The conformational studies of 4,7,10-trioxa-1,13-dithia[13](1,1')ruthenocenophane and its PdCl2 complex by X-ray analyses.
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概要
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Dichlorobis(4,7,10-trioxa-1,13-dithia[13](1,1′)ruthenocenophane)palladium(II) (<B>6</B>) was obtained by the reaction of 4,7,10-trioxa-1,13-dithia[13](1,1′)ruthenocenophane (<B>5</B>) with dichlorobis(acetonitrile)palladium(II) in 72% yield. The crystal structures of the complex <B>6</B> and its metal free ligand <B>5</B> were determined by the X-ray method. The crystal data: <B>5</B>, monoclinic, <I>P</I>2<SUB>1</SUB>⁄<I>a</I>, <I>a</I>=18.783(2), <I>b</I>=7.895(1), <I>c</I>=12.892(1) Å, β=93.53(1)°, <I>U</I>=1908.2 Å<SUP>3</SUP>, <I>Z</I>=4, <I>D</I><SUB>c</SUB>=1.58 g cm<SUP>−3</SUP>, μ(Mo <I>K</I>α)=10 cm<SUP>−1</SUP>. <B>6</B>, triclinic, <I>P</I>\bar1, <I>a</I>=13.956(2), <I>b</I>=9.174(1), <I>c</I>=8.770(1) Å, α=86.61(1), β=75.54(1), γ=94.37(1)°, <I>U</I>=1080.6 Å<SUP>3</SUP>, <I>Z</I>=2, <I>D</I><SUB>c</SUB>=1.94 g cm<SUP>−3</SUP>, μ(Mo <I>K</I>α)=20 cm<SUP>−1</SUP>. The Pd atom of <B>6</B> bonded to the two sulfur atoms of the ligand and the torsion angle (69.2°) around the <I>z</I>-axis of the ruthenocenophane nucleus in the metal-free ligand is much larger than the corresponding one (0.4°) in the complex. These results are completely opposite of the case of 1,4,7,10-tetrathia[10](1,1′)ruthenocenophane and its Pt complex. Furthermore, the intramolecular atomic distance (3.697 Å) between the Ru and Pd atoms in <B>6</B> suggests the absence of the Ru–Pd dative bond.
- 公益社団法人 日本化学会の論文
著者
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AKABORI Sadatoshi
Department of Chemistry, Faculty of Science, Toho University
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Akabori Sadatoshi
Department Of Chemistry Faculty Of Science Toho University
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Sato Sadao
Analytical And Metabolic Research Laboratories Sankyo Co. Ltd.
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Sato Masaru
Chemical Analysis Center Saitama University
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Kawazoe Kayoko
Analytical and Metabolic Research Laboratories, Sankyo Co. Ltd.
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Habata Yoichi
Department of Chemistry, Faculty of Science, Toho University
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