Through-bond connectivity in solids by continuous-wave spin lock

被引:4
作者
Hartmann, P
Zwanziger, JW
Jäger, C
机构
[1] Univ Jena, Inst Opt & Quantenelekt, D-07743 Jena, Germany
[2] Indiana Univ, Dept Chem, Bloomington, IN 47505 USA
基金
美国国家科学基金会;
关键词
P-31 solid state NMR; 2D correlation experiment; through-bond connectivity; J-coupling; cw spin locking;
D O I
10.1016/S0926-2040(00)00074-6
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
A simple two-dimensional correlation experiment that enables determination of through-bond connectivity in the solid state is described. The experiment is performed under fast magic angle spinning (MAS) conditions. After the initial pi/2 pulse, the magnetization develops freely under the MAS Hamiltonian. The t(1)-period is followed by a strong spin locking pulse used as mixing period. The dipolar coupling is averaged out by magic angle spinning, and the chemical shifts and r.f.-offsets are scaled by the applied spin locking field. Hence, for strong locking conditions, the isotropic J-coupling is the dominant interaction. The mixing Hamiltonian is thus identical to the well-known TOCSY-Hamiltonian, resulting in a net through-bond magnetization transfer. The mixing-time dependence of the exchange rates is investigated. Applications to crystalline P4S7 and MgP4O11 are shown. (C) 2000 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:189 / 197
页数:9
相关论文
共 39 条
[1]   Local structure and connectivity in lithium phosphate glasses:: a solid-state 31P MAS NMR and 2D exchange investigation [J].
Alam, TM ;
Brow, RK .
JOURNAL OF NON-CRYSTALLINE SOLIDS, 1998, 223 (1-2) :1-20
[2]   2-DIMENSIONAL SPECTROSCOPY - APPLICATION TO NUCLEAR MAGNETIC-RESONANCE [J].
AUE, WP ;
BARTHOLDI, E ;
ERNST, RR .
JOURNAL OF CHEMICAL PHYSICS, 1976, 64 (05) :2229-2246
[3]   Total correlation spectroscopy in the solid state. The use of scalar couplings to determine the through-bond connectivity [J].
Baldus, M ;
Meier, BH .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1996, 121 (01) :65-69
[4]   BROAD-BAND POLARIZATION-TRANSFER EXPERIMENTS FOR ROTATING SOLIDS [J].
BALDUS, M ;
TOMASELLI, M ;
MEIER, BH ;
ERNST, RR .
CHEMICAL PHYSICS LETTERS, 1994, 230 (4-5) :329-336
[5]   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
[6]  
BENETT AE, 1982, J CHEM PHYS, V96, P8624
[7]  
BENNETT AE, 1994, NMR BASIC PRINCIPLES, V33
[8]  
BJORHOLM T, 1988, CHEM PHYS LETT, V3, P259
[9]   Phase sensitive detection of 2D homonuclear correlation spectra in MAS NMR [J].
Boender, GJ ;
Vega, S .
JOURNAL OF MAGNETIC RESONANCE, 1998, 133 (02) :281-285
[10]  
BORN R, 1995, Z NATURFORSCH A, V50, P169