SIOC English
化学学报
高级检索

化学学报 ›› 1997, Vol. 55 ›› Issue (10): 1009-1018. 上一篇    下一篇

研究论文

N-对R苯基氮杂15冠5八钼多酸钠超分子配合物的合成与结构

鲁晓明;刘顺诚;刘育;卜显和;洪少良   

  1. 首都师范大学化学系;南开大学化学系;北京微量化学所
  • 发布日期:1997-10-15

Synthesis and crystal structure of {Na[N-(p-RPh)15C5](Et2O)}2Na2Mo8O26

LU XIAOMING;LIU SHUNCHENG;LIU YU;BU XIANHE;HONG SHAOLIANG   

  • Published:1997-10-15

PDF

342

被引次数

7 | 3

为研究大环化合物对客体分子的选择性, 合成了通式为[NaL(Et2O)]2Na2Mo8O26的三种新型N-对R苯基氮杂15冠5八钼多酸钠超分子配合物(其中L分别为: N-苯基氮杂15冠5、N-对氯苯基氮杂15冠5和N-对甲苯基氮杂15冠5), 进行了元素分析, 红外光谱与核磁共振等结构参数的表征, 对R基为CH3的标题配合物作了X射线四圆衍射测定, 该晶体属单斜晶系, 空间群为P21/a,a=1.4590(4)nm, b=1.3817(3)nm, c=1.7639(5)nm, β=112.67(2)°, V=3.281(1)nm^3, Mr=2021.3, Dc=2.11g/cm^3,μ=2.37mm^-^1, F(000)=2048, R=0.045和Rw=0.057, 与[Na.(DB18C6)(CH3OH)M6O19和[Na(DB24C8)]2M6O19进行比较,结果表明: 大环化合物不仅对客体金属离子有分子识别性, 而且对与之抗衡的多酸阴离子也具有影响。

关键词: 红外分光光度法, 元素分析, 晶体结构, 核磁共振谱法, 氮杂环化合物, 冠醚

Three new supermolecular complexes of {Na[N-(p-RPh)15C5](Et2O)}2Na2Mo8O26 (R=H, Cl, CH3) were synthesized by reaction of N-(para-substituted phenyl)-aza-15-crown-5 with [(n-Bu)4N]4Mo8O26 and Na^+ in mixed solvent of CH3OH and CH3CN and crystallized in Et2O. The supermolecular complexes were characterized by C/H analysis, IR, and 1H NMR spectra and X-ray structure determination of {Na[N-(p-CH3Ph)15C5](Et2O)}2Na2Mo8O26. This crown ether octamolybdate is monoclinic, space group P21/a, a=1.4590(4)nm, b=1.3817(3)nm, c=1.7639(5)nm, β =112.67(2)°, V=3.281(1)nm^3, Mr=2021.3, Dc=2.11g/cm^3, μ=2.37mm^-^1, F(000)=2048, R=0.045 and Rw=0.057. Comparison with [Na.(DB18C6)(CH3OH)M6O19 and [Na(DB24C8)]2M6O19 (M=W and Mo), it was indicated that the host crown ether compounds could not only recongnize the guest-metal cations, but also choose counterion anions of polymolybdates with defferent degree of polymerization to combine into the crystals.

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, CRYSTAL STRUCTURE, NMR SPECTROMETRY, NITROGEN HETEROCYCLICS, CROWN ETHER

中图分类号: