13C-Detected Through-Bond Correlation Experiments for Protein Resonance Assignment by Ultra-Fast MAS Solid-State NMR

被引：17

作者：

Barbet-Massin, Emeline ^{[1
]}

Pell, Andrew J. ^{[1
]}

Knight, Michael J. ^{[1
]}

Webber, Amy L. ^{[1
]}

Felli, Isabella C. ^{[2
,3
]}

Pierattelli, Roberta ^{[2
,3
]}

Emsley, Lyndon ^{[1
]}

Lesage, Anne ^{[1
]}

Pintacuda, Guido ^{[1
]}

机构：

[1] Univ Lyon, CNRS, UMR 5280, Ecole Normale Super Lyon,Ctr RMN Tres Hauts Champ, F-69100 Villeurbanne, France

[2] Univ Florence, Dept Chem Ugo Schiff, I-50019 Sesto Fiorentino, Italy

[3] Univ Florence, Magnet Resonance Ctr CERM, I-50019 Sesto Fiorentino, Italy

来源：

CHEMPHYSCHEM | 2013年 / 14卷 / 13期

关键词：

J-coupling; paramagnetism; solid-state nuclear magnetic resonance spectroscopy; superoxide dismutase; magic angle spinning; CORRELATION SPECTROSCOPY; CROSS-POLARIZATION; MICROCRYSTALLINE PROTEIN; SPIN SYSTEMS; C-13; RESOLUTION; SENSITIVITY; COHERENCE; DYNAMICS; SEQUENCE;

D O I：

10.1002/cphc.201201097

中图分类号：

O64 [物理化学（理论化学）、化学物理学];

学科分类号：

070304 ; 081704 ;

摘要：

We present two sequences which combine (H-1,N-15) and (N-15,C-13) selective cross-polarization steps with an efficient variant of the J-based homonuclear transfer scheme, in which a spin-state-selective ((SE)-E-3) block is incorporated to improve both resolution and sensitivity in the direct C-13 dimension. We propose these two sequences as a part of a suite of four N-C correlation experiments allowing for the assignment of protein backbone resonances in the solid state. We illustrate these experiments under ultra-fast magic angle spinning conditions on two samples of microcrystalline dimeric human superoxide dismutase (SOD, 153x2 amino acids), in its diamagnetic (empty, Zn-II) and paramagnetic (Cu-II, Zn-II) states.

引用

页码：3131 / 3137

页数：7

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[51] AN IMPROVED SEQUENCE FOR BROAD-BAND DECOUPLING - WALTZ-16 [J].