol. 23
8 kJmol-'. Single-crystal 'H NMR spectra of malonic acid (11) were obtained by Schuff and Haeberlen66 using a two-dimensional technique similar to that used for trichloroacetic acid6' with two important differences. First, Fourier transformation was applied to both time dimensions. This necessitated the second difference, a modified MREV-8 decoupling sequence to allow quadrature sensitivity in o1by preserving the t , phase information at t , = 0. The result was a spectrum with homonuclear dipolar couplings in o1resolved by isotropic chemical shifts in 0,for each crystallographically distinct 'H.
35 1 ........ ,\Q ......... 67 A. Thus, the dipolar NM R results, together with MM2 calculations, led the authors to conclude that the short C-C bond length reported for VI was grossly in error. '08 Examination of the 13C CPnutation NMR spectra of two separate samples of doubly labelled t-butyl cations, ['3CH3'3C(CH,)2]+ and [CH3C('3CH3)2] (see Fig. 51 A, respectively. e. the carbon skeleton of the t-butyl cation in C,H; Sb2F,,X- was planar). This example clearly demonstrated that in situations where single crystals of reactive carbocations are unavailable, valuable structural information could be obtained from dipolar NMR.
Homonuclear and heteronuclear decoupling techniques were required to eliminate 'H-'H, 'H-19F and 19F-19Fdipolar broadening of the various abundant spin spectra. For example, to allow observation of the 'H-'H dipolar splittings, the 19Fnuclei were decoupled by a train of n pulses. 19). Presumably, this was due to the anisotropic libration of the protons in the dimer structure of 111. Recently, other investigators have considered asymmetric dipolar coupling tensors in detail. 2H,O) has two NMR STUDIES OF ISOLATED SPIN PAIRS IN THE SOLID STATE 23 molecules of water of hydration per molecular unit in its crystal lattice.