基于新型甜菜碱类芳香多羧酸配体的配位聚合物：合成、结构和性质研究
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摘要
以多羧酸类配体构筑的配位聚合物以其丰富多样的结构,美丽多变的拓扑结构及其在包括光化学、吸附、催化、和磁性等领域广泛而诱人的潜在的应用价值而成为近年来化学和材料工作人员研究热点之一。本论文致力于利用三个新型甜菜碱类芳香多羧酸配体和含氮辅助配体与过渡或稀土金属离子来构筑具有迷人结构的配位聚合物。采用水热、溶剂热等合成方法,共合成了27个结构新颖的配位聚合物。另外通过元素分析,R和X-射线单晶衍射对化合物的结构进行了表征,并对配位聚合物的热稳定性、相纯度和荧光性质以及部分配合物的非线性光学性能进行了研究。
本论文主要包括以下两个部分：
一、利用刚性的H2L1(3-(4-羟基吡啶基)-1,2-邻苯二甲酸)及柔性H2L2(5-(4-羟基吡啶基-1-甲基)-1,3-间苯二甲酸)与Zn(Ⅱ)、Cd(Ⅱ)在不同含氮辅助配体的协同作用下,制备了十个具有多样性螺旋片段的配位聚合物。其中得到了一个含有三重共轴螺旋体系的手性配位聚合物{[Cd(L1)(p-bix)]·1.75H20}n(1).配合物1是目前合成的重数最多的螺旋配合物,而且三重共轴螺旋体系是通过逐级诱导组装形成的,这为等级组装配位聚合物提供了很好的范例。配合物[Cd(L1)(CH30H)(H20)]n(2)的两种螺旋链是由L12-及L12-上的邻苯二甲酸基团分别与金属离子Cd(II)配位形成的；配合物{[Cd(L1)(1,4-bbi)].(H20)}n(3)中的超分子螺旋链是由配体L12-与游离水通过氢键形成的；配合物{[Cd(L1)(m-bix)(H20)]·(H2O)2}n(4)则形成了一个迷人的夹心型螺旋带,而且它们通过螺旋水链连接成三维超分子网络,这是目前报道的为数不多的结构类型；配合物[Zn(L1)(4,4'-bpy)0.5]n(5)中存在一种meso-螺旋;而配合物[Zn(L1)(bpp)]n(6)中螺旋链则是由含氮辅助配体和金属Zn(Ⅱ)通过配位键连接而成的。配合物{[Cd(L2)(p-bix)(H20)]·H20}n(7)是第一例由一维螺旋管构筑的1D→2D的插指形结构；配合物{[Zn(L2)(H2O)]·H2O}n(8)是由手性面通过ABAB堆积形成的内消旋的三维超分子结构；配合物{[Zn(L2)(p-bix)]·3.5H2O}n(9)是少见报道的由二维螺旋面构筑的2D→3D的插指形结构；配合物{[Zn(L2)(4,4'-bpy)0.5]·2H2O}n(10)是含有螺旋特征的层柱状三重穿插网络。
二、基于刚性的H2L1(3-(4-羟基吡啶基)-1,2-邻苯二甲酸)、柔性的H2L2(5-(4-羟基吡啶基-1-甲基)-1,3-间苯二甲酸)与镧系离子在草酸配体的协同作用下构筑了十七个含有双核金属单元的配位聚合物{[Ln(L1)(OX)0.5(H2O)2]·3H2O}n (11-12)、[Ln(L1)(OX)0.5(H2O)3]n(13-21)和{[Ln2(L2)(OX)2(H2O)3]·6H2O}n(22-27)。结构分析表明11-21它们可分为两大类,但是根据配合物中双核金属单元不同,它们又可分为四组。随着金属离子半径的减小,金属离子的配位数逐渐减少,Ln-O键平均键长逐渐变短。总的来讲,配合物11-21结构的差异是镧系收缩造成的。另外,我们还研究了刚性的H2L1对Eu、Tb、Dy配合物的敏化发光性能。结构分析22-27是异质同晶的,它们都属于单斜晶系P21空间群。对它们的Ln-O键键长及单胞参数分析印证了镧系收缩效应。此外对它们进行了荧光及非线性光学性能的研究。与此同时我们根据当前在掺杂稀土有机配合物中发现了从一种镧系离子到另一种镧系离子间的能量传递可以导致发光变化的现象,制备了一系列Eu-Tb掺杂的配合物。通过粉末衍射分析,表明它们的结构与22-27是类似的。Eu-Tb
In recent years, the coordination polymers based on multi-carboxylate acid, as one of the most intense studied areas for chemists, physicists, and materials scientists, have been extensively explored and realized for their aesthetics of crystalline architectures and their potential functions in luminescence, non-linear optics, adsorption, magnetism, and catalysis. In this paper, with the aim of construct of novel coordination polymers with intriguing structural motifs and good properties, three novel multi-carboxylate betaines (H2L1、H2L2、H2L3) and N-donor ancillary coligands were selected to prepare27complexes in the cooperation of metal ions. These complexes were characterized with X-ray single crystal diffraction, IR, elemental analysis. Furthermore, their thermal stabilities, phase purity, photoluminescence, as well as non-linear optics of some compounds were studied.
1. Ten Zn(Ⅱ)/Cd(Ⅱ) coordination polymers with helical su8bunits was assembled from the mixed liagnds of H2L1(H2L2) and N-donor ancillary coligands. Complex1with homochiral triple concentric helical system has been obtained. Based on our understanding of the coordination with multi-concentric helical system, complex1with triple concentric helical system is the first example. Compound2displays a layered structure containing two kinds of helical chains. Compound3features a3D supramolecular framework embodying a type of supramolecular helical chain. Compound4exhibits a metal-organic ribbon structure with two kinds of helical chains. Compound5features a3D architecture in which a1D lemniscate shape pseudo meso-helix chain is observed. Compound6exhibits a2D achiral layer in which the1D (Zn-bpp)n helical chains are alternately arranged in a right-and left-handed sequence. Compound7displays a1D→2D interdigitated architecture constructed from unique1D independent helical tubes. Compound8is a layered structure with two helical chains. Compound9is also a layered coordination polymer with two types of helical chains and features interesting2D→3D interdigitated architecture. Compound10exhibits a3D3-fold interpenetrating framework with pillared helical-layers.
2. Seventeen Ln(Ⅲ) coordination polymers with dinuclear SBUs based on H2L1(H2L2) and oxalic acid were hydrothermally synthesized. The single-crystal X-ray analyses of the complexes (11-21) reveal that they all have a2D layer structure with different dinuclear SBUs and crystallize in the same triclinic space group P-1. Two kinds of these complexes can be classified by their composition, meanwhile, four groups can be divided by different dinuclear SBUs in them. The average band length of Ln-O in each group and the coordination numbers of the Ln(Ⅲ) ions are decreased by the increase of atomic number. In general, the different structural features of11-21may be related to the ionic size of different lanthanide ions, the so-called "lanthanide contraction". In addition, the luminescent properties of Eu、Tb、Dy compounds have also been investigated in detail. The single-crystal X-ray analyses of the complexes (22-27) reveal that they all crystallize in the same monoclinic space group P21. The result of the analysis with the everage Ln-O band length and cell parameters confirmed the effect of "lanthanide contraction". As is known, energy transfers from one lanthanide to another lanthanide ion have been observed to enhance the luminescence intensity in heterolanthanide coordination polymers. We successfully obtained the functional luminescent MOF materials by doping isostructural Eu3+into Tb3+compounds to tune the emission colors by changing the doped Eu3+concentration. Therefore, the photoluminescence color of the Eu3+doped MOF canbe tuned from green-yellow to yellow, orange, and red-orange, and the corresponding CIE chromaticity coordinates change from (0.368,0.518) to (0.550,0.341) by changing the doping concentration of the Eu3+ions.
本论文主要包括以下两个部分：
一、利用刚性的H2L1(3-(4-羟基吡啶基)-1,2-邻苯二甲酸)及柔性H2L2(5-(4-羟基吡啶基-1-甲基)-1,3-间苯二甲酸)与Zn(Ⅱ)、Cd(Ⅱ)在不同含氮辅助配体的协同作用下,制备了十个具有多样性螺旋片段的配位聚合物。其中得到了一个含有三重共轴螺旋体系的手性配位聚合物{[Cd(L1)(p-bix)]·1.75H20}n(1).配合物1是目前合成的重数最多的螺旋配合物,而且三重共轴螺旋体系是通过逐级诱导组装形成的,这为等级组装配位聚合物提供了很好的范例。配合物[Cd(L1)(CH30H)(H20)]n(2)的两种螺旋链是由L12-及L12-上的邻苯二甲酸基团分别与金属离子Cd(II)配位形成的；配合物{[Cd(L1)(1,4-bbi)].(H20)}n(3)中的超分子螺旋链是由配体L12-与游离水通过氢键形成的；配合物{[Cd(L1)(m-bix)(H20)]·(H2O)2}n(4)则形成了一个迷人的夹心型螺旋带,而且它们通过螺旋水链连接成三维超分子网络,这是目前报道的为数不多的结构类型；配合物[Zn(L1)(4,4'-bpy)0.5]n(5)中存在一种meso-螺旋;而配合物[Zn(L1)(bpp)]n(6)中螺旋链则是由含氮辅助配体和金属Zn(Ⅱ)通过配位键连接而成的。配合物{[Cd(L2)(p-bix)(H20)]·H20}n(7)是第一例由一维螺旋管构筑的1D→2D的插指形结构；配合物{[Zn(L2)(H2O)]·H2O}n(8)是由手性面通过ABAB堆积形成的内消旋的三维超分子结构；配合物{[Zn(L2)(p-bix)]·3.5H2O}n(9)是少见报道的由二维螺旋面构筑的2D→3D的插指形结构；配合物{[Zn(L2)(4,4'-bpy)0.5]·2H2O}n(10)是含有螺旋特征的层柱状三重穿插网络。
二、基于刚性的H2L1(3-(4-羟基吡啶基)-1,2-邻苯二甲酸)、柔性的H2L2(5-(4-羟基吡啶基-1-甲基)-1,3-间苯二甲酸)与镧系离子在草酸配体的协同作用下构筑了十七个含有双核金属单元的配位聚合物{[Ln(L1)(OX)0.5(H2O)2]·3H2O}n (11-12)、[Ln(L1)(OX)0.5(H2O)3]n(13-21)和{[Ln2(L2)(OX)2(H2O)3]·6H2O}n(22-27)。结构分析表明11-21它们可分为两大类,但是根据配合物中双核金属单元不同,它们又可分为四组。随着金属离子半径的减小,金属离子的配位数逐渐减少,Ln-O键平均键长逐渐变短。总的来讲,配合物11-21结构的差异是镧系收缩造成的。另外,我们还研究了刚性的H2L1对Eu、Tb、Dy配合物的敏化发光性能。结构分析22-27是异质同晶的,它们都属于单斜晶系P21空间群。对它们的Ln-O键键长及单胞参数分析印证了镧系收缩效应。此外对它们进行了荧光及非线性光学性能的研究。与此同时我们根据当前在掺杂稀土有机配合物中发现了从一种镧系离子到另一种镧系离子间的能量传递可以导致发光变化的现象,制备了一系列Eu-Tb掺杂的配合物。通过粉末衍射分析,表明它们的结构与22-27是类似的。Eu-Tb
In recent years, the coordination polymers based on multi-carboxylate acid, as one of the most intense studied areas for chemists, physicists, and materials scientists, have been extensively explored and realized for their aesthetics of crystalline architectures and their potential functions in luminescence, non-linear optics, adsorption, magnetism, and catalysis. In this paper, with the aim of construct of novel coordination polymers with intriguing structural motifs and good properties, three novel multi-carboxylate betaines (H2L1、H2L2、H2L3) and N-donor ancillary coligands were selected to prepare27complexes in the cooperation of metal ions. These complexes were characterized with X-ray single crystal diffraction, IR, elemental analysis. Furthermore, their thermal stabilities, phase purity, photoluminescence, as well as non-linear optics of some compounds were studied.
1. Ten Zn(Ⅱ)/Cd(Ⅱ) coordination polymers with helical su8bunits was assembled from the mixed liagnds of H2L1(H2L2) and N-donor ancillary coligands. Complex1with homochiral triple concentric helical system has been obtained. Based on our understanding of the coordination with multi-concentric helical system, complex1with triple concentric helical system is the first example. Compound2displays a layered structure containing two kinds of helical chains. Compound3features a3D supramolecular framework embodying a type of supramolecular helical chain. Compound4exhibits a metal-organic ribbon structure with two kinds of helical chains. Compound5features a3D architecture in which a1D lemniscate shape pseudo meso-helix chain is observed. Compound6exhibits a2D achiral layer in which the1D (Zn-bpp)n helical chains are alternately arranged in a right-and left-handed sequence. Compound7displays a1D→2D interdigitated architecture constructed from unique1D independent helical tubes. Compound8is a layered structure with two helical chains. Compound9is also a layered coordination polymer with two types of helical chains and features interesting2D→3D interdigitated architecture. Compound10exhibits a3D3-fold interpenetrating framework with pillared helical-layers.
2. Seventeen Ln(Ⅲ) coordination polymers with dinuclear SBUs based on H2L1(H2L2) and oxalic acid were hydrothermally synthesized. The single-crystal X-ray analyses of the complexes (11-21) reveal that they all have a2D layer structure with different dinuclear SBUs and crystallize in the same triclinic space group P-1. Two kinds of these complexes can be classified by their composition, meanwhile, four groups can be divided by different dinuclear SBUs in them. The average band length of Ln-O in each group and the coordination numbers of the Ln(Ⅲ) ions are decreased by the increase of atomic number. In general, the different structural features of11-21may be related to the ionic size of different lanthanide ions, the so-called "lanthanide contraction". In addition, the luminescent properties of Eu、Tb、Dy compounds have also been investigated in detail. The single-crystal X-ray analyses of the complexes (22-27) reveal that they all crystallize in the same monoclinic space group P21. The result of the analysis with the everage Ln-O band length and cell parameters confirmed the effect of "lanthanide contraction". As is known, energy transfers from one lanthanide to another lanthanide ion have been observed to enhance the luminescence intensity in heterolanthanide coordination polymers. We successfully obtained the functional luminescent MOF materials by doping isostructural Eu3+into Tb3+compounds to tune the emission colors by changing the doped Eu3+concentration. Therefore, the photoluminescence color of the Eu3+doped MOF canbe tuned from green-yellow to yellow, orange, and red-orange, and the corresponding CIE chromaticity coordinates change from (0.368,0.518) to (0.550,0.341) by changing the doping concentration of the Eu3+ions.
引文
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