Symmetry-based recoupling of proton chemical shift anisotropies in ultrahigh-field solid-state NMR

被引:42
作者
Brouwer, Darren H. [1 ]
Ripmeester, John A. [1 ]
机构
[1] CNR, Steacie Inst Mol Sci, Ottawa, ON K1A 0R6, Canada
基金
加拿大创新基金会;
关键词
proton MAS NMR; chemical shift anisotropy; recoupling; CRAMPS; hydrogen bonding;
D O I
10.1016/j.jmr.2006.12.003
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A two-dimensional NMR experiment for estimating proton chemical shift anisotropies (CSAs) in solid powders under magic-angle spinning conditions is demonstrated in which H-1 CSAs are reintroduced with a symmetry-based recoupling sequence while the individual proton sites are resolved according to their isotropic chemical shifts by magic-angle spinning (MAS) or combined rotation and multiple pulse (CRAMPS) homonuclear decoupling. The experiments where carried out on an ultrahigh-field solid-state NMR instrument (900 MHz H-1 frequency) which leads to increased resolution and reliability of the measured H-1 CSAs. The experiment is expected to be important for investigating hydrogen bonding in solids. Crown Copyright (c) 2006 Published by Elsevier Inc. All rights reserved.
引用
收藏
页码:173 / 178
页数:6
相关论文
共 23 条
[1]  
ALLA MA, 1978, JETP LETT+, V27, P194
[2]   CORRELATIONS BETWEEN PROTON CHEMICAL-SHIFT TENSORS, DEUTERIUM QUADRUPOLE COUPLINGS, AND BOND DISTANCES FOR HYDROGEN-BONDS IN SOLIDS [J].
BERGLUND, B ;
VAUGHAN, RW .
JOURNAL OF CHEMICAL PHYSICS, 1980, 73 (05) :2037-2043
[3]   Symmetry principles in the nuclear magnetic resonance of spinning solids: Heteronuclear recoupling by generalized Hartmann-Hahn sequences [J].
Brinkmann, A ;
Levitt, MH .
JOURNAL OF CHEMICAL PHYSICS, 2001, 115 (01) :357-384
[4]   Solid-state NMR investigations on the nature of hydrogen bonds [J].
Brunner, E ;
Sternberg, U .
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY, 1998, 32 :21-57
[5]   Recoupling of chemical shift anisotropies in solid-state NMR under high-speed magic-angle spinning and in uniformly 13C-labeled systems [J].
Chan, JCC ;
Tycko, R .
JOURNAL OF CHEMICAL PHYSICS, 2003, 118 (18) :8378-8389
[6]   MULTIPLE PULSE STUDY OF PROTON SHIELDING IN SINGLE-CRYSTALS OF MALEIC ACID [J].
GROSESCU, R ;
ACHLAMA, AM ;
HAEBERLEN, U ;
SPIESS, HW .
CHEMICAL PHYSICS, 1974, 5 (01) :119-128
[7]   Tilted n-fold symmetric radio frequency pulse sequences:: Applications to CSA and heteronuclear dipolar recoupling in homonuclear dipolar coupled spin networks [J].
Gross, JD ;
Costa, PR ;
Griffin, RG .
JOURNAL OF CHEMICAL PHYSICS, 1998, 108 (17) :7286-7293
[8]  
HAEBERLEN U, 1976, HIGH RESOLUTION SOLI
[9]   PERSPECTIVES IN HIGH-RESOLUTION SOLID-STATE NUCLEAR MAGNETIC-RESONANCE, WITH EMPHASIS ON COMBINED ROTATION AND MULTIPLE-PULSE SPECTROSCOPY [J].
HARRIS, RK ;
JACKSON, P ;
MERWIN, LH ;
SAY, BJ ;
HAGELE, G .
JOURNAL OF THE CHEMICAL SOCIETY-FARADAY TRANSACTIONS I, 1988, 84 :3649-3672
[10]   1H chemical shielding anisotropies from polycrystalline powders using MSHOT-3 based CRAMPS [J].
Hohwy, M ;
Rasmussen, JT ;
Bower, PV ;
Jakobsen, HJ ;
Nielsen, NC .
JOURNAL OF MAGNETIC RESONANCE, 1998, 133 (02) :374-378