Connectivities in molecules by INADEQUATE: recent developments

被引:29
作者
Buddrus, J [1 ]
Lambert, J [1 ]
机构
[1] Inst Spektrochem & Angew Spektroscopie, D-44013 Dortmund, Germany
关键词
NMR; C-13; Si-29; INADEQUATE; double quantum coherence; connectivity; review;
D O I
10.1002/mrc.923
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The INADEQUATE (Incredible Natural Abundance DoublE QUAntum Transfer Experiment) consists of a pulse sequence which eliminates the NMR signals from isolated spins (spin system A) displaying signals from coupled spins (spin system AX or higher spin systems). It is of great importance when applied to molecules with skeleton elements such as carbon, silicon or tungsten, all of which contain a small percentage of spin-1/2 isotopes embedded in magnetically inactive isotopes. Analysis of the AX type spectra gives one-bond and long-range coupling constants (see compound 6) and, most important, the connectivity pattern of the skeleton atoms in molecules of unknown structure such as the carbon compounds 1 or 2, the silicon compound 3 or the lithium compound 4b. Unfortunately, INADEQUATE is rather insensitive, in the case of carbon only one out of 104 molecules gives the desired response. Efforts to reduce this drawback are described; recently, a remarkable step forward has been made by concentrating the four lines of an AX spin system to just two signals (see Fig. 2). Copyright (C) 2001 John Wiley Sons, Ltd.
引用
收藏
页码:3 / 23
页数:21
相关论文
共 133 条
[1]  
[Anonymous], 1982, 2 DIMENSIONAL NUCL M
[2]   C-13 NMR SPECTRAL ASSIGNMENTS OF REGIOIRREGULAR POLYPROPYLENE DETERMINED FROM 2-DIMENSIONAL INADEQUATE SPECTRA AND CHEMICAL-SHIFT CALCULATIONS [J].
ASAKURA, T ;
NAKAYAMA, N ;
DEMURA, M ;
ASANO, A .
MACROMOLECULES, 1992, 25 (19) :4876-4881
[3]  
ASAKURA T, 1994, ANNU REP NMR SPECTRO, V29, P326
[4]   2-DIMENSIONAL SPECTROSCOPY - APPLICATION TO NUCLEAR MAGNETIC-RESONANCE [J].
AUE, WP ;
BARTHOLDI, E ;
ERNST, RR .
JOURNAL OF CHEMICAL PHYSICS, 1976, 64 (05) :2229-2246
[5]  
Bardet M, 1998, MAGN RESON CHEM, V36, P597, DOI 10.1002/(SICI)1097-458X(199808)36:8<597::AID-OMR345>3.3.CO
[6]  
2-7
[7]   AN NMR TECHNIQUE FOR TRACING OUT THE CARBON SKELETON OF AN ORGANIC-MOLECULE [J].
BAX, A ;
FREEMAN, R ;
FRENKIEL, TA .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1981, 103 (08) :2102-2104
[8]   ASSIGNMENT OF C-13 NMR-SPECTRA VIA DOUBLE-QUANTUM COHERENCE [J].
BAX, A ;
FREEMAN, R ;
FRENKIEL, TA ;
LEVITT, MH .
JOURNAL OF MAGNETIC RESONANCE, 1981, 43 (03) :478-483
[9]   INVESTIGATION OF C-13-C-13 LONG-RANGE COUPLINGS IN NATURAL-ABUNDANCE SAMPLES [J].
BAX, A ;
FREEMAN, R ;
KEMPSELL, SP .
JOURNAL OF MAGNETIC RESONANCE, 1980, 41 (02) :349-353
[10]   THE DETECTION OF CONNECTIVITIES OF RARE SPIN-1/2 NUCLEI IN THE SOLID-STATE USING NATURAL ABUNDANCE SAMPLES - C-13 AND SI-29 INADEQUATE AND COSY TYPE EXPERIMENTS [J].
BENN, R ;
GRONDEY, H ;
BREVARD, C ;
PAGELOT, A .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1988, (02) :102-103