高等学校化学学报

高等学校化学学报

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硫酰杯[4]芳烃羧酸类衍生物及其配合物的合成、晶体结构与表征

郭倩玲1, 屈一新1, 马淑兰2, 朱文祥2
   

    1. 北京化工大学化学工程学院, 北京 100029;
    2. 北京师范大学化学系, 北京 100875
  • 收稿日期:2005-12-29 修回日期:1900-01-01 出版日期:2006-11-10 发布日期:2006-11-10
  • 通讯作者: 屈一新

Synthesis, Crystal Structure and Characterization of Carboxylic Derivatives of Sulfonylcalix[4]arene

GUO Qian-Ling1, QU Yi-Xin1, MA Shu-Lan2, ZHU Wen-Xiang2   

    1. College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029, China;
    2. Department of Chemistry, Beijing Normal University, Beijing 100875, China
  • Received:2005-12-29 Revised:1900-01-01 Online:2006-11-10 Published:2006-11-10
  • Contact: QU Yi-Xin

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被引次数

10

摘要： 合成了5,11,17,23-四叔丁基-25,26,27-三[(乙酯基)甲氧基]-2,8,14,20-四硫酰杯[4]芳烃(L1)和5,11,17,23-四叔丁基-25,26,27-三(氧基乙酸)-2,8,14,20-四硫酰杯[4]芳烃(L2)及L2的稀土配合物, 采用元素分析、紫外光谱、红外光谱和1H NMR对其结构进行了表征. 用SMART 1000 CCD X射线衍射仪测定了L1的晶体结构. 结果表明, L1组成为: C52H65KO18S4·0.5H2O, 属三斜晶系, P1空间群, 晶胞参数a=1.2607(6) nm, b=1.5820(8) nm, c=1.6480(8) nm; α=83.720(8)°, β=69.327(8)°, γ=79.342(9)°, Z=2, V=3.019(3) nm3, Dc=1.270 g/cm3, F(000)=1218, μ=0.293 mm-1, R1=0.0937, wR2=0.2580. 杯芳烃分子采取部分锥式构象.

关键词: 硫酰杯[4]芳烃, 羧酸类衍生物, 稀土配合物, 晶体结构

Abstract: The lower-rim partially substituted sulfonylcalix[4]arenes, 5,11,17,23-tetra-tert-butyl-25,26,27-tris[(ethoxycarbonyl)methoxy]-2,8,14,20-tetrasulfonylcalix[4] arene(L1) and 5,11,17,23-tetra-tert-butyl-25,26,27-tris(oxyacetic acid)-2,8,14,20-tetrasulfonyl calix[4]arene(L2), and the complexes of L2 were synthesized and characterized. The crystal structure of L1 was determined by X-ray diffraction. The results show that the composition of it is C52H65KO18S4·0.5H2O. It belongs to triclinic crystal system, P1 space group, with a=1.2607(6) nm, b=1.5820(8) nm, c=1.648 0(8) nm, α=83.720(8)°, β=69.327(8)°, γ=79.342(9)°, Z=2, V=3.019(3) nm3, Dc=1.270 g·cm-3, F(000)=121.8, μ=0.293 mm-1, R1=0.0937, wR2=0.2580. The calix[4]arene adopts a partial cone conformation.

Key words: Sulfonylcalix[4]arene, Carboxylic derivative, Rare earth complex, Crystal structure

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