Structures of three diastereomers of trans(N-Ph, N-Ph)-2,4-pentanedionatobis(N-phenylethylenediamine)cobalt(III) and of one diastereomer of trans(N-Ph, N-Ph)-oxalatobis(N-phenylethylenediamine)cobalt(III) complex cations.

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• The molecular structures of three racemic pairs of diastereomers, <I>ΔRR</I>(<I>ΛSS</I>)-, <I>ΔSR</I>(<I>ΛRS</I>)-, and <I>ΔSS</I>(<I>ΛRR</I>)-<I>trans</I>(<I>N</I>-Ph, <I>N</I>-Ph)-[Co(pd)(Ph-en)<SUB>2</SUB>]<SUP>2+</SUP> and of one racemic pair of diastereomers, <I>ΔSS</I>(<I>ΛRR</I>)-<I>trans</I>(<I>N</I>-Ph, <I>N</I>-Ph)-[Co(ox) (Ph-en)<SUB>2</SUB>]<SUP>+</SUP> (pd=2,4-pentanedionate ion, ox=oxalate ion, Ph-en=<I>N</I>-phenylethylenediamine) were determined by the single-crystal X-ray diffraction method in order to study the intramolecular interactions between π-systems in the ligands. For the <I>ΔSS</I>(<I>ΛRR</I>)-isomer of [Co(pd)(Ph-en)<SUB>2</SUB>]<SUP>2+</SUP>, three kinds of crystal structures <B>3a</B>, <B>3b</B>, and <B>3c</B> were investigated. The crystal data and final <I>R</I> values are: <I>ΔRR</I>(<I>ΛSS</I>)-[Co(pd)(Ph-en)<SUB>2</SUB>](ClO<SUB>4</SUB>)<SUB>2</SUB>·H<SUB>2</SUB>O (<B>1</B>), orthorhombic, <I>Pbca</I>, <I>a</I>=32.472(9), <I>b</I>=11.120(3), <I>c</I>=15.303(4) Å, <I>V</I>=5526(3) Å<SUP>3</SUP>, <I>Z</I>=8, <I>R</I>=0.065 for 2113 observed unique reflections. <I>ΔSR</I>(<I>ΛRS</I>)-[Co(pd)(Ph-en)<SUB>2</SUB>](ClO<SUB>4</SUB>)<SUB>2</SUB> (<B>2</B>), orthorhombic, <I>P</I>2<SUB>1</SUB>2<SUB>1</SUB>2<SUB>1</SUB>, <I>a</I>=19.440(8), <I>b</I>=16.406(8), <I>c</I>=8.407(3) Å, <I>V</I>=2681(2) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.038 for 2205 reflections. <I>ΔSS</I>(<I>ΛRR</I>)-[Co(pd)(Ph-en)<SUB>2</SUB>]Cl<SUB>2</SUB>·H<SUB>2</SUB>O (<B>3a</B>), monoclinic, <I>P</I>2<SUB>1</SUB>⁄<I>c</I>, <I>a</I>=12.475(3), <I>b</I>=11.590(2), <I>c</I>=19.054(4) Å, β=117.18(2)°, <I>V</I>=2450.6(9) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.035 for 2164 reflections. <I>ΔSS</I>(<I>ΛRR</I>)-[Co(pd)(Ph-en)<SUB>2</SUB>](ClO<SUB>4</SUB>)Cl·H<SUB>2</SUB>O (<B>3b</B>), triclinic, <I>P</I>\bar1, <I>a</I>=11.847(5), <I>b</I>=13.584(4), <I>c</I>=8.367(2) Å, α=103.57(2), β=91.85(3), γ=84.25(3)°, <I>V</I>=1302.1(8) Å<SUP>3</SUP>, <I>Z</I>=2, <I>R</I>=0.087 for 1374 reflections. <I>ΔSS</I>(<I>ΛRR</I>)-[Co(pd)(Ph-en)<SUB>2</SUB>](ClO<SUB>4</SUB>)Cl (<B>3c</B>), triclinic, <I>P</I>\bar1, <I>a</I>=11.660(5), <I>b</I>=14.028(3), <I>c</I>=8.308(7) Å, α=108.00(8), β=101.57(9), γ=92.47(13)°, <I>V</I>=1258(3) Å<SUP>3</SUP>, <I>Z</I>=2, <I>R</I>=0.052 for 1118 reflections. <I>ΔSS</I>(<I>ΛRR</I>)-[Co(ox)(Ph-en)<SUB>2</SUB>] Br·6H<SUB>2</SUB>O (<B>4</B>), orthorhombic, <I>Pna</I>2<SUB>1</SUB>, <I>a</I>=15.804(1), <I>b</I>=15.646(1), <I>c</I>=10.428(2) Å, <I>V</I>=2578.5(4) Å<SUP>3</SUP>, <I>Z</I>=4, <I>R</I>=0.065 for 1496 reflectios. The numbers of phenyl rings of the Ph-en ligands that overlap with the pd π system in the complex cation are 0, 1, and 2 for <B>1</B>, <B>2</B>, and <B>3</B> respectively. The ox ligand of <B>4</B> is ill-sandwiched by the two phenyl rings, whereas the pd ligand is well-sandwiched in <B>3a</B>. The arrangements of the phenyl groups relative to the pd differ slightly from one another in the crystals of <B>3a</B>, <B>3b</B>, and <B>3c</B>. The dihedral angles between the pd (or ox) and phenyl rings range from 25 to 35°.

• 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

• Saito Yoshihiko

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

• Akagawa Toshiaki

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

• Ma Guilin

  Department of Chemistry, Faculty of Science, Nagoya University

• Suzuki Nahomi

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

• Ouyang Yue

  Department of Chemistry, Faculty of Science, Nagoya University

• Suzuki Nahomi

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

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