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

被引：47

作者：

Barbet-Massin, Emeline ^{[1
]}

Pell, Andrew J. ^{[1
]}

Jaudzems, Kristaps ^{[2
]}

Franks, W. Trent ^{[3
]}

Retel, Joren S. ^{[3
]}

Kotelovica, Svetlana ^{[4
]}

Akopjana, Inara ^{[4
]}

Tars, Kaspars ^{[4
]}

Emsley, Lyndon ^{[1
]}

Oschkinat, Hartmut ^{[3
]}

Lesage, Anne ^{[1
]}

Pintacuda, Guido ^{[1
]}

机构：

[1] Univ Lyon, CNRS ENS Lyon UCB Lyon 1, Ctr RMN Tres Hauts Champs, Villeurbanne, France

[2] Latvian Inst Organ Synth, Riga, Latvia

[3] Leibniz Inst Mol Pharmacol, Berlin, Germany

[4] Biomed Res & Study Ctr, Riga, Latvia

来源：

JOURNAL OF BIOMOLECULAR NMR | 2013年 / 56卷 / 04期

关键词：

Fully-protonated and deuterated biosolids; Solid-state NMR; Ultra-fast magic-angle spinning; Through-bond transfers; Sensitivity; CROSS-POLARIZATION; SPECTROSCOPY; RESOLUTION;

D O I：

10.1007/s10858-013-9757-3

中图分类号：

Q5 [生物化学]; Q7 [分子生物学];

学科分类号：

071010 ; 081704 ;

摘要：

We present here H-1-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 H-1-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 %-H-N back-protonated perdeuterated microcrystalline samples of Acinetobacter phage 205 (AP205) capsids at 60 kHz MAS.

引用

页码：379 / 386

页数：8

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