Ultrahigh resolution in proton solid-state NMR spectroscopy at high levels of deuteration

被引:251
作者
Chevelkov, V [1 ]
Rehbein, K [1 ]
Diehl, A [1 ]
Reif, B [1 ]
机构
[1] Leibniz Inst Mol Pharmakol FMP, D-13125 Berlin, Germany
关键词
line widths; magic-angle spinning; predeuteration; proteins; solid-state NMR spectroscopy; structure elucidation;
D O I
10.1002/anie.200600328
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
(Figure Presented) Slim peaks: Using a perdeuterated protein recrystallized from a 10:90 H2O:D2O mixture in magic-angle spinning (MAS) solid-state NMR spectroscopy experiments gives small 1H line widths at moderate spinning frequencies without application of homonuclear decoupling. This labeling strategy opens new perspectives for assignment of large protein spin systems. © 2006 Wiley-VCH Verlag GmbH & Co. KGaA.
引用
收藏
页码:3878 / 3881
页数:4
相关论文
共 28 条
[1]   Structure of a protein determined by solid-state magic-angle-spinning NMR spectroscopy [J].
Castellani, F ;
van Rossum, B ;
Diehl, A ;
Schubert, M ;
Rehbein, K ;
Oschkinat, H .
NATURE, 2002, 420 (6911) :98-102
[2]   Detection of dynamic water molecules in a microcrystalline sample of the SH3 domain of a-spectrin by MAS solid-state NMR [J].
Chevelkov, V ;
Faelber, K ;
Diehl, A ;
Heinemann, U ;
Oschkinat, H ;
Reif, B .
JOURNAL OF BIOMOLECULAR NMR, 2005, 31 (04) :295-310
[3]   1H detection in MAS solid-state NMR Spectroscopy of biomacromolecules employing pulsed field gradients for residual solvent suppression [J].
Chevelkov, V ;
van Rossum, BJ ;
Castellani, F ;
Rehbein, K ;
Diehl, A ;
Hohwy, M ;
Steuernagel, S ;
Engelke, F ;
Oschkinat, H ;
Reif, B .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (26) :7788-7789
[4]   Low-power high-resolution solid-state NMR of peptides and proteins [J].
Ernst, M ;
Meier, MA ;
Tuherm, T ;
Samoson, A ;
Meier, BH .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (15) :4764-4765
[5]   Solid-state nuclear magnetic resonance spectra of dipolar-coupled multi-spin systems under fast magic angle spinning [J].
Filip, C ;
Hafner, S ;
Schnell, I ;
Demco, DE ;
Spiess, HW .
JOURNAL OF CHEMICAL PHYSICS, 1999, 110 (01) :423-440
[6]   Quantitative analysis of backbone dynamics in a crystalline protein from nitrogen-15 spin-lattice relaxation [J].
Giraud, N ;
Blackledge, M ;
Goldman, M ;
Böckmann, A ;
Lesage, A ;
Penin, F ;
Emsley, L .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2005, 127 (51) :18190-18201
[7]   Site-specific backbone dynamics from a crystalline protein by solid-state NMR spectroscopy [J].
Giraud, N ;
Böckmann, A ;
Lesage, A ;
Penin, F ;
Blackledge, M ;
Emsley, L .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2004, 126 (37) :11422-11423
[8]   Characterization of dynamic processes using deuterium in uniformly 2H, 13C, 15N enriched peptides by MAS solid-state NMR [J].
Hologne, M ;
Chen, ZJ ;
Reif, B .
JOURNAL OF MAGNETIC RESONANCE, 2006, 179 (01) :20-28
[9]   Characterization of dynamics of perdeuterated proteins by MAS solid-state NMR [J].
Hologne, M ;
Faelber, K ;
Diehl, A ;
Reif, B .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2005, 127 (32) :11208-11209
[10]   Sensitivity enhancement in solid state 15N NMR by indirect detection with high-speed magic angle spinning [J].
Ishii, Y ;
Tycko, R .
JOURNAL OF MAGNETIC RESONANCE, 2000, 142 (01) :199-204