THE 2D QUADSHIFT EXPERIMENT - SEPARATION OF DEUTERIUM CHEMICAL-SHIFTS AND QUADRUPOLAR COUPLINGS BY 2-DIMENSIONAL SOLID-STATE MAS NMR-SPECTROSCOPY

被引:12
作者
CHANDRAKUMAR, N [1 ]
VONFIRCKS, G [1 ]
GUNTHER, H [1 ]
机构
[1] CSIR,CENT LEATHER RES INST,CHEM PHYS LAB,MADRAS 600020,TAMIL NADU,INDIA
关键词
NMR; H-2; SOLID-STATE MAS H-2 NMR; 2D MAS H-2 NMR; DEUTERIUM CHEMICAL SHIFT; QUADRUPOLAR COUPLING;
D O I
10.1002/mrc.1260320710
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The two-dimensional QUADSHIFT experiment is introduced, which permits the separation of chemical shifts and quadrupolar couplings in solid-state magic angle spinning MMR spectra of powder samples. The technique was applied to partially deuteriated norcamphor and camphor under slow magic angle spinning. Double quantum chemical shift resolutions down to 0.2 ppm were achieved, with double quantum linewidths in the range 6-12 Hz. Separation and correlation of deuterium chemical shifts and quadrupolar couplings is demonstrated for individual sites.
引用
收藏
页码:433 / 435
页数:3
相关论文
共 21 条
[11]   APPLICATION OF PHASE SENSITIVE TWO-DIMENSIONAL CORRELATED SPECTROSCOPY (COSY) FOR MEASUREMENTS OF H-1-H-1 SPIN-SPIN COUPLING-CONSTANTS IN PROTEINS [J].
MARION, D ;
WUTHRICH, K .
BIOCHEMICAL AND BIOPHYSICAL RESEARCH COMMUNICATIONS, 1983, 113 (03) :967-974
[12]   COMPLETE PROTON NUCLEAR MAGNETIC-RESONANCE ANALYSIS OF NORCAMPHOR [J].
MARSHALL, JL ;
WALTER, SR .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1974, 96 (20) :6358-6362
[13]   DEUTERON CHEMICAL-SHIFT AND EFG TENSORS IN ALPHA-GLYCINE [J].
MULLER, C ;
SCHAJOR, W ;
ZIMMERMANN, H ;
HAEBERLEN, U .
JOURNAL OF MAGNETIC RESONANCE, 1984, 56 (02) :235-246
[14]   DOUBLE QUANTUM CROSS POLARIZATION VIA DIPOLAR ORDER [J].
REINHOLD, M ;
BRUNNER, P ;
ERNST, RR .
JOURNAL OF CHEMICAL PHYSICS, 1981, 74 (01) :184-188
[15]   STRUCTURE AND DYNAMICS OF SOLID POLYMERS FROM 2D-NMR AND 3D-NMR [J].
SPIESS, HW .
CHEMICAL REVIEWS, 1991, 91 (07) :1321-1338
[16]   HIGH-RESOLUTION, SLOW-SPINNING MAGIC-ANGLE C-13 NMR [J].
STEJSKAL, EO ;
SCHAEFER, J ;
MCKAY, RA .
JOURNAL OF MAGNETIC RESONANCE, 1977, 25 (03) :569-573
[17]   DOUBLE-QUANTUM CROSS-POLARIZATION NMR IN SOLIDS [J].
VEGA, S ;
SHATTUCK, TW ;
PINES, A .
PHYSICAL REVIEW A, 1980, 22 (02) :638-661
[18]   FOURIER-TRANSFORM DOUBLE-QUANTUM NMR IN SOLIDS [J].
VEGA, S ;
SHATTUCK, TW ;
PINES, A .
PHYSICAL REVIEW LETTERS, 1976, 37 (01) :43-46
[19]   DEUTERIUM NMR-STUDY OF ORIENTATIONAL ORDER IN CAMPHOR [J].
WASYLISHEN, RE ;
PETTITT, BA ;
LEWIS, JS .
CHEMICAL PHYSICS LETTERS, 1979, 67 (2-3) :459-462
[20]  
WIMPERIS S, 1993, J MAGN RESON, V102, P305