Title | Using switched angle spinning to simplify NMR spectra of strongly oriented samples |
Publication Type | Journal Article |
Year of Publication | 2003 |
Authors | Havlin R.H, Park G.HJ, Mazur T., Pines A |
Journal | Journal of the American Chemical Society |
Volume | 125 |
Issue | 26 |
Pagination | 7998-8006 |
Date Published | Jul 2 |
ISBN Number | 0002-7863 |
Accession Number | WOS:000183814500059 |
Keywords | solids |
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. |
URL | <Go to ISI>://WOS:000183814500059 |
DOI | 10.1021/Ja0342244 |
Short Title | Using switched angle spinning to simplify NMR spectra of strongly oriented samples |
Using switched angle spinning to simplify NMR spectra of strongly oriented samples
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