High-resolution NMR spectroscopy in solids by truly magic-angle spinning

被引：30

作者：

Antonijevic, S

Bodenhausen, G ^{[1
]}

机构：

[1] Ecole Polytech Fed Lausanne, Inst Sci & Ingn Chim, ISIC, Lab Resonance Magnet Biomol,BCH, CH-1015 Lausanne, Switzerland

[2] Ecole Normale Super, CNRS, Dept Chim, F-75231 Paris, France

来源：

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION | 2005年 / 44卷 / 19期

关键词：

line widths; NMR spectroscopy; solid-state NMR spectroscopy; temperature gradients;

D O I：

10.1002/anie.200463049

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

Right angles: In solid-state magic-angle spinning (MAS) NMR spectra, the line widths of carbonyl carbon atoms in polycrystalline cholesteryl acetate are found to be as narrow as 0.039 ppm if the magic angle is adjusted very accurately, that is, within ±0.004° (see picture). The line broadening observed for slightly miss-set angles is mostly due to residual chemical shift anisotropy (CSA) interactions. Long spin-echo life times up to T′2 = 3.6 s open the way to sophisticated NMR methods. (Graph Presented) © 2005 Wiley-VCH Verlag GmbH & Co. KGaA.

引用

页码：2935 / 2938

页数：4

共 25 条

[1] TEMPERATURE-GRADIENTS AND SAMPLE HEATING IN VARIABLE TEMPERATURE HIGH-SPEED MAS NMR-SPECTROSCOPY [J].

AGUILARPARRILLA, F ;

WEHRLE, B ;

BRAUNLING, H ;

LIMBACH, HH .

JOURNAL OF MAGNETIC RESONANCE, 1990, 87 (03) :592-597

[2] RESOLUTION LIMITS IN MAGIC-ANGLE ROTATION NMR-SPECTRA OF POLYCRYSTALLINE SOLIDS [J].

ALLA, M ;

LIPPMAA, E .

CHEMICAL PHYSICS LETTERS, 1982, 87 (01) :30-33

[3] Motional broadening: an important distinction between multiple-quantum and satellite-transition MAS NMR of quadrupolar nuclei [J].

Ashbrook, SE ;

Antonijevic, S ;

Berry, AJ ;

Wimperis, S .

CHEMICAL PHYSICS LETTERS, 2002, 364 (5-6) :634-642

[4] Satellite-transition MAS NMR of spin I=3/2, 5/2, 7/2, and 9/2 nuclei: Sensitivity, resolution, and practical implementation [J].

Ashbrook, SE ;

Wimperis, S .

JOURNAL OF MAGNETIC RESONANCE, 2002, 156 (02) :269-281

[5] A thermometer for nonspinning solid-state NMR spectroscopy [J].

Beckmann, PA ;

Dybowski, C .

JOURNAL OF MAGNETIC RESONANCE, 2000, 146 (02) :379-380

[6] 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

[7] Transverse dephasing optimised NMR spectroscopy in solids:: Natural-abundance 13C correlation spectra [J].

De Paëpe, G ;

Lesage, A ;

Steuernagel, S ;

Emsley, L .

CHEMPHYSCHEM, 2004, 5 (06) :869-875

[8] Transverse dephasing optimized solid-state NMR spectroscopy [J].

De Paëpe, G ;

Giraud, N ;

Lesage, A ;

Hodgkinson, P ;

Böckmann, A ;

Emsley, L .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (46) :13938-13939

[9] The performance of phase modulated heteronuclear dipolar decoupling schemes in fast magic-angle-spinning nuclear magnetic resonance experiments [J].

De Paëpe, G ;

Lesage, A ;

Emsley, L .

JOURNAL OF CHEMICAL PHYSICS, 2003, 119 (09) :4833-4841

[10] NMR spectra of a microcrystalline protein at 30 kHz MAS [J].

Ernst, M ;

Detken, A ;

Böckmann, A ;

Meier, BH .

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (51) :15807-15810

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