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Development of A Loop-Gap Resonator For Pulse ESR At Very Low-Temperature

Research Project

Project/Area Number 09554041
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section展開研究
Research Field Inorganic chemistry
Research InstitutionKinki University

Principal Investigator

MUNAKATA Megumu  KINKI UNIVERSITY,DEPATMENT OF CHEMISTRY,PROFESSOR, 理工学部, 教授 (80090942)

Co-Investigator(Kenkyū-buntansha) MIZUTA Satio  日本電子(株), ESR応用研究室, 主任
FUJII Kanae  日本電子(株), ESRグループ, グループ長
KURODA Takayosi (SOWA Tak)  近畿大学, 理工学部, 講師 (80257964)
Project Period (FY) 1997 – 1998
Project Status Completed (Fiscal Year 1998)
Budget Amount *help
¥5,600,000 (Direct Cost: ¥5,600,000)
Fiscal Year 1998: ¥2,000,000 (Direct Cost: ¥2,000,000)
Fiscal Year 1997: ¥3,600,000 (Direct Cost: ¥3,600,000)
Keywordsdevelopment of pulse resonator / pulse ESR / multi-nuclear complex / structure analysis / N-14 ESEEM / 核変調構造 / 誘電体型共振器 / 多核遷移金属錯体 / 3核パラジウム錯体
Research Abstract

We have carried out a development of a new type of resonator for pulse ESR at very low-temperature. We have also accomplished syntheses and characterization of a series of novel multi-nuclear transition metal compounds.
The resonator we have developed is a loop-gap type which can focus a microwave magnetic field in high density at the sample position. It can be assembled into a liquidhelium temperature controller which has been used for conventional F,SR, which enables to control sample temperature from room temperature to 2.7 K with an accuracy of less than 0.1 K.This means we can control a relaxation time of an electron spin in a radical complex. For the connection between a resonator and a microwave circuit, we adopted a Gordon-type coupler which can widely adjust coupling. By using this coupler a resonator can be overcoupled and the dead time after an irradiation of a microwave pulse could be reducedappreciably.
As for syntheses of multi-nuclear transition-metal compounds, we chose N … More i(mnt)_2 derivatives which are known to be active for ^<14>N ESEEM.We succeeded in syntheses and structural characterizations of a series of novel compounds with formula A_2[M(mnt)_2(Cu_4X_4)] (A = Na, TBA ; M = Ni, Pd, Pt ; X= I, Br). Each compound contains a Ni(mnt)_2 moiety which retains the original planar structure and there is no significant change in Ni-S bond lengths compared to those of the parent compound. One side of the Ni(mnt)_2 moiety is covered with an eight-membered ring of Cu_4I_4 with copper atoms being close to the mnt sulfur atoms (Cu-S = 2.35 A in average). Depending on counter cations, the connection of dianionic [M(mnt)_2(Cu_4X_4)] part can be varied from a discrete molecule with A = Na(18-crown-6), one-dimensional chain with A = TBA, and to two-dimensional sheet with A = Na. Among these compounds, the one with A = Na(18-crown-6), M = Ni, and X= I shows strong ESR signal. The ESEEM measurements on this paramagnetic salt was conducted using the above-mentioned resonator and we could observe ^<14>N ESEEM clearly. Less

Report

(3 results)
  • 1998 Annual Research Report   Final Research Report Summary
  • 1997 Annual Research Report
  • Research Products

    (26 results)

All Other

All Publications (26 results)

  • [Publications] 宗像 恵: "Construction of Metal Sandwich Systems Derived from Assembly of Silver(I) Complexes with Polymeric Aromatic Compounds" J. Am. Chem. Soc.(1999 印刷中)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Supramolecular Silver(I) Complexes with Highly Strained Polycyclic Aromatic Compounds" J. Am. Chem. Soc.120・34. 8610-8618 (1998)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Construction of Copper(I) Coordination Polymers of 1, 2, 4, 5- Tetracyanobenzene with Zigzag Sheet and Porous Frameworks" Inorg. Chem.37・21. 5651-5656 (1998)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Structural Control of Copper(I) Coordination Polymers : Construction of One, Two and Three-Dimensional Frameworks..." Inorg. Chem.36・27. 6382-6389 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Two Types of New Polymeric Copper(I) Complexes of Pyrazinecarboxamide Having Channel and Helix Structures" Inorg. Chem.36・23. 5416-5418 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Construction and Conductivity of W-Type Sandwich Silver(I) Polymers with Pyrene and Perylene" Inorg. Chem.36・21. 4903-4905 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 恵: "Adv. Inorg. Chem." Academic Press, 173-303 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, G.L.Ning, T.Kuroda-Sowa, M.Maekawa, Y.Suenaga, and N.Maeno.: "Construction of Metal Sandwich Systems Derived from Assembly of Silver (I) Complexes with Polymeric Aromatic Compounds" J.Am.Chem.Soc.(in press). (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, and T.Kuroda-Sowa.: "Towards the Construction of Functional Solid-State Supramolecular Metal Complexes Containing Copper (I) and Silver (I)" Adv.Inorg.Chem.46. 173-303 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, T.Kuroda-Sowa'M.Maekawa, Y.Suenaga, K.Moriwaki, and I.Ino.: "Open Dimeric and Closed Polymeric Container Molecules : Calixarene Complexes of Ag (I) Coordinated by Upper-rim Carbon Atoms" J.Am.Chem.Soc., Dalton Trans. 3. 373-378 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, T.Kuroda-Sowa M.Maekawa, Y.Suenaga, G.L.Ning , and T.Kojima.: "Supramolecular Silver (I) Complexes with Highly Strained Polycyclic Aromatic Compounds" J.Am.Chem.Soc.120・34. 8610-8618 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, G.L.Ning, T.Kuroda-Sowa M.Maekawa, Y.Suenaga, and T.Horino.: "Construction of Copper (I) Coordination Polymers of 1,2,4,5-Tetracyanobenzene with Zigzag Sheet and Porous Frameworks" Inorg.Chem.37・21. 5651-5656 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, H.He, T.Kuroda-Sowa M.Maekawa, Y.Suenaga.: "Dicopper Complexes Derived from 4-Amino-2,1,3-benzothiadiazole with Versatile Coordination Number and Geometry" J.Am.Chem.Soc., Dalton Trans. 499-1502 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Y.Suenaga, S.G.Yan, L.P.Wu, I.Ino, T.Kuroda-Sowa, M.Maekawa, and M.Munakata: "Self-assembly of Copper (I) and Silver (I) Complexes with Square Grid and Channel Structures" J.Am.Chem.Soc., Dalton Trans. 121-1125 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] T.Kuroda-Sowa, T.Horino, M.Yamamoto, Y.Ohno, M.Maekawa, and M.Munakata: "Structural Control of Copper (I) Coordination Polymers : Construction of One, Two and Three-Dimensional Frameworks of Tetrahedral Copper (I) Ions Bridged by Dicyanobenzene derivatives" Inorg.Chem.36・27. 6382-6389 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, T.Kuroda-Sowa, M.Maekawa, K.Moriwaki, and S.Kitagawa.: "Two Types of New Polymeric Copper (I) Complexes of Pyrazinecarboxamide Having Channel and Helix Structures" Inorg.Chem.36・23. 5416-5418 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, L.P.Wu, T.Kuroda-Sowa, M.Maekawa, Y.Suenaga, and K.Sugimoto.: "Construction and Conductivity of W-Type Sandwich Silver (I) Polymers with Pyrene and Perylene" Inorg.Chem.36・21. 4903-4905 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] M.Munakata, S.G.Yan, T.Kuroda-Sowa, M.Maekawa, M.Akiyama, and S.Kitagawa: "The Solid and Solution Structures of Ternary Gold (I) Complexes with Triphenylphosphine and N-Ligands" J.Am.Chem.Soc., Dalton Trans. 22. 4257-4262 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] 宗像 惠: "Construction of Copper(I)Coordination Polymers of 1,2,4,5-Tetracyanobenzene with Zigzag Sheet and Porous Frameworks" Inorg.Chem.37・21. 5651-5656 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像 惠: "S・・・・S Contact-assembled Tetrathiafulvalene Derivatives of COpper and Siver(I)Coordination Polymers and Organic Radical Cation Salt." J.Chem.Soc.,Dalton Trans.・19. 3255-3261 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像 惠: "Supramolecular Silver(I)Complexes with Highly Strained Polycyclic Aromatic Compounds" J.Am.Chem.Soc.120・34. 8610-8618 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像 惠: "Dicopper Complexes Derived from 4-Amino-2,1,3-benzothiadiazole with Versatile Coordination Number and Geometry" J.Chem.Soc.,Dalton Trans.・9. 1499-1502 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像 惠: "Self-assembly of Copper(I)and Silver(I)Complexes with Square Grid and Channel Structures." J.Chem.Soc.,Dalton Trans.・7. 1121-1125 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像 惠: "Synthesis and Crystal Structure of Dinuclear Palladium(I)dppm Complex with 4-Mercaptopyridine in the Thione Mode." Inorg.Chim.Acta. 281・. 116-119 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] 宗像惠・黒田孝義, 他: "Assembly of a mixed-valence Cu(I/II) System coupled by multiple hydrogen bounding through tetrahydroxy benzoguinone" Inorganica Chimica Acta. 268. 317-321 (1998)

    • Related Report
      1997 Annual Research Report
  • [Publications] 黒田孝義・宗像惠, 他: "Preparation,characterization and X-ray Crystal structures of I_2 and copper(II) complexes of 2,11-dithia[3.3]paracyclophane" Inorganica Chimica Acta. 258. 87-91 (1997)

    • Related Report
      1997 Annual Research Report

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Published: 1997-04-01   Modified: 2016-04-21  

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