Preparation and Characterization of Cobalt(III), Nickel(II), and Copper(I) Complexes Containing 5,8-Diphenyl-5,8-diphospha-2,11-dithiadodecane (L), CH3SCH2CH2P(C6H5)CH2CH2P(C6H5)CH2CH2SCH3, and Molecular Structure of (Ni(rac(P)-L)2)(BF4)2.

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概要

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• <I>Δ</I>-<I>RR</I>,<I>Λ</I>-<I>SS</I>-[Co(acac)<SUB>2</SUB>(<I>rac</I>(<I>P</I>)-L]<SUP>+</SUP> and [Co(acac)<SUB>2</SUB>(<I>meso</I>(<I>P</I>)-L)]<SUP>+</SUP> were obtained by reaction of [Co(acac)<SUB>3</SUB>] (acac=2,4-pentanedionate ion) with 5,8-diphenyl-5,8-diphospha-2,11-dithiadodecane (L) in 1 : 1 molar ratio in dichloromethane in the presence of active charcoal, no <I>Δ</I>-<I>SS</I>,<I>Λ</I>-<I>RR</I> isomer of the <I>rac</I>(<I>P</I>)-L complex being formed. Five-coordinate [Ni(<I>rac</I>(<I>P</I>)-L)<SUB>2</SUB>]<SUP>2+</SUP> and [Ni(<I>meso</I>(<I>P</I>)-L)<SUB>2</SUB>]<SUP>2+</SUP> were yielded by reaction of Ni(II) and L in 1 : 2 molar ratio in methanol, and the molecular structure of less soluble [Ni(<I>rac</I>(<I>P</I>)-L)<SUB>2</SUB>](BF<SUB>4</SUB>)<SUB>2</SUB> was determined by X-ray analysis. Crystal data: monoclinic, space group <I>P</I>2<SUB>1</SUB>⁄<I>n</I>, <I>a</I>=17.136(3), <I>b</I>=20.134(5), <I>c</I>=14.106(3) Å, β=93.30(2)°, <I>V</I>=4859(2) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.089 for 8001 reflections. The Ni atom is surrounded square pyramidally by four P atoms in the basal plane and one S atom at the apical position with distances of the Ni–P: 2.214(2)–2.234(2) Å and the Ni–S: 2.603(2) Å. Both [Ni(<I>rac</I>(<I>P</I>)-L)<SUB>2</SUB>]<SUP>2+</SUP> and [Ni(<I>meso</I>(<I>P</I>)-L)<SUB>2</SUB>]<SUP>2+</SUP> in CH<SUB>2</SUB>Cl<SUB>2</SUB> solutions exchange four –SCH<SUB>3</SUB> groups at the apical positin on the NMR time scale. White [Cu(<I>rac</I>(<I>P</I>)-L)]BF<SUB>4</SUB> was precipitated selectively by reaction of Cu(BF<SUB>4</SUB>)<SUB>2</SUB>·6H<SUB>2</SUB>O and L in 1 : 1 molar ratio in ethanol.

• 公益社団法人 日本化学会の論文

著者

• KASHIWABARA Kazuo

  Department of Chemistry, Faculty of Science, Nagoya University

• Kashiwabara Kazuo

  Department Of Chemistry Faculty Of Science Nagoya University

• Fujita Junnosuke

  Department of Chemistry Faculty of Science Osaka University

• Kita Masakazu

  Department of Chemistry, Faculty of Science, Nagoya University

• Kitagawa Tetsuji

  Department of Chemistry, Faculty of Science, Nagoya University

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