The molecular structure of tricarbonyl(triple-layered[2.2]paracyclophane)chromium at -95.DEG.C(monoclinic form) and -160.DEG.C(triclinic form).

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• The tricarbonylchromium complex of triple-layered [2.2]paracyclophane shows a reversible phase transition in the solid state from the monoclinic to the triclinic form at a temperature between −100 and −110°C. The monoclinic form crystallizes in the space group <I>P</I>2<SUB>1</SUB>⁄<I>c</I>, with <I>a</I>=15.095(6), <I>b</I>=9.950(3), <I>c</I>=15.641(5) Å, β=103.46(3)° (−95°C), and <I>Z</I>=4: The triclinic form belongs to the space group <I>P</I>\bar1, with <I>a</I>=15.037(5) Å, <I>b</I>=9.913(2), <I>c</I>=15.662(5) Å, α=89.41(3), β=104.51(3), γ=89.39(4)° (−160°C), and <I>Z</I>=4. In the triclinic crystal, two molecules are crystallographically independent. The crystal structures were solved by the direct method and then refined by the block-diagonal least-squares procedure to the <I>R</I> indices of 0.067 for 3530 (monoclinic form) and 0.079 for 6776 (triclinic form) observed reflections. No essential difference is found between the structures of the monoclinic-form molecule and the two triclinic-form molecules. The interlayer distance between the upper-layer benzene ring coordinated to the Cr(CO)<SUB>3</SUB> group and the middle-layer benzene ring is unusually shorter than the corresponding distance between the middle- and lower-layer benzene rings. No bond alternation is found in the upper-layer benzene ring, unlike as in the tricarbonyl(benzene)chromium complex and the (tricarbonyl)chromium complex of double-layered [2.2]paracyclophane. The phase transition of the crystal can be explained by a slight change in the molecular packing.

• 公益社団法人 日本化学会の論文

著者

• Miki Kunio

  Department Of Chemistry Graduate School Of Science Kyoto University

• Kai Yasushi

  Department Of Applied Chemistry Faculty Of Engineering Osaka University

• Kasai Nobutami

  Department Of Applied Biological Science Tokyo University Of Science

• Tanaka Nobuo

  Department Of Agro-environmental Sciences Graduate School Of Bioresource And Bioenvironmental Scienc

• Oike Hitoshi

  Department of Applied Chemistry, Faculty of Engineering, Osaka University

• Miki Kunio

  Department of Applied Chemistry, Faculty of Engineering, Osaka University

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