Preparation and characterization of some Co(III) complexes containing (1R,2R)-dimethyl-1,2-cyclohexanediamine. Crystal structure of (+)435-trans-(CoCl2(R,R-dmchxn)2)ClHCl2H2O.

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• (−)<SUB>546</SUB>-<I>trans</I>-[Co(NO<SUB>2</SUB>)<SUB>2</SUB>(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]<SUP>+</SUP> and (+)<SUB>546</SUB>-<I>Λ</I>-Co(CO<SUB>3</SUB>)(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]<SUP>+</SUP>, which had been newly prepared, reacted with concentrated HCl to give, respectively, (−)<SUB>435</SUB>-<I>trans</I>-(<I>SSSS</I>)-[CoCl<SUB>2</SUB>(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]<SUP>+</SUP> and (+)<SUB>435</SUB>-<I>trans</I>-(<I>SRRS</I>)-[CoCl<SUB>2</SUB>(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]<SUP>+</SUP> stereospecifically, where <I>R</I>,<I>R</I>-dmchxn=(1<I>R</I>,2<I>R</I>)-<I>N</I>,<I>N</I>′-dimethyl-1,2-cyclohexanediamine. The stereospecific formation of (+)<SUB>546</SUB>-<I>Λ</I>-[Co(CO<SUB>3</SUB>)(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]<SUP>+</SUP> has been observed. The <I>trans</I>-dichloro complexes and their precursors have been characterized by elemental analysis and by electronic absorption, circular dichroism, <SUP>1</SUP>H NMR, and <SUP>13</SUP>C NMR spectroscopies. An X-ray crystal-structure determination was undertaken on one of the <I>trans</I>-dichloro isomers, (+)<SUB>435</SUB>-[CoCl<SUB>2</SUB>(<I>R</I>,<I>R</I>-dmchxn)<SUB>2</SUB>]Cl·HCl·2H<SUB>2</SUB>O, whose structure could not be characterized by usual spectroscopies. This complex forms triclinic crystals with <I>a</I>=11.395(10) Å, <I>b</I>=11.674(8) Å, <I>c</I>=11.031(8) Å, α=98.62(6)°, β=102.48(8)°, γ=118.24(5)°, and <I>Z</I>=2, in the space group P1. Least-squares refinements converged at an <I>R</I> value of 0.041 for 4870 independent reflections with <I>F</I><SUB>o</SUB>>3[σ(<I>F</I><SUB>o</SUB>)]. The complex cation has an approximately twofold symmetry. The conformations of the two five-membered chelate rings are both λ. The arrangements of the groups around the two secondary nitrogen atoms are <I>R</I> and <I>S</I> in each diamine. The isomerization from the (+)<SUB>435</SUB>-<I>trans</I>-dichloro complex to the (−)<SUB>435</SUB> isomer has been observed under mild basic conditions.

• 公益社団法人 日本化学会の論文

著者

• KOBAYASHI Kimiko

  The Institute of Physical and Chemical Research

• Sato Mitsunobu

  Department Of General Chemistry Faculty Of Engneering Kogakuin University

• Yano Shigenobu

  Department Of Chemistry Faculty Of Science Nara Women's University

• YASHIRO Morio

  Department of Applied Chemistry, Faculty of Engineering, Tokyo Institute of Polytechnics

• Yoshikawa Sadao

  Department Of Applied Chemistry Faculty Of Science And Technology Keio University

• SAKURAI Tosio

  The Institute of Physical and Chemical Research

• Sato Mitsunobu

  Department of Synthetic Chemistry, Faculty of Engineering, The University of Tokyo

• Yashiro Morio

  Department of Synthetic Chemistry, Faculty of Engineering, The University of Tokyo

• Kobayashi Kimiko

  The Institute of Physical and Chemical Research (Rikagaku Kenkyusho)

• Yokoo Yasuhiko

  Department of Synthetic Chemistry, Faculty of Engineering, The University of Tokyo

• Sakurai Tosio

  The Institute of Physical and Chemical Research (Rikagaku Kenkyusho)

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