配合物[Cd(phen)_3]SO_4·3(Hhca)的合成、结构及其性能的表征

Syntheses,crystal structure and properties of [Cd(phen)_3]SO_4·3(Hhca)

以4-羟基肉桂酸（Hhca）,1,10-邻菲啰啉（phen）与硫酸镉（CdSO4.8H2O）反应得到了一个结构新颖的单核配合物[Cd（phen）3]SO4.3（Hhca）,元素分析、红外光谱、热重分析和单晶结构衍射等测试表征了它的结构,晶体结构分析表明它属于三方晶系,空间群R3 c,a=b=1.906 79（2）nm,c=2.542 8（3）nm,γ=120°,V=8.006 5（1）nm^3,Z=6,Dc=1.545 g/cm^3,F（000）=3 816,μ=62.7 mm^-1,R=0.037 3,wR=0.083 7,GOF=1.180.在该配合物中,Cd^2＋与phen形成六配位的配位构型,与Hhca并没有配位.Hhca与阴离子硫酸根通过氢键作用,使配合物形成了三维超分子孔洞结构,[Cd（phen）3]^2＋位于孔洞之中.更有意思的是,配合物的固体荧光谱在450-650nm展示了较强的宽峰,类似于白光发射峰,这可能与配合物的空间结构及氢键作用相关.

The reaction of CdSO4 · 8H2O, 4-hydroxycinnamic acid （Hhca） and 1,10-phenanthroline （phen） ligand afforded a novel mononuclear compound [ Cd （phen） 3 ] SO4·3（Hhca） which was characterized by IR, elemental analysis, TGA and single-crystal X-ray diffraction. X-ray crystallography analysis reveals that the compound is of trigonal, space group R3c, with a = b = 1. 906 79 （2）nm, c= 2.5428（3）nm,γ=120°, V=8.0065（1） nm^3,Z= 6,Dc = 1.545 g/cm^3,F（000） = 381 6,μ = 62.7 mm^-1 ,R =0. 037 3, wR =0. 083 7 and GOF = 1. 180. Hhca and sulfate H-bond to form a 3D supramolecular structure with large cavities and [ Cd （phen）3 ]^2＋ cations were occupied in voids. More interestingly, it exhibits a strong broad emission band from 450 - 650 nm in solid state.