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Developments of SASS-NMR methods and the spectrometer

Research Project

Project/Area Number 63840015
Research Category

Grant-in-Aid for Developmental Scientific Research

Allocation TypeSingle-year Grants
Research Field 構造化学
Research InstitutionKYOTO UNIVERSITY

Principal Investigator

TERAO Takehiko  Kyoto Univ. Science Professor, 理学部, 教授 (50093274)

Co-Investigator(Kenkyū-buntansha) FUJITO Teruaki  JEOL Co. NMR Group Chief, 理科学機器第2技術部NMG, 主任
NAGAYAMA Kuniaki  JEOL Co. Biology Research Associate, 生体計測学研究室, 室長
NAITO Akira  Kyoto Univ. Science Instructor, 理学部, 助手 (80172245)
Project Period (FY) 1988 – 1989
Project Status Completed (Fiscal Year 1989)
Budget Amount *help
¥13,600,000 (Direct Cost: ¥13,600,000)
Fiscal Year 1989: ¥800,000 (Direct Cost: ¥800,000)
Fiscal Year 1988: ¥12,800,000 (Direct Cost: ¥12,800,000)
KeywordsSASS / powder pattern / chemical shift anisotropy / ferrocene / Powder Pattern / 固体NMR / SASS法
Research Abstract

1.A spectrometer for SASS-NMR was built.
2.Computer programs for execution of SASS-NMR, control of various systems, and data manipulation were made. A simulation program of 1D and 2D powder patterns were also made for the data analysis.
3.SASS-NMR was successfully performed-using a test sample.
4.3D SASS-NMR was developed, which was applied to study small vibrations in calcium formate.
5.lD SASS-NMR techniques for separately obtaining individual powder patterns for chemically distinct nuclei using selective rf irradiation and switching of the spinner axis were proposed, which considerably save time compared with the previous 2D approaches. A method has been applied for simultaneously obtaining all of the C-1 chemical -shift powder patterns in p-diacetylbenzene.
6.The individual powder patterns due to C-13 chemical shift anisotropy in guest ferrocene molecules of , , and cyclodextrin-ferrocene clathrates were separately obtained using SASS-NMR. Enclathrated ferrocene molecules were concluded to undergo C5 rotation. precessio and libration.

Report

(3 results)
  • 1989 Annual Research Report   Final Research Report Summary
  • 1988 Annual Research Report
  • Research Products

    (33 results)

All Other

All Publications (33 results)

  • [Publications] T.Nakai: "Determination of ^<13>C Chemical shift tensor oricntations in cis-and trans-polyacetylene by measurements of two-dimensional NMR powder patterns in rotating solids" Chem.Phys.Lett.145. 90-94 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T.Yamabe: "^<13>C Solid-state NMR Study of polyacenic materials" Phys.Rev.B. 37. 5808-5810 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T.Nakai: "Measurements of two-dimensional NMR powder patterns in rotating solids" J.Chem.Phys. 88. 6049-6058 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] F.Imashiro: "Crystal structure of 1,4,9,10-tetramethyltryptycene and barriers to rotation of bridgehead-methyl groups in 1,4,9,10-tetramethyl-and 1,4-dichloro-9,10-dimethyl-tryptycene" J.Chem.Soc.Perkin.Trans.II. 1401-1408 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] K.Akasaka: "Proton spin-lattice relaxation in a solid protein Streptomyces sibtilisin inhibitor. Enhancement of Segmental motions by adsorbed mater" Canad.J.Chem.66. 2014-2017 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] F.Imashiro: "Study on conformations of n-alkanes in urea inclusion compounds using CH dipolar switching angle sample spinning NMR and MM2 molecular mechanics calculations" J.Chem.Phys.3356-3362 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T.Nakai: "Determination of the ^<13>C Chemical Shift Tensors in Isotactic Polypropylene via the Two-Dimensional Powder Pattern in Ratating Solids" Magn.Reson.Chem. 27. 666-668 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T.Nakai: "Influence of small-amplitude motions on two-dimensional N.M.R.Powder patterns Anisotropic vibrations in calcium formate" Mol.Phys.67. 839-847 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] J.Ashida: "ID NMR separation of overlapping powder patterns by selective rf irradiation and switching-angle spinning" Chem.Phys.Lett submitted.

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] 寺尾武彦: "固体NMRの新しい展開" 化学と工業. 42. 36-40 (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] 寺尾武彦: "高分子における固体二次元NMR" 高分子. 39. 230-233 (1990)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T. Nakai, T. Terao, H. Shirakawa: "Determination of ^<13>C chemical shift tensor orientations in cis and trans polyacetylene by measurements of two-dimensional NMR powder patterns in rotating solids" Chem. Phys. Lett., 145, 90 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T. Yamabe, S. Yamanaka, K. Tanaka, T. Terao, S. Maeda, and S. Yata: "^<13>C solid-state NMR study of polyacenic materials" Phys. Rev. B37, 5808 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T. Nakai, J. Ashida, and T. Terao: "Measurements of two-dimensional NMR powder patterns in rotating solids" J. Chem. Phys., 88, 6049 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] F. Imashiro, K. Hirayama, K. Takegoshi, T. Terao, and A. Saika: "Crystal structure of 1, 4, 9, 10-tetramethyltriptycene and barriers to rotation of bridgehead-methyl groups in 1, 4, 9, 10-tetramethyl- and 1, 4-dichloro-9, 10-dimethyl-triptycene" J. Chem. Soc., Perkin Trans. 2, 1401 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] K. Akasaka, K. Takegoshi, T. Terao, and S. Ganapathy: "Proton spin-lattice relaxation in a solid protein streptomyces subtilisin inhibitor. Enhancement of segmental motions by adsorbed water" Can. J. Chem., 66, 2014 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] G. C. Chingas, C. J. Lee, E. Lippmaa, K. T. Mueller, A. Pines, A. Samoson, B. Q. Sun, D. Suter, and T. Terao: "New angles in sample spinning" Proceeding of the XXIV Congress Ampere, Poznan, 1988, D62 (1988).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] F. Imashiro, D. Kuwabara, T. Nakai, and T. Terao: "Study on conformations of n-alkanes in urea inclusion compounds using CH dipolar switching-angle sample spinning nuclear magnetic resonance and MM2 molecular mechanics calculations" J. Chem. Phys., 90, 3356 (1989).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T. Nakai, J. Ashida, and T. Terao: "Determination of the ^<13>C chemical shift tensors in isotactic polypropylene via the two-dimensional powder pattern in rotating solids" Magn. Reson. Chem., 27, 666 (1989).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T. Nakai, J. Ashida, and T. Terao: "Influence of small-amplitude motions on two-dimensional NMR powder patterns. Anisotropic vibrations in calcium formate" Mol. Phys., 67, 839 (1989).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] K. T. Mueller, B. Q. Sun, G. C. Chingas, J. W. Zwanziger, T. Terao, and A. Pines: "Dynamic-angle spinning of quadrupole nuclei" J. Magn. Reson. in press.

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] "1D NMR separation of overlapping powder patterns by selective rf irradiation and switching-angle spinning" Chem. Phys. Lett.

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1989 Final Research Report Summary
  • [Publications] T.Nakai: "Determination of the ^<13>C Chemical Shift Tensors in Isotactic Polypropylene via the Two-Dimensioral Powder Pattern in Rotating Solids" Magn.Resom.Chem.27. 666-668 (1989)

    • Related Report
      1989 Annual Research Report
  • [Publications] T.Nakai: "Influence of Small-amplitude motions on two-dimensional N.M.R.powder patterns Anisotropic vibrations in calcium formate" Mol Phys. 67. 839-847 (1989)

    • Related Report
      1989 Annual Research Report
  • [Publications] J.Ashida: "ID NMR separation of overlapping powder patterns by selective rf irradiation and switching-angle spinning" Chem.Phys.Lett.

    • Related Report
      1989 Annual Research Report
  • [Publications] 寺尾武彦: "固体NMRの新しい展開" 化学と工業. 42. 36-40 (1989)

    • Related Report
      1989 Annual Research Report
  • [Publications] 寺尾武彦: "高分子における固体二次元NMR" 高分子. 39. 230-233 (1990)

    • Related Report
      1989 Annual Research Report
  • [Publications] T.Nakai: Chem.Phys.Lett.145. 90-94 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] T.Yamabe: Phys.Rev.B. 37. 5808-5810 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] T.Nakai: J.Chem.Phys.88. 6049-6058 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] F.Imashiro: J.Chem.Soc.Perkin.Trans.II. 1401-1408 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] K.Akasaka: Canad.J.Chem.66. 2014-2017 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] F.Imashiro: J.Chem.Phys.(1989)

    • Related Report
      1988 Annual Research Report

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Published: 1988-04-01   Modified: 2016-04-21  

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