Preparation and characterization of rhodium(III) complexes containing (2-aminoethyl)dimethylphosphine (edmp) or 1,2-bis(dimethylphosphino)ethane (dmpe). Structures of fac-[Rh(edmp)3]3+, trans(Cl,Cl),cis(P,P)-[RhCl2(edmp)2]+, and trans-[RhCl2(dmpe)2]+.

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概要

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• The <I>fac</I>-[Rh(edmp)<SUB>3</SUB>]<SUP>3+</SUP> (edmp=(2-aminoethyl)dimethylphosphine), <I>trans</I>(<I>Cl</I>,<I>Cl</I>),<I>cis</I>(<I>P</I>,<I>P</I>)-[RhCl<SUB>2</SUB>(edmp)<SUB>2</SUB>]<SUP>+</SUP>, and <I>trans</I>-[RhCl<SUB>2</SUB>(dmpe)<SUB>2</SUB>]<SUP>+</SUP> (dmpe=1,2-bis(dimethylphosphino)ethane) complexes were prepared and the molecular structures were determined by the single crystal X-ray diffraction method. Crystal data and final <I>R</I> values are: <I>fac</I>-[Rh(edmp)<SUB>3</SUB>]Br<SUB>3</SUB>·3H<SUB>2</SUB>O, orthorhombic, <I>Pna</I>2<SUB>1</SUB>, <I>a</I>=26.750(4), <I>b</I>=10.125(1), <I>c</I>=9.592(1) Å, <I>V</I>=2598.2(5) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.039 for 1590 observed unique reflections. <I>trans</I>(<I>Cl</I>,<I>Cl</I>),<I>cis</I>(<I>P</I>,<I>P</I>)-[RhCl<SUB>2</SUB>(edmp)<SUB>2</SUB>]PF<SUB>6</SUB>, monoclinic, <I>P</I>2<SUB>1</SUB>/<I>a</I>, <I>a</I>=18.197(4), <I>b</I>=12.574(2), <I>c</I>=8.615(1) Å, β=96.59(2)°, <I>V</I>=1958.2(6) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.032 for 3379 reflections. <I>trans</I>(<I>Cl</I>,<I>Cl</I>),<I>cis</I>(<I>P</I>,<I>P</I>)-[RhCl<SUB>2</SUB>(edmp)<SUB>2</SUB>]ClO<SUB>4</SUB>, triclinic, P\bar1, <I>a</I>=13.122(2), <I>b</I>=17.952(2), <I>c</I>=12.343(2) Å, α=91.65(2), β=102.46(2), γ=80.74(1)°, <I>V</I>=2802.0(7) Å<SUP>3</SUP>, <I>Z</I>=6, <I>R</I>=0.070 for 7513 reflections, <I>trans</I>-[RhCl<SUB>2</SUB>(dmpe)<SUB>2</SUB>]CF<SUB>3</SUB>SO<SUB>3</SUB>, monoclinic, <I>P</I>2<SUB>1</SUB>/<I>a</I>, <I>a</I>=13.166(2), <I>b</I>=24.337(4), <I>c</I>=8.002(2) Å, β=95.95(2)°, <I>V</I>=2550.1(8) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.040 for 3201 reflections. It was found that the shorter the Rh–P bond length, the larger the trans Rh–N bond elongation. The mean Rh–P bond distance in <I>trans</I>-[RhCl<SUB>2</SUB>(dmpe)<SUB>2</SUB>]CF<SUB>3</SUB>SO<SUB>3</SUB> (2.337(2) Å) is longer than those in <I>fac</I>-[Rh(edmp)<SUB>3</SUB>]Br<SUB>3</SUB>·3H<SUB>2</SUB>O (2.283(4) Å) and <I>trans</I>(<I>Cl</I>,<I>Cl</I>),<I>cis</I>(<I>P</I>,<I>P</I>)-[RhCl<SUB>2</SUB>(edmp)<SUB>2</SUB>]PF<SUB>6</SUB> (2.252(2) Å). A series of complexes of <I>trans</I>(<I>X</I>,<I>X</I>),<I>cis</I>(<I>P</I>,<I>P</I>)-[RhX<SUB>2</SUB>(edmp)<SUB>2</SUB>]<SUP>+</SUP> (X=Cl, Br, I) and <I>trans</I>-[RhX<SUB>2</SUB>(dmpe)<SUB>2</SUB>]<SUP>+</SUP> (X=Cl, Br) were also prepared and their absorption spectra were compared with one another and with those of the corresponding cobalt(III) complexes.

• 公益社団法人 日本化学会の論文

著者

• Kojima Masaaki

  Department Of Chemistry Faculty Of Science Okayama 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

• HAMADA Masatoshi

  Department of Applied Mathematics, Faculty of Engineering, Yokohama National University

• Suzuki Nahomi

  Department of Chemistry, Faculty of Science and Technology, Keio University

• Simonsen Kim

  Department of Chemistry, Faculty of Science, Nagoya University

• Hamada Masatoshi

  Department of Chemistry, Faculty of Science and Technology, Keio University

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