Correlation of fast and slow chemical shift spinning sideband patterns under fast magic-angle spinning.
A new two-dimensional solid-state NMR experiment, which correlates slow and fast chemical shift anisotropy sideband patterns is proposed. The experiment, dubbed ROSES, is performed under fast magic-angle spinning and leads to an isotropic spectrum in the directly detected omega(2) dimension. In the evolution dimension omega(1), the isotropic chemical shift is reduced by a factor S, and spinning sidebands are observed spaced by a scaled effective spinning speed omega(R)/S. These spinning sidebands patterns are not identical to those observed with standard slow magic-angle spinning experiments. Chemical shift anisotropy parameters can be accurately extracted with standard methods from these spinning sideband patterns. The experiment is demonstrated with carbon-13 experiments on powdered samples of a dipeptide and a cyclic undecapeptide, cyclosporin-A.
Eléna
Bénédicte
B
Laboratoire de Stéréochimie et des Interactions Moléculaires, UMR 5532, CNRS/ENS Lyon, France.
Hediger
Sabine
S
Emsley
Lyndon
L
D016880:Anisotropy; D002247:Carbon Isotopes; D003198:Computer Simulation; D016572:Cyclosporine / Q000737:chemistry*; D004151:Dipeptides / Q000737:chemistry*; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*
D002247:Carbon Isotopes; D004151:Dipeptides; D016572:Cyclosporine