Cobalt(III)-peroxo complexes containing 1,2-bis(dimethylphosphino)ethane (dmpe) or 1,3-bis(dimethylphosphino)propane (dmpp). Molecular structures of (Co(O2)(dmpe)2)B(C6H5)4 and (Co(O2)(dmpp)2)BF4H2O.

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概要

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• Monomeric (yellow) and dimeric (red) cobalt(III)–dioxygen complexes containing 1,2-bis(dimethylphosphino)ethane (dmpe) have been prepared from [Co(dmpe)<SUB>2</SUB>]<SUP>+</SUP> and [Co(dmpe)<SUB>2</SUB>]<SUP>2+</SUP>, respectively, by air oxidation. The 1,3-bis(dimethylphosphino)propane (dmpp) complex afforded only the monomeric dioxygen complex by either preparative method. The crystal structures of [Co(O<SUB>2</SUB>)(dmpe)<SUB>2</SUB>]B(C<SUB>6</SUB>H<SUB>5</SUB>)<SUB>4</SUB> (<B>1</B>) and [Co(O<SUB>2</SUB>)(dmpp)<SUB>2</SUB>]BF<SUB>4</SUB>·H<SUB>2</SUB>O (<B>2</B>) have been determined by X-ray analysis. Crystal data for <B>1</B>; monoclinic, <I>P</I>2<SUB>1</SUB>⁄<I>a</I>, <I>a</I>=18.011(12), <I>b</I>=18.761(10), <I>c</I>=11.455(6) Å, β=107.78(4)°, <I>V</I>=3686(4) Å<SUP>3</SUP>, <I>Z</I>=4, and <I>R</I>=0.064. Crystal data for <B>2</B>; orthorhombic, <I>Pbcn</I>, <I>a</I>=14.540(5), <I>b</I>=13.123(4), <I>c</I>=13.138(2) Å, <I>V</I>=2507(1) Å<SUP>3</SUP>, <I>Z</I>=4, and <I>R</I>=0.076. The complex ions in both <B>1</B> and <B>2</B> have a trigonal-bipyramidal coordination geometry when the O<SUB>2</SUB> group bonded to the Co atom in the side-on form at a coordination site of the trigonal plane is assumed to be a unidentate ligand. Bond lengths. Co–O (1.858(7)–1.881(4) Å) and O–O (1.414(12) and 1.425(6) Å), and O–O stretching frequencies (877 and 862 cm<SUP>−1</SUP>) indicate that both <B>1</B> and <B>2</B> are the peroxo complexes. The monomeric dioxygen complexes react immediately with SO<SUB>2</SUB> and with concd HCl to afford [Co(SO<SUB>4</SUB>)(dmpe or dmpp)<SUB>2</SUB>]<SUP>+</SUP> and <I>cis</I>-[CoCl<SUB>2</SUB>(dmpe or dmpp)<SUB>2</SUB>]<SUP>+</SUP>, respectively. The red dimeric <I>trans</I>-[(dmso)(dmpe)<SUB>2</SUB>Co(μ-O<SUB>2</SUB>)Co(dmpe)<SUB>2</SUB>(dmso)](BF<SUB>4</SUB>)<SUB>4</SUB> (dmso=dimethyl sulfoxide) complex was isolated and characterized.

• 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

• Saito Yoshihiko

  Department Of Cardiology Juntendo University School Of Medicine

• OHBA SHIGERU

  Deparment of Biology, Faculty of Science, Tokyo Metropolitan University

• Fujita Junnosuke

  Department of Chemistry Faculty of Science Osaka University

• Ohishi Tomoji

  Department of Chemistry, Faculty of Science, Nagoya University

• Ishii Toshio

  Chiba Institute of Technology

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