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Determination of structure and dynamics of liquid crystalline molecules by state-correlated 2D NMR spectroscopy

Research Project

Project/Area Number 03640405
Research Category

Grant-in-Aid for General Scientific Research (C)

Allocation TypeSingle-year Grants
Research Field 物理化学一般
Research InstitutionHIMEJI INSTITUTE OF TECHNOLOGY

Principal Investigator

NAITO Akira  Himeji Institute of Technology, Science, Associate Professor, 理学部, 助教授 (80172245)

Co-Investigator(Kenkyū-buntansha) AKASAKA Kazuyuki  Kobe University, Science, Professor, 理学部, 教授 (50025368)
SAITO Hazime  Himeji Institute of Technology, Science, Professor, 理学部, 教授 (30100150)
Project Period (FY) 1991 – 1992
Project Status Completed (Fiscal Year 1992)
Budget Amount *help
¥1,900,000 (Direct Cost: ¥1,900,000)
Fiscal Year 1992: ¥200,000 (Direct Cost: ¥200,000)
Fiscal Year 1991: ¥1,700,000 (Direct Cost: ¥1,700,000)
Keywords2D NMR / liquid crystal / microwave / temperature jump NMR / phase transition / dipolar pattern / 双極子パタ-ン
Research Abstract

A novel two dimensional NMR experiment, state-correlated 2D NMR, were applied in liquid crystalline samples to investigate the structure and the dynamics of the liquid crystalline molecules. In the first year, the microwave part of the NMR probe head was modified to improve the efficiency of temperature jump. As a results, we have succeeded to obtain nematic-isotropic phase correlated 2D NMR spectra of 4'-methoxybenzylidene-4-acetoxyaniline(APAPA) and 4'-ethoxybenzylidene-4-n-butylaniline(EBBA). In the second year, we have focused attention on investigating the structure and dynamics of liquid crystalline molecules and obtained the following results.
1. Phase transition from nematic to isotropic phase was completed within 10 msec so that the dipolar patterns for individual protons in APAPA were separately observed.
2. A triplet pattern with the intensity ratio of 1 : 2 : 1 was observed for the alpha methyl protons. This fact indicates the presence of three protons with equal value of dipolar couplings. A doublet pattern was clearly seen for 2,6 and 3,5 aromatic protons with a splitting frequency of 9.7 kHz and the order parameter was determined to be 0.41 for APAPA.
3. A mixing of the cross sections due to the spin exchange effects was observed. We found that spin exchange occurs more efficiently within the aromatic ring, which is considered to be a core group of the liquid crystal molecule, than between the aromatic and alpha methyl protons.
4. Spectral analysis could be performed for a subspin system with a small number of spins rather than the entire spin system.
5. Phase transition from nematic to isotropic phase was completed within 5 msec for EBBA by using a sample tube of 3 mm diameter and the dipolar splittings for the individual protons of the butyl group were separately determined.

Report

(3 results)
  • 1992 Annual Research Report   Final Research Report Summary
  • 1991 Annual Research Report
  • Research Products

    (15 results)

All Other

All Publications (15 results)

  • [Publications] Akira Naito: "Separation of Local Magnetic Fields of Individual protous in Nematic Phase by State-correlated 2D NMR Spectroscopy" J.Mogn.Reson.92. 85-93 (1991)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Kazuyuki Akasaka: "Novel Method for NMR Spectral Correlation betneen the Native and Denatured States of a Protein.Application to Ribonnclease A" J.Am.Chem.Soc.113. 4688-4689 (1991)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Satoru Tuzi: "A High-rosolution Solid-state 13C-NMR Studey on crystalline Bovine Heart Crychrome-C Oxidase and Lysozyme Dynamic Behavior of Protein and and Detergent in the Complex." Em.J.Biochem.208. 713-720 (1992)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Kazumi Akasaka: "Temperature-jump NMR study of protein folding:Ribonndease A at low pH" J.Biomolec.NMR. 1. 65-70 (1991)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Akira Naito: "Combinod sample rotation and mulfiple-pmlse NMR spectroscopic studies on protons bonded to 14N nuclei in solid Amino acids." J.Phys.Chem.95. 3578-3581 (1991)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Akira Naito: "Separation of local magnetic fields of individual protons in nematic phase by state-correlated 2D NMR spectroscopy." J.Magn.Reson.92. 85-93 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Kazuyuki Akasaka: "Novel method for NMR spectral correlation between the native and denatured states of a protein. Application to ribonuclease A." J.Am.Chem.Soc.113. 4688-4689 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Akira Naito: "Combined sample rotation and multiplepulse NMR spectroscopic studies on protons bonded to ^<14>N nuclei in solid amino acids." J.Phys.Chem.95. 3578-3581 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Kazuyuki Akasaka: "Temperature-jump NMR study of protein folding : Ribonuclease A at low pH." J.Biomolec.NMR. 1. 65-70 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Satoru Tuzi: "A high-resolution solid-state ^<13>C NMR spectroscopic study on crystalline bovine heart cytochrome-c oxidase and lysozyme. Dynamic behavior of protein and detergent in the complex." Eur.J.Biochem.208. 713-720 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1992 Final Research Report Summary
  • [Publications] Akira Naito: "Separation of Local Magnetic Fields of Individual protons in Nematic Phase by State-correlated 2D NMR Spectroscopy" J.Magn.Reson.92. 85-93 (1991)

    • Related Report
      1992 Annual Research Report
  • [Publications] Kazuyuki Akasaka: "Novel Method for NMR Spectral Correlation between the Native and Denaturated States of a Protein.Application to Ribonnclease A" J.Am.Chem.Soc.113. 4688-4689 (1991)

    • Related Report
      1992 Annual Research Report
  • [Publications] Satoru Tuzi: "A High-resolution Solid-state ^<13>C-NMR Study on Crystallire Bovine Heart Cytochrome-C oxidase and Lysozyme Dynamic Behavior of Protein and Detegent in the Complex" Eur.J.Biochem.208. 713-720 (1992)

    • Related Report
      1992 Annual Research Report
  • [Publications] Akira Naito: "Separation of Local Magnetic Fields of Individual in Nematic Phase by StateーCorrelated 2D NMR Spectroscopy" J.Magn.Reson.92. 85-93 (1991)

    • Related Report
      1991 Annual Research Report
  • [Publications] Kazuyuki Akasaka: "Novel Method for NMR Spectral Correlation between the Native and the Denatured States of a Protein.Application to Ribonuclease A" J.Am.Chem.Soc.113. 4688-4689 (1991)

    • Related Report
      1991 Annual Research Report

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Published: 1991-04-01   Modified: 2016-04-21  

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