一种新型三维包结物的合成和晶体结构

Synthesis and Crystal Structure of a New Three-dimensional Sandwich Inclusion Compound

以六氰合钴酸钾,五水硫酸铜和乙二胺为原料,通过采用不同溶剂、不同配比实验对比,合成了一种新的三维夹心配位包结物[Cu(en)2]2{K[Co(CN)6]}2 [en=乙二胺]晶体,对其进行了元素分析、红外光谱表征和单晶结构测定。X射线单晶衍射测定表明,该配位包结物属单斜晶系,C2／c空间群,晶胞参数为a=0.8406(3)nm.b=1.6906(5)nm,c=1.1803(4)nm,β=98.931(5)°,V=0.16570(9)nm3,Z=2,de=1.755g／cm3,μ=2.549mm-1,F(000)=884.R1=0.0323,wR2=0.0807。这种新的三维的夹心配位包结物由[Co(CN)6]3-与外界的K+离子通过氰根(-CN-)配位形成三维网络格子,在每个网格中镶嵌着二乙胺合铜(Ⅱ)配合物。

A three-dimensional sandwich inclusion compound [Cu(en)2]2{K[Co(CN)6]}2 was obtained as deep purple crystals by the reaction of K3[Co(CN)6], CuSO4·5H2O and NH2CH2CH2NH2 in 2:2:3 molar radio in an aqueous solution. The title compound was determined by elemental analysis, IR spectroscopy and X-ray single crystal diffraction. The crystal crystallized in monoclinic belongs to space group C2/c, α=0.8406(3) nm, b=1.6906(5) nm, c=1.1803(4) nm, β=98.931(5)°, V=0.16570(9) nm3, Z=2, dc=1.755 g/cm3, μ=2.549 mm-1, F(000)=884, R1=0.0323, wR2=0.0807. X-ray analysis displays that all the cyanide groups of [Co(CN)6]3- are involved in the coordination to adjacent K+ ions to form a three-dimensional network structure through order CN-bridges. [Cu(en)2]2+ cation is located in the center of each grid.