Communication
Fast MAS Total Through-Bond Correlation Spectroscopy

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Abstract

Mixing sequences for total through-bond correlation spectroscopy in solids (TOBSY) were developed. The motivation is the design of broadband, effective, and robust sequences adapted for “fast” MAS. Possible sequences with the desired Hamiltonian (the homonuclear isotropic J interaction) were identified using lowest order average Hamiltonian theory. Numerical simulations as a function of the MAS frequency were then employed to further characterize the performance. An experimental TOBSY spectrum of a uniformly 13C-labeled decapeptide at 20 kHz MAS was obtained using one of the new sequences. The spectrum allows us to assign the 13C resonances to the respective spin systems.

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      Citation Excerpt :

      As a result of these multiple features, numerous 13C–13C correlation experiments have been proposed where homonuclear interactions in spinning solids are reintroduced by manipulating the 1Hs that are present in the system; i.e., not the species whose correlations are being sought, but rather heteronuclear species that couple strongly to them. These include methods such as DARR, MIRROR, RAD, and AL-FRESCO, where 1Hs manipulations are timed with the MAS, so as to reinstate the effects of truncated 13C–13C (or 15N–15N) couplings [20–27]. While these experiments rely on dipolar couplings that are not meaningful in isotropic liquids, solution-phase counterparts might also exist where isotropic J couplings drive similar effects.

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    Presented, in part, at the 41st ENC, Pacific Grove, CA.

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