Structures of 1,4,13,16-tetraoxa-7,10-dithia[16](1,1')ruthenocenophane and its 1:2 HgCl2 complex.

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概要

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• The reaction of 1,1′-bis(6-chloro-1,4-dioxahexyl)ruthenocene with disodium 1,2-ethanedithiolate gave 1,4,13,16-tetraoxa-7,9-dithia[16](1,1′)ruthenocenophane (<B>5</B>) in 63% yield. The reaction of <B>5</B> with HgCl<SUB>2</SUB> in acetonitrile gave a 1: 2 complex (<B>6</B>) in 47% yield. The crystal structure of complex <B>6</B> and its metal free ligand <B>5</B> were determined by an X-ray method. Crystal data: <B>5</B>, triclinic, <I>a</I>=11.128(2), <I>b</I>=12.720(2), <I>c</I>=10.196(2)Å, α=113.55(1), β=64.13(1), γ=122.01(1)°, <I>U</I>=1074.1 Å<SUP>3</SUP>. <I>P</I>\bar1, <I>Z</I>=2, <I>D</I><SUB>c</SUB>=1.54 Mg m<SUP>−3</SUP>, μ(Mo <I>K</I>α)=9 mm<SUP>−1</SUP>. <I>R</I>=0.028. <B>6</B>, triclinic, <I>a</I>=16.595(4), <I>b</I>=12.645(3), <I>c</I>=7.401(1)Å, α=104.92(1), β=92.37(1), γ=69.38(2)°, <I>U</I>=1402.4Å<SUP>3</SUP>, <I>P</I>\bar1, <I>Z</I>=2, <I>D</I><SUB>c</SUB>=2.46 Mg m<SUP>−3</SUP>, μ(Mo <I>K</I>α)=12.2 mm<SUP>−1</SUP>, <I>R</I>=0.081. The X-ray analysis of <B>6</B> revealed that one Hg atom was bonded to the Ru atom of the ruthenocene nucleus with a distorted trigonal-planar configuration and another Hg atom was bonded to the two sulfur atoms of the macrocycle. This result is completely different from that obtained regarding complex 4,7,10,13-tetraoxa-1,16-dithia[16](1,1′)ruthenocenophane with HgCl<SUB>2</SUB>.

• 公益社団法人 日本化学会の論文

著者

• Akabori Sadatoshi

  Department Of Chemistry Faculty Of Science Toho University

• Sato Sadao

  Analytical And Metabolic Research Laboratories Sankyo Co. Ltd.

• Sato Masaru

  Chemical Analysis Center Saitama University

• Habata Yoichi

  Department of Chemistry, Faculty of Science, Toho University

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