Topochemical studies. VII. The crystal and molecular structures of tetrachlorophthalic acid hemihydrate and tetrabromophthalic anhydride.

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概要

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• The crystal structures of tetrachlorophthalic acid hemihydrate (TCPH) and tetrabromophthalic anhydride (TBPA) have been determined from visually estimated Cu<I>K</I>α data. The crystals of TGPH are monoclinic, space group A2/a, <I>a</I>=19.81(1), <I>b</I>=7.091(5), <I>c</I>=16.22(1) Å, β=101.2(2)° and <I>Z</I>=8. Those of TBPA are monoclinic, space group P2<SUB>1</SUB>/n, <I>a</I>=13.39(3), <I>b</I>=6.19(2), <I>c</I>=12.66(3) Å, β=91.1(3)° and <I>Z</I>=4. The structures of TGPH and TBPA were solved from the sharpened Patterson maps, and refined by the block-diagonal least-squares method to <I>R</I> values of 0.112 and 0.112 for 1287 and 1278 non-zero reflections, respectively. The molecules of TCPH related by a twofold screw axis are linked together by hydrogen bonds between the carboxylic groups to form a chain along the b axis and the chains are held together by hydrogen bonds through water molecules to form a sheet parallel to the (100) plane. The sheets are stacked by van der Waals forces. The dihedral angles of the carboxylic groups with the benzene ring are 68.2 and 48.9°. The crystals of TBPA are isomorphous to those of tetrachlorophthalic anhydride. The benzene ring of TBPA are distorted by the attachment of five membered ring. There is considerable molecular overlap in TCPH, while in TBPA there is no overlap.

• 公益社団法人 日本化学会の論文

著者

• Kashino Setsuo

  Department Of Chemistry Faculty Of Science Okayama University

• Ito Kuniaki

  Department Of Architecture Faculty Of Engineering Tohoku University

• Haisa Masao

  Department of Chemistry Faculty of Science Kwansei Gakuin University

• Moriya Keigo

  Department of Chemistry, Faculty of Science, Okayama University

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