SSNMR, Duer, CSA-amplified PASS

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Solid State Nuclear Magnetic Resonance
Volume 30, Issue 1 , July 2006, Pages 1-8

Applications of the CSA-amplified PASS experiment

Robin M. Orr and Melinda J. Duer
Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK

Abstract

The recently reported CSA-amplified PASS experiment correlates the spinning sidebands at the true spinning frequency ?r with the spinning sidebands that would be obtained at the effective spinning frequency ?r/N, where N is termed the scaling factor. The experiment is useful for the measurement of small chemical shift anisotropies, for which slow magic-angle spinning frequencies, required to measure several spinning sidebands, can be unstable. We have experimentally evaluated the reliability of this experiment for this application. In particular we have demonstrated that large scaling factors of the order of N=27 may be used, whilst still obtaining accurate chemical shift sideband intensities at the effective spinning frequency from the F1 projection. Moreover, the sideband intensities are accurately obtained even in the presence of significant pulse imperfections. A second application of the CSA-amplified PASS experiment is the measurement of the chemical shift anisotropy of sites that experience homonuclear dipolar coupling, as may be found in uniformly labelled biological molecules, or for nuclei with a high natural abundance. The effects of homonuclear dipolar coupling on CSA-amplified PASS spectra has been investigated by numerical simulations and are demonstrated using uniformly 13C enriched l-histidine monohydrochloride monohydrate.

Keywords: Solid-state NMR; Magic-angle spinning; Chemical shift anisotropy; Recoupling; Homonuclear dipolar coupling