Recoupling of chemical-shift anisotropy powder patterns in MAS NMR

被引:15
|
作者
Orr, Robin M. [1 ]
Duer, Melinda J. [1 ]
机构
[1] Univ Cambridge, Dept Chem, Cambridge CB2 1EW, England
基金
英国工程与自然科学研究理事会;
关键词
solid-state NMR; magic-angle spinning; chemical-shift anisotropy; recoupling;
D O I
10.1016/j.jmr.2006.03.010
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A comparison of three different implementations of the chemical-shift recoupling experiment of Tycko et at. [R. Tycko, G. Dabbagh, P.A. Mirau, Determination of chemical-shift-anisotropy lineshapes in a two-dimensional magic-angle-spinning NMR experiment, J. Magn. Reson. 85 (1989) 265-274] is presented. The methods seek to reduce the effects of artefacts resulting from pulse imperfections and residual C-H dipolar coupling in organic solids. An optimised and constant time implementation are shown to give well-defined and artefact free powder pattern lineshapes in the indirectly observed dimension for both sp(2) and sp(3) carbon sites. Experimental setup is no more demanding than for the original experiment, and can be implemented using standard commercial hardware. (c) 2006 Elsevier Inc. All rights reserved.
引用
收藏
页码:1 / 8
页数:8
相关论文
共 50 条
  • [1] The effects of chemical-shift anisotropy on deuterium powder patterns
    DiNatale, JA
    Vold, RR
    [J]. JOURNAL OF MAGNETIC RESONANCE SERIES A, 1995, 117 (02) : 304 - 306
  • [2] Effect of proton chemical-shift anisotropy on double-quantum MAS NMR sideband patterns
    Tekely, P
    Demco, DE
    Canet, D
    Malveau, C
    [J]. CHEMICAL PHYSICS LETTERS, 1999, 309 (1-2) : 101 - 110
  • [3] CALCULATION OF CHEMICAL-SHIFT ANISOTROPY IN NMR
    SCHMIEDER, H
    [J]. PHYSICA STATUS SOLIDI B-BASIC RESEARCH, 1975, 67 (01): : K27 - K29
  • [4] CHEMICAL-SHIFT ANISOTROPY IN POWDERED SOLIDS STUDIED BY 2D FT CP MAS NMR
    BAX, A
    SZEVERENYI, NM
    MACIEL, GE
    [J]. JOURNAL OF MAGNETIC RESONANCE, 1983, 51 (03) : 400 - 408
  • [5] A NOVEL METHOD TO DETERMINE THE PRINCIPAL VALUES OF A CHEMICAL-SHIFT TENSOR FROM MAS NMR POWDER SPECTRA
    FENZKE, D
    MAESS, B
    PFEIFER, H
    [J]. JOURNAL OF MAGNETIC RESONANCE, 1990, 88 (01): : 172 - 176
  • [6] C-13-NMR CHEMICAL-SHIFT ANISOTROPY OF ACETYLENE
    ENGLERT, G
    [J]. ZEITSCHRIFT FUR NATURFORSCHUNG PART A-ASTROPHYSIK PHYSIK UND PHYSIKALISCHE CHEMIE, 1972, A 27 (10): : 1536 - &
  • [7] CHEMICAL-SHIFT ANISOTROPY RELAXATION IN RH-103 NMR
    SOCOL, SM
    MEEK, DW
    [J]. INORGANICA CHIMICA ACTA-ARTICLES AND LETTERS, 1985, 101 (03): : L45 - L46
  • [8] A robust technique for two-dimensional separation of undistorted chemical-shift anisotropy powder patterns in magic-angle-spinning NMR
    Liu, SF
    Mao, JD
    Schmidt-Rohr, K
    [J]. JOURNAL OF MAGNETIC RESONANCE, 2002, 155 (01) : 15 - 28
  • [9] INDUCED CHEMICAL-SHIFT ANISOTROPY
    FUJIWARA, FY
    REEVES, LW
    [J]. MOLECULAR PHYSICS, 1978, 36 (06) : 1897 - 1900
  • [10] DETERMINATION OF NUCLEAR DISTANCES AND CHEMICAL-SHIFT ANISOTROPY FROM H-1 MAS NMR SIDE-BAND PATTERNS OF SURFACE OH GROUPS
    FENZKE, D
    HUNGER, M
    PFEIFER, H
    [J]. JOURNAL OF MAGNETIC RESONANCE, 1991, 95 (03): : 477 - 483