Rotational resonance NMR of 13C2-labelled retinal:: quantitative internuclear distance determination

被引:17
|
作者
Feng, X
Verdegem, PJE
Lee, YK
Helmle, M
Shekar, SC
de Groot, HJM
Lugtenburg, J
Levitt, MH [1 ]
机构
[1] Univ Stockholm, Arrhenius Lab, Div Phys Chem, S-10691 Stockholm, Sweden
[2] Leiden Univ, Leiden Inst Chem, Gorlaeus Labs, NL-2300 RA Leiden, Netherlands
关键词
rotational resonance NMR; internuclear distance; C-13(2)-labelled retinal;
D O I
10.1016/S0926-2040(99)00019-3
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
Rotational resonance phenomena are investigated in the solid-state magic-angle spinning NMR of all-E-[11,20-C-13(2)]-retinal at a magnetic field of 4.7 T. We find good agreement between experiments and numerical simulations for the rotational resonance spectral peakshapes and for the rotor-driven magnetization exchange. The internuclear distance between the C-13-labelled C11 and C20 sites is determined to be 0.301 +/- 0.008 nm (from rotational resonance spectra) and 0.300 +/- 0.010 nm (from rotor-driven magnetization exchange), in agreement with the X-ray crystallographic distance of 0.296 nm. We show rotational resonance spectra which display perturbations from intermolecular homonuclear spin-spin interactions. (C) 1999 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:81 / 90
页数:10
相关论文
共 50 条
  • [1] INTERNUCLEAR DISTANCE MEASUREMENTS IN MEMBRANES USING ROTATIONAL RESONANCE NMR
    SMITH, SO
    BIOPHYSICAL JOURNAL, 1994, 66 (02) : A348 - A348
  • [2] Syntheses of 13C2-labelled 11Z-retinals
    McLean, Neville J.
    Gansmuller, Axel
    Concistre, Maria
    Brown, Lynda J.
    Levitt, Malcom H.
    Brown, Richard C. D.
    TETRAHEDRON, 2011, 67 (43) : 8404 - 8410
  • [3] INTERNUCLEAR DISTANCE MEASUREMENT IN A REACTION INTERMEDIATE - SOLID-STATE C-13 NMR ROTATIONAL RESONANCE DETERMINATION OF THE SCHIFF-BASE CONFIGURATION IN THE M-PHOTOINTERMEDIATE OF BACTERIORHODOPSIN
    LAKSHMI, KV
    AUGER, M
    RAAP, J
    LUGTENBURG, J
    GRIFFIN, RG
    HERZFELD, J
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1993, 115 (18) : 8515 - 8516
  • [4] DETERMINATION OF C-N INTERNUCLEAR DISTANCES BY ROTATIONAL-ECHO DOUBLE-RESONANCE NMR OF SOLIDS
    PAN, Y
    GULLION, T
    SCHAEFER, J
    JOURNAL OF MAGNETIC RESONANCE, 1990, 90 (02): : 330 - 340
  • [5] Internuclear distance measurements up to 0.44 nm for retinals in the solid state with 1-D rotational resonance C-13 MAS NMR spectroscopy
    Verdegem, PJE
    Helmle, M
    Lugtenburg, J
    deGroot, HJM
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1997, 119 (01) : 169 - 174
  • [6] Internuclear distance measurements up to 0.44 nm for retinals in the solid state with 1-D rotational resonance 13C MAS NMR spectroscopy
    Verdegem, P.J.E.
    Helmle, M.
    Lugtenbu, J.
    Groot, H.J.M.
    Journal of the American Chemical Society, 1997, 119 (01):
  • [7] DETERMINATION OF INTERNUCLEAR DISTANCES AND THE ORIENTATION OF FUNCTIONAL-GROUPS BY SOLID-STATE NMR - ROTATIONAL RESONANCE STUDY OF THE CONFORMATION OF RETINAL IN BACTERIORHODOPSIN
    MCDERMOTT, AE
    CREUZET, F
    GEBHARD, R
    VANDERHOEF, K
    LEVITT, MH
    HERZFELD, J
    LUGTENBURG, J
    GRIFFIN, RG
    BIOCHEMISTRY, 1994, 33 (20) : 6129 - 6136
  • [8] Determination of internuclear distances in uniformly labeled molecules by rotational-resonance solid-state NMR
    Williamson, PTF
    Verhoeven, A
    Ernst, M
    Meier, BH
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (09) : 2718 - 2722
  • [10] 13C-13C correlations and internuclear distance measurements with 2D-MELODRAMA
    Jarrell, HC
    Lu, DL
    Siminovitch, DJ
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (40) : 10453 - 10462