2,3-双-(2-吡啶)喹喔啉-CuⅡ配合物的合成、表征及晶体结构

报道了配合物[Cu(DPQ)2(ClO4)](ClO4)·H2O·0.5CH2Cl2·CHCl3(DPQ=2,3-双-(2-吡啶)喹喔啉)的合成及表征(元素分析、电导、红外和紫外光谱).室温X-射线单晶衍射分析结果表明,标题配合物(C37.5H28Cl6CuN8O9,分子量=1010.92)处于正交晶系,Pmmn空间群,a=1.0547(2)nm,b=1.1819(2)nm,c=2.0014(4)nm,V=2.4949(9)nm,Z=2,Dc=1.346g/cm3,F(000)=1024,μ(MoKα)=0.813mm-1.最终精修得到的R及wR因子分别为0.0452和0.1070,独立衍射点个数为2367.配合物由分立的[Cu(DPQ)2(ClO4)] 阳离子,未配位的ClO4-阴离子和溶剂分子组成.中心Cu 离子分别与两个DPQ配体上的4个吡啶氮原子以及高氯酸根上的一个氧原子配位,其配位几何构型为理想四方锥.两个DPQ配体仅通过吡啶氮原子与Cu 离子螯合配位,形成两个七元环.此外,结构中两个平行喹喔啉环之间存在着π…π堆积相互作用.

Synthesis, Characterization and Crystal Structure of a CuⅡ Complex with 2,3-Di-2-Pyridylquinoxaline (DPQ)

The title complex [Cu(DPQ)2(ClO4)](ClO4)·H2O·0.5CH2Cl2·CHCl3 (DPQ=2,3-di-2-pyridylquinoxaline) has been synthesized and characterized by elemental analysis, conductivity, infrared and UV-vis spectra. X-ray diffraction analysis at room temperature indicates that the complex (C37.5H28Cl6CuN8O9, Mr=1 010.92) crystallizes in orthorhombic system, space group Pmmn with a=1.054 7(2) nm, b=1.181 9(2) nm, c=2.001 4(4) nm, V=2.494 9(9) nm3, Z=2, Dc=1.346 g/cm3, F(000)=1 024, μ(MoKα)=0.813 mm-1. The final R and wR factors are 0.045 2 and 0.107 0, respectively with 2 367 independent reflections. The title complex is composed of discrete [Cu(DPQ)2(ClO4)]+ cations, uncoordinated ClO4- counter anions and solvent molecules. The central CuⅡ atom is penta-coordinated by four nitrogen donors of the pyridine rings of two DPQ and an oxygen atom of the perchlorate, and the coordination geometry of CuⅡ could be considered as an ideal square-pyramidal environment. Both DPQ ligands chelated the CuⅡ atom by forming two seven-membered rings involving only the N-atoms of the pyridine rings and there exists intramolecular π…π interaction between the two parallel quinoxaline rings.