Through-bond heteronuclear single-quantum correlation spectroscopy in solid-state NMR, and comparison to other through-bond and through-space experiments

被引:91
作者
Lesage, A [1 ]
Emsley, L [1 ]
机构
[1] Ecole Normale Super Lyon, Lab Stereochim & Interact Mol, CNRS, UMR 117, F-69364 Lyon, France
关键词
through-bond spectroscopy; heteronuclear correlation methods; scalar couplings; homonuclear decoupling;
D O I
10.1006/jmre.2000.2249
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A new through-bond carbon-proton correlation technique, the MAS-J-HSQC experiment, is described for solid-state NMR. This new pulse scheme is compared experimentally with the previously proposed MAS-J-HMQC experiment in terms of proton resolution on a model sample of powdered L-alanine. We show that for natural abundance compounds, the MAS-J-HMQC and MAS-J-HSQC experiments give about the same proton resolution, whereas, for C-13-labeled materials, narrower proton linewidths are obtained with the MAS-J-HSQC experiment. In addition we show that in scalar as well as in dipolar heteronuclear shift correlation experiments, when the proton chemical shift is encoded by the evolution of a single-quantum coherence, the proton resolution can be enhanced by simply adding a 180 degrees carbon pulse in the middle of the t(1) evolution time. (C) 2001 Academic Press.
引用
收藏
页码:449 / 454
页数:6
相关论文
共 27 条
[1]   CORRELATION OF PROTON AND N-15 CHEMICAL-SHIFTS BY MULTIPLE QUANTUM NMR [J].
BAX, A ;
GRIFFEY, RH ;
HAWKINS, BL .
JOURNAL OF MAGNETIC RESONANCE, 1983, 55 (02) :301-315
[2]   HETERONUCLEAR DECOUPLING IN ROTATING SOLIDS [J].
BENNETT, AE ;
RIENSTRA, CM ;
AUGER, M ;
LAKSHMI, KV ;
GRIFFIN, RG .
JOURNAL OF CHEMICAL PHYSICS, 1995, 103 (16) :6951-6958
[3]   FREQUENCY-SWITCHED PULSE SEQUENCES - HOMONUCLEAR DECOUPLING AND DILUTE SPIN NMR IN SOLIDS [J].
BIELECKI, A ;
KOLBERT, AC ;
LEVITT, MH .
CHEMICAL PHYSICS LETTERS, 1989, 155 (4-5) :341-346
[4]  
Bielecki A., 1990, ADV MAGN RESON, V14, P111, DOI [10.1016/b978-0-12-025514-6.50011-3, DOI 10.1016/B978-0-12-025514-6.50011-3]
[5]   NATURAL ABUNDANCE N-15 NMR BY ENHANCED HETERONUCLEAR SPECTROSCOPY [J].
BODENHAUSEN, G ;
RUBEN, DJ .
CHEMICAL PHYSICS LETTERS, 1980, 69 (01) :185-189
[6]   2D H-1-C-13 HETERONUCLEAR CORRELATION SPECTRA OF REPRESENTATIVE ORGANIC-SOLIDS [J].
BRONNIMANN, CE ;
RIDENOUR, CF ;
KINNEY, DR ;
MACIEL, GE .
JOURNAL OF MAGNETIC RESONANCE, 1992, 97 (03) :522-534
[7]   AN IMPROVED EXPERIMENT FOR HETERONUCLEAR-CORRELATION 2D-NMR IN SOLIDS [J].
BURUM, DP ;
BIELECKI, A .
JOURNAL OF MAGNETIC RESONANCE, 1991, 94 (03) :645-652
[8]  
BURUM DP, 1997, ENCY NMR, P2323
[9]   HETERONUCLEAR SOLID-STATE CORRELATION SPECTROSCOPY [J].
CARAVATTI, P ;
BODENHAUSEN, G ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1982, 89 (05) :363-367
[10]   HETERONUCLEAR CORRELATION SPECTROSCOPY IN ROTATING SOLIDS [J].
CARAVATTI, P ;
BRAUNSCHWEILER, L ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1983, 100 (04) :305-310