X-ray structural studies of green and brown crystals of trans-(CoC)2(N48))X(N48=1,4,7,10-tetraazacyclopentadecane, X=NO3-, BF4-, and ClO4-).

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概要

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• Crystal structures of green (X=NO<SUB>3</SUB><SUP>−</SUP>(<B>1</B>), BF<SUB>4</SUB><SUP>−</SUP>(<B>2</B>)) and brown (X=BF<SUB>4</SUB><SUP>−</SUP>(<B>3</B>) and ClO<SUB>4</SUB><SUP>−</SUP>(<B>4</B>)) salts of <I>trans</I>-[CoCl<SUB>2</SUB>(N<SUB>4</SUB>8)]X (N<SUB>4</SUB>8=1,4,7,10-tetraazacyclopentadecane) were determined by an X-ray diffraction method. The complex cation is a <I>RSSR</I>(<I>SRRS</I>) isomer for the four chiral nitrogen atoms and has approximate C<SUB>2</SUB> symmetry. Green crystals <B>1</B> and <B>2</B> are monoclinic and have the chiral space group <I>P</I>2<SUB>1</SUB>, comprising one antipode of the complex ion by spontaneous resolution, whereas brown crystals <B>3</B> and <B>4</B> are orthorhombic and a racemate. The eight-membered chelate ring formed by the N<SUB>4</SUB>8 ligand and the Co atom takes a distorted boat–boat (BB) form in <B>1</B> and <B>2</B>, whereas the conformation is disordered in <B>3</B> and <B>4</B> with BB (40%) and distorted twist–boat-chair (TBC; 60%) forms at room temperature. At 113 K, the eight-membered chelate ring in <B>4</B> takes exclusively the TBC form. The crystal data are as follows: [CoCl<SUB>2</SUB>(C<SUB>11</SUB>H<SUB>26</SUB>N<SUB>4</SUB>)]X, monoclinic NO<SUB>3</SUB> salt, <B>1</B>, <I>P</I>2<SUB>1</SUB>, <I>a</I>=9.672(3), <I>b</I>=12.285(5), <I>c</I>=7.051(2) Å, β=94.70(3)°, <I>V</I>=835.0(5) Å<SUP>3</SUP>, <I>Z</I>=2, <I>T</I>=300(1) K, final <I>R</I>=0.037 for 2381 reflections. Monoclinic BF<SUB>4</SUB> salt, <B>2</B>, <B>2</B>, <I>P</I>2<SUB>1</SUB>, <I>a</I>=9.857(2), <I>b</I>=12.694(2), <I>c</I>=7.065(1) Å, β=94.34(2)°, <I>V</I>=881.5(2) Å<SUP>3</SUP>, <I>Z</I>=2, <I>T</I>=300(1) K, final <I>R</I>=0.031 for 1880 reflections. Orthorhombic BF<SUB>4</SUB> salt, <B>3</B>, <I>Pcab</I>, <I>a</I>=12.816(1), <I>b</I>=22.359(2), <I>c</I>=12.388(1) Å, <I>V</I>=3549.8(5) Å<SUP>3</SUP>, <I>Z</I>=8, <I>T</I>=300(1) K, final <I>R</I>=0.095 for 2086 reflections. Orthorhombic ClO<SUB>4</SUB> salt at 300(1) K, <B>4a</B>, <I>Pcab</I>, <I>a</I>=12.829(1), <I>b</I>=22.376(2), <I>c</I>=12.425(1) Å, <I>V</I>=3566.7(6) Å<SUP>3</SUP>, <I>Z</I>=8, final <I>R</I>=0.070 for 1764 reflections; orthorhombic ClO<SUB>4</SUB> salt at 113(2) K, <B>4b</B>, <I>a</I>=12.630(2), <I>b</I>=22.276(5), <I>c</I>=12.354(2) Å, <I>V</I>=3475.7(11) Å<SUP>3</SUP>, final <I>R</I>=0.109 for 2215 reflections.

著者

• Saito Yoshihiko

  Department Of Cardiology Juntendo University School Of Medicine

• Tsuchimoto Masanobu

  Department Of Chemistry Chiba Institute Of Technology

• Nonoyama Matsuo

  Department Of Chemistry Faculty Of Science Nagoya University

• OHBA SHIGERU

  Deparment of Biology, Faculty of Science, Tokyo Metropolitan University

• Fujita Junnosuke

  Department of Chemistry Faculty of Science Osaka University

• Kita Masakazu

  Department of Chemistry, Faculty of Science, Nagoya University

• Takazawa Hiroyuki

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

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