化学学报 ›› 2005, Vol. 63 ›› Issue (6): 519-524. 上一篇    下一篇

研究论文

硫杂杯[4]芳烃氧化膦衍生物的合成与晶体结构

马淑兰1,郭倩玲2,朱文祥*,1,赵明新1,张静1,刘迎春1   

  1. (1北京师范大学化学系 北京 100875)
    (2北京化工大学化学工程学院 北京 100029)
  • 收稿日期:2004-08-23 修回日期:2004-11-28 出版日期:2005-03-28 发布日期:2010-12-10
  • 通讯作者: 朱文祥

Synthesis and Crystal Structure of Thiacalix[4]arene Substituted by Two Diphenylphosphinylmethoxy Groups [OCH2P(O)Ph2]

MA Shu-Lan1, GUO Qian-Ling2, ZHU Wen-Xiang*,1, ZHAO Ming-Xin1, ZHANG Jing1, LIU Ying-Chun1   

  1. (1 Department of Chemistry, Beijing Normal University, Beijing 100875)
    (2 College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029)
  • Received:2004-08-23 Revised:2004-11-28 Online:2005-03-28 Published:2010-12-10
  • Contact: ZHU Wen-Xiang

合成了部分取代的硫杂杯[4]芳烃氧化膦衍生物, 二(亚甲基二苯基氧化膦)对叔丁基硫杂杯[4]芳烃(化合物1), 培养了化合物的单晶, 用Smart 1000 CCD衍射仪测定了其晶体结构. 结果表明, 1的组成为: C66H70O6P2S4•2CH3OH, 属三斜晶系, P1空间群, 晶胞参数a=1.3453(6) nm, b=1.5289(7) nm, c=1.7893(9) nm; α=75.707(9)°, β=69.131(8)°, γ=79.734(9)°, Z=2; V=3.316(3) nm3, d=1.215 g/cm3, F(000)=1288, μ (Mo Kα)=0.244 mm-1, R1=0.0625, wR2=0.1372. 杯芳烃分子采取了锥式构象.

关键词: 硫杂杯[4]芳烃, 氧化膦衍生物, 晶体结构

The lower-rim doubly substituted thiacalixarene, 5,11,17,23-tetra-tert-butyl-25,27-bis(diphenylphosphinylmethoxy)thiacalix[4]arene (compound 1), has been synthesized. The crystal structure of the compound was determined by X-ray diffraction. The result shows that the composition of compound 1 is C66H70O6P2S4•2CH3OH. It belongs to triclinic crystal system, space group P1, with a=1.3453(6) nm, b=1.5289(7), c=1.7893(9) nm, α=75.707(9)°, β=69.131(8)°, γ=79.734(9)°, Z=2, V=3.316(3) nm3, d=1.215 g/cm3, F(000)=1288, μ(Mo Kα)=0.244 mm-1, R1=0.0625, wR2=0.1372. The compound adopts a cone conformation.

Key words: thiacalix[4]arene, phosphinoxide, crystal structure