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机构地区:[1]宿州学院化学化工学院,宿州234000 [2]南京大学化学化工学院,配位化学国家重点实验室,人工微结构科学与技术协同创新中心,南京210093
出 处:《无机化学学报》2016年第4期706-712,共7页Chinese Journal of Inorganic Chemistry
基 金:国家自然科学基金(No.21371092);安徽高校省级自然科学研究重点项目(No.KJ2015A203);宿州学院自旋电子与纳米材料安徽省重点实验室开放课题(No.2014YKF51)资助
摘 要:以双(4-吡啶-4-苯基)胺(BPPA)和4,4-(六氟)双(苯甲酸)(H2hfipbb)或对苯二甲酸(p-H2bdc)为配体,采用溶剂热法与M(NO3)2·6H2O(M=Co、Zn)组装合成了2个新的配合物{[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1)、{[Zn2(BPPA)2(p-bdc)2]·H2O·DMF}n(2),利用元素分析、X射线粉末衍射(PXRD)、红外光谱等手段分别对它们进行了表征,并用X射线单晶衍射仪测定了配合物的单晶结构。X射线单晶衍射测定结果表明:配合物1和2均为二维结构。配合物1具有新的拓扑结构。配合物2的二维结构又可以组成三维框架结构。配合物1为正交晶系,Pnna空间群,a=2.640 9(2)nm,b=1.715 78(13)nm,c=1.504 11(11)nm,V=6.8154(9)nm3,Z=4,μ=0.571 mm-1,F(000)=2 592,Dc=1.245 g·cm-3,Mr=1 383.76,R1=0.066 6,w R2=0.208 9(I>2σ(I));配合物2为单斜晶系,C2/c空间群,a=2.796 70(9)nm,b=1.814 82(6)nm,c=2.303 13(7)nm,β=102.136 0(10)°,V=11.428 3(6)nm3,Z=8,μ=0.906 mm-1,F(000)=4 944,Dc=1.391 g·cm-3,Mr=1 196.85,R1=0.039 8,w R2=0.106 4(I>2σ(I))。此外,热重分析表明配合物1和2均具有良好的热稳定性。Two complexes {[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1) and {[Zn2(BPPA)2( p-bdc)2]·H2O·DMF}nwere synthesized by solvothermal method using bis(4-(pyridin-4-yl)phenyl)amine(BPPA), 4,4′-(hexafluoroisopropylidenene)bis(benzoic acid)(H2hfipbb), terephthalic acid( p-H2bdc) and M(NO3)26H2O(M =Co, Zn), respectively. The complexes were characterized by elemental analysis, IR spectra, XRD and TGA, and the crystal structures were determined by single-crystal X-ray diffraction. Crystal structures were determined by single-crystal X-ray diffraction. Structural analyses reveal that complexes 1 and 2 exhibit a two-dimensional(2D) framework structure.Complex 1 represents new 6-connected net with Point Symbol of(411.64), and the complex 2 assembles into a 3D supramolecular network. Complex 1 crystallizes in the monoclinic system, space group Pnna, with cell parameter:a=2.640 9(2) nm, b=1.715 78(13) nm, c=1.504 11(11) nm, V=6.815 4(9) nm^3, Z=4, μ=0.571 mm^-1, F(000)=2 592,Dc=1.245 g·cm^-3, Mr=1 383.76, R1=0.066 6, and wR2=0.208 9(I〉2σ(I)); Complex 2 crystallizes in the monoclinic system, space group C2/c, with cell parameter: a=2.796 70(9) nm, b=1.814 82(6) nm, c=2.303 13(7) nm, β=102.136 0(10)°, V=11.428 3(6) nm^3, Z=8, μ=0.906 mm-1, F(000)=4 944, Dc=1.391 g·cm^-3, Mr=1 196.85, R1=0.0398, and wR2=0.106 4(I〉2σ(I)). Additionally, complexes 1 and 2 display good thermal stability.
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