Out-and-back 13C–13C scalar transfers in protein resonance assignment by proton-detected solid-state NMR under ultra-fast MAS

被引：0
作者：
Emeline Barbet-Massin
Andrew J. Pell
Kristaps Jaudzems
W. Trent Franks
Joren S. Retel
Svetlana Kotelovica
Inara Akopjana
Kaspars Tars
Lyndon Emsley
Hartmut Oschkinat
Anne Lesage
Guido Pintacuda
机构：
[1] University of Lyon,CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN à Très Hauts Champs
[2] Leibniz-Institut für Molekulare Pharmakologie,undefined
[3] Latvian Institute of Organic Synthesis,undefined
[4] Biomedical Research and Study Center,undefined
来源：
Journal of Biomolecular NMR | 2013年 / 56卷
关键词：
Fully-protonated and deuterated biosolids; Solid-state NMR; Ultra-fast magic-angle spinning; Through-bond transfers; Sensitivity;
D O I：
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学科分类号：
摘要：
We 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.
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页码：379 / 386
页数：7
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