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Trial production of single-crystal X-ray diffractometer with 2D detector for high-pressure crystallography

Research Project

Project/Area Number 12354008
Research Category

Grant-in-Aid for Scientific Research (A)

Allocation TypeSingle-year Grants
Section展開研究
Research Field Inorganic chemistry
Research InstitutionThe University of Tokyo

Principal Investigator

MATSUSHITA Nobuyuki  The University of Tokyo, Graduate School of Arts and Science, Associate Professor, 大学院・総合文化研究科, 助教授 (80219427)

Co-Investigator(Kenkyū-buntansha) NISHIKIORI Shin-ichi  The University of Tokyo, Graduate School of Arts and Science, Associate Professor, 大学院・総合文化研究科, 助教授 (70134400)
SHIMOI Mamoru  The University of Tokyo, Graduate School of Arts and Science, Professor, 大学院・総合文化研究科, 教授 (30092240)
KOJIMA Norimichi  The University of Tokyo, Graduate School of Arts and Science, Professor, 大学院・総合文化研究科, 教授 (60149656)
城 始勇  理学電機(株), X線研究所, 主任研究員
MOTOO Shiro  RIGAKU CO., LTD., X-ray Research Laboratory, Chief Scientist
Project Period (FY) 2000 – 2003
Project Status Completed (Fiscal Year 2003)
Budget Amount *help
¥43,080,000 (Direct Cost: ¥40,200,000、Indirect Cost: ¥2,880,000)
Fiscal Year 2003: ¥3,510,000 (Direct Cost: ¥2,700,000、Indirect Cost: ¥810,000)
Fiscal Year 2002: ¥2,990,000 (Direct Cost: ¥2,300,000、Indirect Cost: ¥690,000)
Fiscal Year 2001: ¥5,980,000 (Direct Cost: ¥4,600,000、Indirect Cost: ¥1,380,000)
Fiscal Year 2000: ¥30,600,000 (Direct Cost: ¥30,600,000)
Keywordshigh pressure / crystal structure analysis / X-ray diffraction / Imaging Plate / diamond anvil / ダイヤモンドアンビルセル
Research Abstract

A single-crystal X-ray diffractometer with Imaging Plate(IP) as a two dimensional detector was assessed suitable for structure analysis of metal complexes. X-ray diffraction data were measured for a number of single-crystals of various metal complexes using the IP X-ray diffractometer, and their structure analyses were performed To compare with these results, ten of their metal complexes were also measured by using a 4-circle X-ray diffractometer, which is a typical one for the single-crystal structure analysis. The results of the analyses from the IP X-ray diffractometer were satisfactory.
A diamond-anvil-cell (DAC) being able to be mount with the IP X-ray diffractometer was developed as a high-pressure apparatus. That is a 40 mmφ DAC, which is lather than a typical DAC for single-crystal diffraction. A goniometer-head was also developed suitable for the 40 mmφDAC and the IP X-ray diffractometer.
A high precise drilling machine for gasket hole and various jigs were manufactured to precisely manipulate very small single crystals in the DAC.
A lighting system, a beam-stopper, and collimaters around the goniometer were rebuilt to mount the DAC on the IP X-my diffractometer.
Movement of the goniometer with DAC was checked It is confirmed that the collision and any other trouble were not happened in the movement As a torsion of the goniometer-head was, however, observed due to the weight of the DAC in the check process, the goniometer-head was rebuilt to strengthen it.
Measurement procedures and technique were studied and developed for the single crystal in the DAC on the IP X-ray diffractometer.

Report

(5 results)
  • 2003 Annual Research Report   Final Research Report Summary
  • 2002 Annual Research Report
  • 2001 Annual Research Report
  • 2000 Annual Research Report
  • Research Products

    (34 results)

All Other

All Publications (34 results)

  • [Publications] N.Matsushita: "A one-dimensional Cl-bridged Pt^<II/IV> mixed-valence complex, catena-poly[[bis(ethylenediamine)platinum(II)-μ-chloro-bis(ethylenediamin)platinum(IV)-μ-chloro] tetrakis(hydrogensulfate)]."Acta Crystallogr.Sect.E. E59. M26-M28 (2003)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] H.Yoshikawa, S.Nishikiori, T.Ishida: "Crystal structure and spectroscopic properties of the CT complex of methyl viologen dication and o-dimethoxybenzene included in a polycyano-polycadmate host, and electrostatic effects on its CT absorption."J.Phys.Chem.B. 107. 9261-9267 (2003)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] T.Yasue, Y.Kawano, M.Shimoi: "Proton-Induced Change of the Coordination Mode of a Boron Group : Boryl Complexes [Mn(CO)_4(PR_3)(BH_<2->・PMe_3)] and Cationic Borane s Complexes [Mn(CO)_4(PR_3)(η^1BH_<3->PMe_3)]^+"Angew.Chem.Int.Ed.. 42. 1727-1730 (2003)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] M.Itoi, A.Taira, M.Enomoto, N.Matsushita, N.Kojima, Y.Kobayashi, K.Asai, K.Koyama, et al.: "Crystal structure and structural transition caused by charge-transfer phase transition for iron mixed-valence complex (n-C_3H_7)_4N[Fe^<II>Fe^<III>(dto)_3](dto=C_2O_2S_2)"Solid State Commun.. 130. 415-420 (2004)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] A.Taira, N.Matsushita: "Mixed-Valence State of a One-Dimensional Platinum Complex with a Counter Ion Having Two Alkyl Chains and its Liquid Crystal Phase."Mol.Cryst.Liq.Cryst.. 379. 297-302 (2002)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] H.Nishimura, N.Matsushita: "Single-Crystalline Photochromism of Bis[2-(aminomethyl)pyridine]platinum(II) Chloride Monohydrate."Chemistry Letters. 930-931 (2002)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] N.Matsushita: "A one-dimensional Cl-bridged Pt^<II/IV> mixed-valence complex, catena-poly[[bis(ethylenediamine)platinum(II)-μ-chloro-bis(etylenediamine)platinum (IV)-μ-chloro]tetrakis(hudrogensulfate)]"Acta Crystallogr.Sect.E. E59. M26-M28 (2003)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] H.Yoshikawa, S.Nishikiori, T.Ishida: "Crystal structure and spectroscopic properties of the CT complex of methyl viologen dication and o-dimethoxybenzene induced in a polycyano-polycadmate host, and electrostatic effects on its CT absorption"J.Phys.Chem.B. 107. 9261-9267 (2003)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] T.Yasue, Y.Kawano, M.Shimoi: "Proton-Induced Change of the Coordination Mode of a Boron Group : Boryl Complexes [Mn(CO)_4(PR_3)(BH_2-PMe_3)] and Cationic Borane σ Complexes [Mn(CO)4(PR_3)(η^1-BH_3-PMe_3)]^+"Angew.Chem.Int.Ed.. 42. 1727-1730 (2003)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] M.Itoi, A.Taira, M.Enomoto, N.Matsushita, N.Kojima, Y.Kobayashi, K.Asai, K., Koyama, et al.: "Crystal structure and structural transition caused by charge-transfer phase transition for iron mixed-valence complex (n-C_3H_7)_4NFe^<II>Fe^<III>(dto)_3(dto=C_2O_2S_2)"Solid State Commun.. 130. 415-420 (2004)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] A.Taira, N.Matsushita: "Mixed-Valence State of a One-Dimensional Platinum Complex with a Counter Ion Having Two Alkyl Chains and its Liquid Crystal Phase"Mol.Cryst.Liq.Cryst.. 379. 297-302 (2002)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] H.Nishimura, N.Matsushita: "Single-Crystalline Photochromism of Bis[2-(aminomethyl)pyridine]platinum(II) Chloride Monohydrate"Chemistry Letters. 930-931 (2002)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      2003 Final Research Report Summary
  • [Publications] N.Matsushita: "A one-dimensional Cl-bridged Pt^<IIIV> mixed-valence complex, catena-poly[[bis(ethylenediamine) platinum(II)-μ-chloro-bis(ethylenediamine)platinum(IV)-μ-chloro]tetrakis(hydrogensulfate)]."Acta Crystallogr.Sect.E. E59. M26-M28 (2003)

    • Related Report
      2003 Annual Research Report
  • [Publications] H.Yoshikawa, S.Nishikiori, T.Ishida: "Crystal structure and spectroscopic properties of the CT complex of methyl viologen dication and o-dimethoxybenzene induced in a polycyano-polycadmate host, and electrostatic effects on its CT absorption."J.Phys.Chem.B. 107. 9261-9267 (2003)

    • Related Report
      2003 Annual Research Report
  • [Publications] T.Yasue, Y.Kawano, M.Shimoi: "Proton-Induced Change of the Coordination Mode of a Boron Group : Boryl Complexes [Mn(CO)_4(PR_3)(BH_2-PMe_3)] and Cationic Borane σ Complexes [Mn(CO)_4(PR_3)(η^1-BH_3-PMe_3)]^+"Angew.Chem.Int.Ed.. 42. 1727-1730 (2003)

    • Related Report
      2003 Annual Research Report
  • [Publications] M.Itoi, A.Taira, M.Enomoto, N.Matsushita, N.Kojima, Y.Kobayashi, K.Asai, K.Koyama, et al.: "Crystal structure and structural transition caused by charge-transfer phase transition for iron mixed-valence complex (n-C_3H_7)_4N[Fe^<II>Fe^<III>(dto)_3](dto=C_2O_2S_2)"Solid State Commun.. (印刷中). (2004)

    • Related Report
      2003 Annual Research Report
  • [Publications] A.Taira, N.Matsushita: "Mixed-Valence State of a One-Dimensional Platinum Complex with a Counter Ion Having Two Alkyl Chains and its Liquid Crystal Phase"Mol. Cryst. Liq. Cryst.. 379. 297-302 (2002)

    • Related Report
      2002 Annual Research Report
  • [Publications] H.Nishimura, N.Matsushita: "Single-Crystalline Photochromism of Bis[2-(aminomethyl)pyridine]platinum(II) Chloride Monohydrate"Chemistry Letters. 930-931 (2002)

    • Related Report
      2002 Annual Research Report
  • [Publications] N.Matsushita: "A one-dimensional CI-bridged Pt^<II/IV>mixed-valence complex, catena-poly[bis(ethylenediamine)platinum(II)-μ-chloro-bis(ethylenediamine)Platinum(IV)-μ-chloro]tetrakis(hydrogensulfate)]"Acta Crystallogr. Sect. E. E59. M26-M28 (2003)

    • Related Report
      2002 Annual Research Report
  • [Publications] M.Ohkubo, T.Komatsu, N.Matsushita, N.Kojima, G.Saito: "Crystal Structure and Physical Properties of BEDT-TTF(bis(ethylenedithio)tetrathiafulvalene)Salt Coupled with a Photo-Sensitive Transition Metal Complex"Mol. Cryst. Liq. Cryst.. 376. 147-152 (2002)

    • Related Report
      2002 Annual Research Report
  • [Publications] M.Shimoi, K.Katoh, G.Kodama, Y.Kawano, H.Ogino: "Fluxtional Behavior of chromium and Tungusten Complexes of Monodentate Bis(trimethylphosphine)diborane(4) : A Model Case for AlkaneMmetal Comlexes"J. Organomet. Chem.. 659. 102-104 (2002)

    • Related Report
      2002 Annual Research Report
  • [Publications] R.Sekiya, S.Nishikiori: "Design and Structural Extension of a Supramolecular Inclusion-Compound Host Made by the Formation of Dimers of Isonicotinic Acid and Thiocyanato Coordinating Bridges"Chem. Eur. J.. 8. 4803-4810 (2002)

    • Related Report
      2002 Annual Research Report
  • [Publications] Y.WADA, N.MATSUSHITA, A.TAIRA, T.MITSUHASHI: "Transient absorption and luminescence studies of the relaxation processes of the photoexcited states in wide gap MX-chain compounds"Synth. Metals. 116. 397-400 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] Y.WADA, N.MATSUSHITA, A.TAIRA, T.MITSUHASHI: "Ultrafast relaxation processes of the photoexcited states in MX-chains"Synth. Metals. 120. 1063-1064 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] N.Kojima, W.Aoki, M.Itoi, Y.Ono, M.Seto, Y.Kobayashi, Y.Maed: "Charge transfer phase transition and ferromagnetism in a mixed-valence iron complex,(n-C_3H_7)4N[Fe^<II>Fe^<III>(dto)_3](dto=C_2O_2S_2)"Solid State Commun.. 120. 165-170 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] Y.Kawano, H.Kawakami, M.Shimoi: "Synthesis, Structure, and Phosphine-Induced Degradation of a Ruthenapentaboarne Cluster with a Sterically Damanding Haxamethylbenzen Ligand"Chem. Lett.. 2001. 1006-1007 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] L.N.Pangan, Y.Kawano, M.Shimoi: "Synthesis of nido-[1-OMe-2, 3-(Cp^*Ru)_2{μ-P(0Me)_2}B_3H_5] : Methoxy Transfer from Phosphorus to Boron and Cluster Core Rearrangement"Inorg. Chem.. 40. 1985-1986 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] R.Sekiya, S.Nishikiori: "A preparative strategy for supramolecular inclusion compounds by combination of dimer formation of isonicotinic acid and coordination bonding"Chem. Commun.. 2001. 2612-2613 (2001)

    • Related Report
      2001 Annual Research Report
  • [Publications] N.Kojima,N.Matsushita: "P-T Phase Diagram and Au Valence State of the Perovskite-type Au Mixed-Valence Complexes M_2 [AU^IX_2] [Au^<III>X_4] (M=K, Rb, Cs ; X=Cl, Br, I)"Coordination Chemistry Reviews. 198. 251-263 (2000)

    • Related Report
      2000 Annual Research Report
  • [Publications] Y.Wada,N.Matsushita,A.Taira,T.Mitsuhashi: "Transient absorption and Iuminescence studies of the relaxation processes of the photoexcited states in wide gap MX-chain compounds"Synthetic Metals. 116. 397-400 (2000)

    • Related Report
      2000 Annual Research Report
  • [Publications] X.Liu,Y.Moritomo,A.Nakamura,S.Matsuba,N.Kojima: "Pressure-Induced Phase Transition in Quasi-1D Mixed-Valence Gold Complexes"Journal of the Physical Society of Japan. 69. 3158-3161 (2000)

    • Related Report
      2000 Annual Research Report
  • [Publications] T.Yasue,Y.Kawano,M.Shimoi: "Syntheses and Structures of Trimethylphosphine-Complexed Primary Boryl Complexes of Group 8 Metals, Cp^*M (CO) 2 (BH2.-PMe3) (M=Fe, Ru)"Chemistry Letters. 2000. 58-59 (2000)

    • Related Report
      2000 Annual Research Report
  • [Publications] H.Yoshikawa,S.Nishikiori: "Photoinduced Color Change of Methylviologen in Polycyano-Polycadmate Host Clathrates"Chemistry Letters. 2000. 142-143 (2000)

    • Related Report
      2000 Annual Research Report
  • [Publications] S.Hayami,Zhong-ze Gu,M.Shiro,Y.Einaga,A.Fujishima,O.Sato: "First Observation of Light-Induced Excited Spin State Trapping for an Iron (III) Complex"Journal of the American Chemical Society. 122. 7126-7127 (2000)

    • Related Report
      2000 Annual Research Report

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Published: 2000-04-01   Modified: 2016-04-21  

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