Out-and-back (13)C-(13)C Scalar Transfers in Protein Resonance Assignment by Proton-Detected Solid-State NMR under Ultra-Fast MAS

Journal of Biomolecular NMR 2013
E. Barbet-Massin, A.J. Pell, Kristaps Jaudzems, W.T. Franks, J.S. Retel, S. Kotelovica, I. Akopjana, K. Tars, L. Emsley, H. Oschkinat, A. Lesage, G. Pintacuda

e present here 1H-detected triple-resonance H/N/C experiments that incorporate CO–CA and CA–CB out-and-back scalar-transfer blocks optimized for robust resonance assignment in biosolids under ultra-fast magic-angle spinning (MAS). The first experiment, (H)(CO)CA(CO)NH, yields 1H-detected inter-residue correlations, in which we record the chemical shifts of the CA spins in the first indirect dimension while during the scalar-transfer delays the coherences are present only on the longer-lived CO spins. The second experiment, (H)(CA)CB(CA)NH, correlates the side-chain CB chemical shifts with the NH of the same residue. These high sensitivity experiments are demonstrated on both fully-protonated and 100 %-HN back-protonated perdeuterated microcrystalline samples of Acinetobacter phage 205 (AP205) capsids at 60 kHz MAS.

Atslēgas vārdi
Fully-protonated and deuterated biosolids; Solid-state NMR; Ultra-fast magic-angle spinning; Through-bond transfers; Sensitivity
DOI
10.1007/s10858-013-9757-3
Hipersaite
http://link.springer.com/article/10.1007%2Fs10858-013-9757-3

Barbet-Massin, E., Pell, A., Jaudzems, K., Franks, W., Retel, J., Kotelovica, S., Akopjana, I., Tars, K., Emsley, L., Oschkinat, H., Lesage, A., Pintacuda, G. Out-and-back (13)C-(13)C Scalar Transfers in Protein Resonance Assignment by Proton-Detected Solid-State NMR under Ultra-Fast MAS. Journal of Biomolecular NMR , 2013, Vol.56, Iss.4, 379.-386.lpp. e-ISSN 1573-5001. ISSN 0925-2738. Pieejams: doi:10.1007/s10858-013-9757-3

Publikācijas valoda
English (en)