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
  • [41] 13C-1H dipolar-assisted rotational resonance in magic-angle spinning NMR
    Takegoshi, K
    Nakamura, S
    Terao, T
    CHEMICAL PHYSICS LETTERS, 2001, 344 (5-6) : 631 - 637
  • [42] Preparation and C-13 NMR spectroscopy of C-13-1 labelled 2,2-diaryl-1-fluoro-1-lithioalkenes
    Pelter, A
    Kvicala, J
    TETRAHEDRON LETTERS, 1997, 38 (27) : 4877 - 4880
  • [43] Identification and Quantitative Determination of Lignans in Cedrus atlantica Resins using 13C NMR Spectroscopy
    Nam, Anne-Marie
    Paoli, Mathieu
    Castola, Vincent
    Casanova, Joseph
    Bighelli, Ange
    NATURAL PRODUCT COMMUNICATIONS, 2011, 6 (03) : 379 - 385
  • [44] Rapid quantitative determination by 13C NMR of the composition of acetylglycerol mixtures as byproduct in biodiesel synthesis
    Casas, Abraham
    Jesus Ramos, Maria
    Perez, Angel
    Simon, Adolfo
    Lucas-Torres, Covadonga
    Moreno, Andres
    FUEL, 2012, 92 (01) : 180 - 186
  • [45] DETERMINATION OF FUNCTIONALITY AND FUNCTIONALITY DISTRIBUTION OF POLYETHER POLYOLS BY QUANTITATIVE C-13 NMR-SPECTROSCOPY
    CARR, RH
    HERNALSTEEN, J
    DEVOS, J
    JOURNAL OF APPLIED POLYMER SCIENCE, 1994, 52 (08) : 1015 - 1022
  • [46] Identification and quantitative determination of carbohydrate molecules in Greek honey by employing 13C NMR spectroscopy
    Kazalaki, Aristea
    Misiak, Maria
    Spyros, Apostolos
    Dais, Photis
    ANALYTICAL METHODS, 2015, 7 (14) : 5962 - 5972
  • [47] Identification and Quantitative Determination of Dipropylene Glycol in Terpene Mixtures Using 13C NMR Spectroscopy
    Ottavioli, Josephine
    Casanova, Joseph
    Bighelli, Ange
    SPECTROSCOPY LETTERS, 2011, 44 (03) : 221 - 228
  • [48] Triad sequence determination of ethylene-propylene copolymers - application of quantitative 13C NMR
    Singh, Gurmeet
    Kothari, Ajay V.
    Gupta, Virendra K.
    POLYMER TESTING, 2009, 28 (05) : 475 - 479
  • [49] A theoretical perspective on the accuracy of rotational resonance (R2)-based distance measurements in solid-state NMR
    Pandey, Manoj Kumar
    Ramachandran, Ramesh
    MOLECULAR PHYSICS, 2010, 108 (05) : 619 - 635
  • [50] In situ analysis of [8-13C-7-15N]-double-labelled theophylline by a triple resonance NMR technique
    Yamaguchi, Koya
    Ueki, Ryosuke
    Yamada, Hisatsugu
    Aoyama, Yasuhiro
    Nonaka, Hiroshi
    Sando, Shinsuke
    ANALYTICAL METHODS, 2011, 3 (07) : 1664 - 1666