Heteronuclear local field NMR spectroscopy under fast magic-angle sample spinning conditions

被引:23
作者
McElheny, D [1 ]
DeVita, E [1 ]
Frydman, L [1 ]
机构
[1] Univ Illinois, Dept Chem, Chicago, IL 60607 USA
基金
美国国家科学基金会;
关键词
D O I
10.1006/jmre.1999.1995
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The acquisition of bidimensional heteronuclear nuclear magnetic resonance local field spectra under moderately fast magic-angle spinning (MAS) conditions is discussed. It is shown both experimentally and with the aid of numerical simulations on multispin systems that when sufficiently fast MAS rates are employed, quantitative dipolar sideband patterns from directly bonded spin pairs can be acquired in the absence of H-1-H-1 multiple-pulse homonuclear decoupling even for "real" organic solids. The MAS speeds involved are web within the range of commercially available systems (10-14 kHz) and provide sidebands with sufficient intensity to enable a reliable quantification of heteronuclear dipolar couplings from methine groups. Simulations and experiments show that useful information can be extracted in this manner even from more tightly coupled -CH2- moieties, although the agreement with the patterns simulated solely on the basis of heteronuclear interactions is not in this case as satisfactory as for methines, Preliminary applications of this simple approach to the analysis of molecular motions in solids are presented; characteristics and potential extensions of the method are also discussed. (C) 2000 Academic Press.
引用
收藏
页码:321 / 328
页数:8
相关论文
共 43 条
[41]   ASYNCHRONOUS MASSLF SPECTROSCOPY - A CONVENIENT METHOD FOR ASSIGNING SOLID-STATE C-13 CPMAS SPECTRA [J].
WEBB, GG ;
ZILM, KW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1989, 111 (07) :2455-2463
[42]   MOLECULAR-DYNAMICS IN ORDERED STRUCTURES - COMPUTER-SIMULATION AND EXPERIMENTAL RESULTS FOR NYLON-66 CRYSTALS [J].
WENDOLOSKI, JJ ;
GARDNER, KH ;
HIRSCHINGER, J ;
MIURA, H ;
ENGLISH, AD .
SCIENCE, 1990, 247 (4941) :431-436
[43]   HYDROGEN-SILICON NUCLEAR-SPIN CORRELATIONS IN ALPHA-SI-H - A TWO-DIMENSIONAL NMR-STUDY [J].
ZUMBULYADIS, N .
PHYSICAL REVIEW B, 1986, 33 (09) :6495-6496