硫杂杯[4]芳烃氧化膦衍生物的合成与晶体结构  

Synthesis and Crystal Structure of Thiacalix[4]arene Substituted by Two Diphenylphosphinylmethoxy Groups [OCH_2P(O)Ph_2]

作　　者：马淑兰[1] 郭倩玲[2] 朱文祥[1] 赵明新[1] 张静[1] 刘迎春[1] 

机构地区：[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

出　　处：《化学学报》2005年第6期519-524,F008,共7页Acta Chimica Sinica

基　　金：北京市自然科学基金(No.2022011);北京师范大学青年基金(No.10770005)资助项目.

摘　　要：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Smart1000CCD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=1.215g/cm3,F(000)=1288,μ(MoKα)=0.244mm-1,R1=0.0625,wR2=0.1372.杯芳烃分子采取了锥式构象.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 I is C(66)H(7)O(6)P(2)S(4)center dot 2CH(3)OH. It belongs to triclinic crystal system, space group P <(1)over bar>, with a=1.3453(6) nm, b=1.5289(7), c=1.7893(9) nm, alpha=75.707(9)degrees, beta=69.131(8)degrees, gamma=79.734(9)degrees, Z=2, V=3.316(3) nm(3), d=1.215 g/cm(3), F(000) = 1288, mu(Mo K alpha) = 0.244 mm(-1), R-1=0.0625, wR(2)=0.1372. The compound adopts a cone conformation.

关 键 词：杯[4]芳烃 晶体结构 杯芳烃 亚甲基 空间群 CH3OH 叔丁基 氧化 合成 衍生物 

分 类 号：O627.51[理学—有机化学]