水热合成三维超分子配位聚合物[Cd(C_2O_4)(H_2O)_2]·H_2O及晶体结构  

Hydrothermal Synthesis of a Three-dimensional Supramolecular [Cd(C_2O_4)(H_2O)_2]·H2O and Crystal Structure

作　　者：于连香[1] 马奎蓉[1] 范勇[1] 张萍[1] 

机构地区：[1]吉林大学化学学院无机合成与制备化学国家重点实验室,长春130012

出　　处：《人工晶体学报》2007年第1期146-151,共6页Journal of Synthetic Crystals

基　　金：国家自然科学基金(No.3A405F281412)资助

摘　　要：在水热条件下,制备了二维层状配位聚合物[Cd(C2O4)(H2O)2].H2O(1)的单晶体,对其进行了X射线粉末衍射、元素分析、红外光谱、热重分析和X射线单晶衍射测定。单晶结构分析表明,该晶体属于三斜晶系,P-1空间群,晶胞参数a=0.60109(12)nm,b=0.66607(13)nm,c=0.84987(17)nm,α=74.72(3)°,β=74.33(3)°,γ=81.07(3)°,V=0.31473(11)nm3,Z=2,R1=0.015,ωR2=0.0368。草酸镉单晶结构由两个2D层构成,每一个2D层是由[Cd2(C2O4)2(H2O)4].2H2O的重复单元形成,每个单元是由一个七配位独立镉原子配位而成(五个草酸氧原子和两个水分子氧原子)。2D层与层之间通过不同层草酸分子与配位水分子之间及草酸与客体水分子之间形成的氢键将2D层状化合物连成一个3D超分子结构。热重分析表明该配位聚合物在340℃下稳定。A 3 D supramolecular [ Cd （ C2O4 ） （ H2 O） 2 ]·H2O （ 1 ） was synthesized under the hydrothermal condition. Its structure was determined by single crystal X-ray diffraction analysis, and further characterized by XRD, ICP, IR, TG and elemental analysis. The title compound crystallizes in triclinic space group P-1 ,with a = 0. 60109 （ 12 ） nm, b = 0. 66607 （ 13 ） nm, c = 0. 84987 （ 17 ） nm, α = 74.72 （3）°,β =74.33 （3）°,γ = 81.07（3）°, Ⅴ =0. 31473（ 11 ） nm^3 ,Z =2,R1 =0. 015,ωR2 =0. 0368. The cadmium（ Ⅱ ） atoms in the compound 1 are in a seven-coordinate environment of five oxalate and two water oxygens. The coordination geometry about each metal atom is approximately that of a pentagonal bipyramid with a water and an oxalate oxygen in the apical positions. The crystal structure consists of twodimensional arrays formed by the [ Cd2 （C2O4 ）2 （H2O）4 ]·2H2O repeat unit. Layers are further interlinked via hydrogen bonds between oxygen atoms and waters to form three-dimensional supramolecular. The TGA-DTA data shows the compound 1 has good thermal stability.

关 键 词：水热合成 3D超分子 晶体结构 

分 类 号：O78[理学—晶体学]