两个基于双(4-吡啶-4-苯基)胺的钴(Ⅱ)、锌(Ⅱ)配合物的合成和晶体结构 |
Syntheses, Crystal Structures of Two Cobalt(Ⅱ)/Zinc(Ⅱ) Complexes Based on Bis(4-(pyridin-4-yl) phenyl) amine |
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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=2.6409(2)nm,b=1.71578(13)nm,c=1.50411(11)nm,V=6.8154(9)nm3,Z=4,μ=0.571 mm-1,F(000)=2592,Dc=1.245 g·cm-3,Mr=1383.76,R1=0.0666,ωR2=0.2089(I>2σ(I));配合物2为单斜晶系,C2/c空间群,a=2.79670(9)nm,b=1.81482(6)nm,c=2.30313(7)nm,β=102.1360(10)°,V=11.4283(6)nm3,Z=8,μ=0.906 mm-1,F(000)=4944,Dc=1.391 g·cm-3,Mr=1196.85,R1=0.0398,ωR2=0.1064(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。 |
关键词: 钴(Ⅱ)配合物 锌(Ⅱ)配合物 合成 晶体结构 |
基金项目: 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)和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。 |
Abstract: Two complexes{[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1) and {[Zn2(BPPA)2(p-bdc)2]·H2O·DMF}n were synthesized by solvothermal method using bis(4-(pyridin-4-yl) phenyl) amine(BPPA), 4, 4'-(hexafluoroisopropyliden-ene) 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=2.6409(2) nm, b=1.71578(13) nm, c=1.50411(11) nm, V=6.8154(9) nm3, Z=4, μ=0.571 mm-1, F(000)=2592, Dc=1.245 g·cm-3, Mr=1383.76, R1=0.0666, and ωR2=0.2089(I>2σ(I)); Complex 2 crystallizes in the monoclinic system, space group C2/c, with cell parameter:a=2.79670(9) nm, b=1.81482(6) nm, c=2.30313(7) nm, β=102.1360(10)°, V=11.4283(6) nm3, Z=8, μ=0.906 mm-1, F(000)=4944, Dc=1.391 g·cm-3, Mr=1196.85, R1=0.0398, and ωR2=0.1064(I>2σ(I)).Additionally, complexes 1 and 2 display good thermal stability. CCDC:1434213, 1; 1434214, 2. |
Keywords: Co(Ⅱ) complex Zn(Ⅱ) complex crystal structure synthesis |
投稿时间:2015-11-06 修订日期:2015-12-16 |
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张春丽,郑和根.两个基于双(4-吡啶-4-苯基)胺的钴(Ⅱ)、锌(Ⅱ)配合物的合成和晶体结构[J].无机化学学报,2016,32(4):706-712. |
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