化学学报 ›› 1996, Vol. 54 ›› Issue (6): 562-567. 上一篇    下一篇

研究论文

含N, O和S的Schiff碱配体的双核锌配合物的合成与晶体结构

马长勤;王绪宁;张文兴;于正刚;蒋德华;董士利   

  1. 山东大学化学学院;淄博市公安局
  • 发布日期:1996-06-15

Synthesis and crystal structure of dinuclear zinc complex with Schiff base ligand containing N, O, and S dornors

MA CHANGQIN;WANG XUNING;ZHANG WENXING;YU ZHENGGANG;JIANG DEHUA;DONG SHILI   

  • Published:1996-06-15

本文合成了具有隔室构造的Schiff碱配体H3L(L^3^-=C11H11N6OS2^3^-), 并对其进行了元素分析, IR, ^1H NMR和MS等项表征。制备了该配体的分别由醋酸根和吡啶分子协配的两种锌的双核配合物, 对后者进行了X射线单晶结构分析。[Zn2L(OH)(py)2](py)2, P21/c, a=0.9195(1), b=2.3334(6), c=1.6111(3)nm,β=93.99(1)°, Z=4。结构用直接法解得, 最终的R=0.066。测定的结果表明,两锌原子间存在酚氧和羟基的两μ2-O-桥, 每个五配位的锌均具有四方锥型的配位构型。

关键词: 吡啶 P, 红外分光光度法, 元素分析, 锌络合物, 晶体结构, X射线衍射分析, 质谱法, 质子磁共振谱法, 席夫碱

A compartmental Schiff base ligand H3L (L^3^-=C11H11N6OS2^3^-) has been synthesized and characterized by elemental analysis, ^1H NMR, IR and MS as well as etc.. Its dinuclear zinc complex, which are co- coordinated by acetate radicals and pyridine molecules respectively, have been prepared. For the later the single crystal structure has been determinated by X-ray diffraction. [Zn2L(OH)(py)2](py)2, P21/c, a=0.9195(1), b=2.3334(6), c=1.6111(3), β=93.99(1)°, Z=4. The structure was solved by direct method. The refinement converges with R=0.066 and Rw=0.070 based on 2028 reflections with I>=3σ(I). The results indicate that between two zinc atoms exist two μ2-O^- bridges formed by a phenolic oxygen atom and a hydroxy group in the lattice, respectively; and every five-coordinate zinc atom possesses a square pyramidal construction.

Key words: PYRIDINE P, INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, ZINC COMPLEX, CRYSTAL STRUCTURE, X-RAY DIFFRACTION ANALYSIS, MASS SPECTROGRAPHY, PROTON MAGNETIC RESONANCE SPECTROMETRY, SCHIFF BASE

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