Long-range 1H-15N heteronuclear shift correlation at natural abundance

被引:169
作者
Martin, GE [1 ]
Hadden, CE [1 ]
机构
[1] Pharmacia & Upjohn Inc, Pharmaceut Dev, Rapid Struct Characterizat Grp, Kalamazoo, MI 49001 USA
来源
JOURNAL OF NATURAL PRODUCTS | 2000年 / 63卷 / 04期
关键词
D O I
10.1021/np9903191
中图分类号
Q94 [植物学];
学科分类号
071001 ;
摘要
Despite the inherently low sensitivity of N-15 NMR because of its low gyromagnetic ratio (gamma(N)) and its relatively low natural abundance (0.37%), this important nuclide still has useful potential as a structural probe even at natural abundance. Inverse-detected NMR methods coupled with major advances in NMR probe designs have made it possible to acquire long-range H-1-N-15 heteronuclear shift correlation data on samples as small as a micromole overnight. Chemical shift, referencing schemes for N-15 and the range of N-15 shifts are discussed, followed by a discussion of the currently available pulse sequences, pulse calibration, parametrization and processing of long-range H-1-N-15 data, and the implications of probe selection. These topics are followed by a review of the applications contained in the literature that have utilized H-1-N-15 heteronuclear shift correlation experiments at natural abundance, with emphasis placed on the observed long-range coupling pathways.
引用
收藏
页码:543 / 585
页数:43
相关论文
共 168 条
[1]   MOLECULAR MODELING, NMR-SPECTROSCOPY, AND CONFORMATIONAL-ANALYSIS OF 3',4'-ANHYDROVINBLASTINE [J].
ANDREWS, CW ;
WISOWATY, J ;
DAVIS, AO ;
CROUCH, RC ;
MARTIN, GE .
JOURNAL OF HETEROCYCLIC CHEMISTRY, 1995, 32 (03) :1011-1017
[2]   Amphistin, a new melanogenesis inhibitor, produced by an actinomycete [J].
Arai, N ;
Shiomi, K ;
Takamatsu, S ;
Komiyama, K ;
Shinose, M ;
Takahashi, Y ;
Tanaka, Y ;
Iwai, Y ;
Liu, JR ;
Omura, S .
JOURNAL OF ANTIBIOTICS, 1997, 50 (10) :808-814
[3]   PHASE SEPARATION IN 2-DIMENSIONAL SPECTROSCOPY [J].
BACHMANN, P ;
AUE, WP ;
MULLER, L ;
ERNST, RR .
JOURNAL OF MAGNETIC RESONANCE, 1977, 28 (01) :29-39
[4]   PULSED FIELD GRADIENTS IN NMR - AN ALTERNATIVE TO PHASE CYCLING [J].
BARKER, P ;
FREEMAN, R .
JOURNAL OF MAGNETIC RESONANCE, 1985, 64 (02) :334-338
[5]   SEPARATION OF THE DIFFERENT ORDERS OF NMR MULTIPLE-QUANTUM TRANSITIONS BY THE USE OF PULSED FIELD GRADIENTS [J].
BAX, A ;
DEJONG, PG ;
MEHLKOPF, AF ;
SMIDT, J .
CHEMICAL PHYSICS LETTERS, 1980, 69 (03) :567-570
[6]   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
[7]   H-1 AND C-13 ASSIGNMENTS FROM SENSITIVITY-ENHANCED DETECTION OF HETERONUCLEAR MULTIPLE-BOND CONNECTIVITY BY 2D MULTIPLE QUANTUM NMR [J].
BAX, A ;
SUMMERS, MF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1986, 108 (08) :2093-2094
[8]   SENSITIVITY-ENHANCED TWO-DIMENSIONAL HETERONUCLEAR SHIFT CORRELATION NMR-SPECTROSCOPY [J].
BAX, A ;
SUBRAMANIAN, S .
JOURNAL OF MAGNETIC RESONANCE, 1986, 67 (03) :565-569
[9]   OPTIMIZED RECORDING OF HETERONUCLEAR MULTIDIMENSIONAL NMR-SPECTRA USING PULSED FIELD GRADIENTS [J].
BAX, A ;
POCHAPSKY, SS .
JOURNAL OF MAGNETIC RESONANCE, 1992, 99 (03) :638-643
[10]   IMPROVED RESOLUTION AND SENSITIVITY IN H-1-DETECTED HETERONUCLEAR MULTIPLE-BOND CORRELATION SPECTROSCOPY [J].
BAX, A ;
MARION, D .
JOURNAL OF MAGNETIC RESONANCE, 1988, 78 (01) :186-191