Crystal structure and 35Cl NQR of copper(II) trichloroacetate trihydrate.
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概要
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The crystal structure of the title compound has been determined by means of X-ray diffraction. The crystal data and the final <I>R</I> value are: Cu(CCl<SUB>3</SUB>COO)<SUB>2</SUB>·3H<SUB>2</SUB>O, monoclinic <I>C</I>2⁄<I>c</I>, <I>a</I>=23.082(3), <I>b</I>=6.253(1), <I>c</I>=9.726(2) Å, β=94.67(1)°, <I>Z</I>=4, <I>R</I>=0.049. The structure consists of monomeric Cu(CCl<SUB>3</SUB>COO)<SUB>2</SUB>(H<SUB>2</SUB>O)<SUB>3</SUB> molecules, which are linked together by intermolecular O–H···O hydrogen bonds to form a layer parallel to (100). Each Cu(II) atom is coordinated by five oxygen atoms which form nearly a square pyramid; two oxygen atoms of two carboxylate ions and two water molecules form its basal plane and the remaining water molecule occupies the apical position. The mean basal Cu–O length is 1.961 Å and the apical one 2.183 Å. The Cu(II) atom is displaced from the basal plane by 0.110 Å toward the apical oxygen. Thermal analysis (DSC) disclosed two phase transitions at 163 and 207 K, their estimated molar enthalpies being about 0.4 and 0.7 kJ mol<SUP>−1</SUP>, respectively. At 77 K, 24 <SUP>35</SUP>Cl NQR signals are observed in the frequency range 38.7–40.3 MHz. The X-ray diffraction photographs for both low-temperature phases indicate the appearance of superstructures with less symmetrical space groups; the <I>b</I> spacing doubles below 207 K, while both <I>b</I> and <I>c</I> spacings double below 163 K.
- 公益社団法人 日本化学会の論文
著者
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Hashimoto Masao
Department Of Chemistry Faculty Of Science Kobe University
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Kiriyama Hideko
Department of Chemistry, Faculty of Science, Kobe University
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Okuno Nanami
Department of Chemistry, Faculty of Science, Kobe University
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