基于一个柔性三酸配体设计和调控配位聚合物的结构及维度的研究
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摘要
随着配位化学的不断发展,具有特定结构和功能的配位聚合物已经成为该领域的研究热点。在气体吸附、分子离子识别以及选择催化等方面有卓越表现的金属有机框架化合物(MOFs)更是受到了研究者们的广泛关注。配位聚合物拥有零维、一维、二维、三维以及很多新颖的穿插缠绕结构,不同的结构更是对应的不同的性能表现。MOFs材料的孔道形状、孔道尺寸以及孔表面官能团等因素直接决定了最终的性能。因此,如何定向的设计和组装不同结构的配位聚合物或MOFs材料是该领域的重大挑战。在配位聚合物的组装过程中,很多因素都会对其最终结构造成影响,那么如何有效的使用这些手段,而不是被它们制约仍旧需要深入的研究。
本论文致力于这部分研究内容,选择了1,3-双(4’-羧基苯氧基)苯甲酸(H3cpbda)作为配体合成了17例配位聚合物。其中通过与不同的过渡金属离子组装了系列的超分子异构体以及异质同晶体,并且通过引入刚性含氮辅助配体组装了一系列不同维度的配位聚合物等。文中深入研究了不同系列结构之间的构效关系以及其影响因素,主要的研究结果有：
1.选取金属Mn2+离子与柔性的三齿配体H3cpbda作为构筑模块,通过系统的改变溶剂体系、温度以及反应器,实现了一系列超分子异构体的调控和合成。当配体采取不同的“T”型以及“Y”型的分子构型时,会拓展出“矩形”和“菱形”的一维孔道。对比三维的超分子异构体MOFs材料的孔隙率,发现配合物6>配合物1>配合物4>配合物3,符合溶剂分子尺寸(H2O MeOH> DMF> DMP)的顺序。说明溶剂分子尺寸越大或者极性越小,倾向于得到孔隙率较大的结构。
2.选取金属Mn2+和金属Co2+与H3cpbda作为构筑模块,通过溶剂体系的调控实现了两组二维及三维的异质同晶现象的调控。对比三维结构中的孔隙率,配合物6>配合物7>配合物8。在二维结构中,由于溶剂分子填充于孔道中支撑骨架,导致孔道的形状以及孔隙率均发生改变。对比孔道尺寸和孔隙率,配合物9<配合物10<配合物11。两组配合物均符合溶剂分子尺寸(DMF DMA> DMP)的顺序。在异质同晶体间得到了与超分子异构体相似的结论：溶剂分子尺寸越大或者极性越小,倾向于得到孔道尺寸以及孔隙率较大的结构。
3.选取金属Cd2+离子与H3cpbda作为构筑模块的同时,添加了一组刚性含氮辅助配体,螯合配体(Phen和2,2'-bipy)和桥连配体(4,4'-bipy和Bpe),实现了对配位聚合物维度的调控(1D,2D,3D)。在该组配合物中出现了新的“M”型构型,它属于降低维数的因素。另外,桥连辅助配体属于拓展维度和稳定结构的因素,封端辅助配体属于典型的降低维数的因素。通过这一系列不同维度配合物的调控验证了柔性配体的分子构型以及刚性辅助配体的种类对最终结构维度的重要影响。除此之外对荧光的研究发现,刚性辅助配体的选择促进了配合物的红移现象,其中引入封端配体的红移小,引入桥连配体的红移大。
4.基于柔性三齿配体H3cpbda,分别与金属离子Mn2+和Zn2+通过不同的反应方法以及溶剂体系分别合成了两组疏途同晶结构,先前关于疏途同晶现象的报道中虽然晶体的结构相同,但是宏观的晶体形貌(形状和尺寸)完全不同。本文中的两组实验方案均得到了相似的晶体形貌及产率。这是由于本文选取的柔性配体H3cpbda能够更好的适应外界溶剂及环境,在结晶过程中形成了形貌相似。说明晶体的宏观形貌的变化不仅与溶剂体系有关,它还与选择的配体种类有关。
本文的研究内容为如何调控配合物的超分子异构和异质同晶现象,定向的合成不同结构和性能的配位聚合物提供了理论依据,具有非常重要的意义。
Coordination polymers not only have variform charming structures, such as1D,2D,3D structures and novel interpenetrating or intertwine structures, but also possess various functions. Design and construction of the metal-organic frameworks (MOFs) have become an attractive prospect for their potential applications in gas absorption, separation, molecular sensing, and catalysis. As we known, the porous shape, dimensions and function groups are key factors for the applications of MOFs, and lots of factors can influence the final structure of MOFs, such as pH values, solvents temperature and so on. Therefore, the targeted design and assembly coordination polymers or MOFs is still a great challenge, which is urgent need to be intensive researched. Besides, the rational selection of metal cations and organic ligands with suitable shape, size, symmetry, functional groups and flexibility is considered to be a pivotal role to construct MOFs
In this dissertation, the1,3-bis(4'-carboxyl phenoxy)benzoic acid (H3cpbda) is choosen as main building block, and successfully construct17coordination polymers. H3cpbda react with different transition metal ions, result various supramolecular isomers and isomorphor. When a series of rigid N-donor ligand is introduced to the react systerm, five vari-dimension coordination polymers are synthesized. The properties and influence factor are intensively discussed. The major contents of this dissertation are listed as follows:
(1) H3cpbda reacts with Mn2+, and results a series of supramolecular isomers, by changing the solvent systerms, temperature and reactors. The "T" and "Y" shaped configurations of cpbda3" lead to rectangle and parallelogram shaped1D channel in structures。 The solvent void volumes of complex6>1>4>3are according with the solvent molecular size (H2O MeOH> DMF> DMP)。The higher molecular size and lower solvent polarity is tending to construct the structure with higher solvent void volume.
(2) Hacpbda react with Mn2+and Co2+, and result two groups of isomorphors, by changing the solvent systerms. In the3D structures group, the solvents voids volume of complex6>7>8。Besides, in the2D structures group, the porous size and the solvents voids volume of complex9<10<11. Both the two groups are according with the solvent molecular size (DMF DMA> DMP). Similar to supramolecular isomers, the isomorphors are also keeping the rule that the higher molecular size and lower solvent polarity is tending to construct the structure with higher porous size and solvent void volume.
(3) Along with the Cd+and H3cpbda, four rigid N-donor ligands are introduced, and five complexes with different dimensions are successfully constructed. The phen and2,2'-bipy are terminal ligands, which are adverse to increase the dimension of coordination polymers. However,4,4'-bipy and bpe are bridged ligands, tend to assembly high dimension MOFs. Besides, the new type of "M" molecular configuration is a factor to decrease the dimension. The fluorescence researches find that the red shifts are brought out by the introductions of rigid N-donor ligands. The red shift of terminal N-donor ligand is litter than bridged N-donor ligand.
(4) Using various synthesis methods, resulting same crystal products. According to the literature, the synthesis methods can bring out the variform crystal morphologies (crystal size and shape). However, the various synthesis ways of complexe in this dissertation are get the similar crystal morphologies and productive rate. It's must bescause of the flexible ligand H3cpbda can adapt the solvent environment and tend to form the similar crystal morphologies.
The research of this dissertation provide the theoretical basis for assembly of supramolecular isomers and isomorphors with different structures and functions.
本论文致力于这部分研究内容,选择了1,3-双(4’-羧基苯氧基)苯甲酸(H3cpbda)作为配体合成了17例配位聚合物。其中通过与不同的过渡金属离子组装了系列的超分子异构体以及异质同晶体,并且通过引入刚性含氮辅助配体组装了一系列不同维度的配位聚合物等。文中深入研究了不同系列结构之间的构效关系以及其影响因素,主要的研究结果有：
1.选取金属Mn2+离子与柔性的三齿配体H3cpbda作为构筑模块,通过系统的改变溶剂体系、温度以及反应器,实现了一系列超分子异构体的调控和合成。当配体采取不同的“T”型以及“Y”型的分子构型时,会拓展出“矩形”和“菱形”的一维孔道。对比三维的超分子异构体MOFs材料的孔隙率,发现配合物6>配合物1>配合物4>配合物3,符合溶剂分子尺寸(H2O
2.选取金属Mn2+和金属Co2+与H3cpbda作为构筑模块,通过溶剂体系的调控实现了两组二维及三维的异质同晶现象的调控。对比三维结构中的孔隙率,配合物6>配合物7>配合物8。在二维结构中,由于溶剂分子填充于孔道中支撑骨架,导致孔道的形状以及孔隙率均发生改变。对比孔道尺寸和孔隙率,配合物9<配合物10<配合物11。两组配合物均符合溶剂分子尺寸(DMF
3.选取金属Cd2+离子与H3cpbda作为构筑模块的同时,添加了一组刚性含氮辅助配体,螯合配体(Phen和2,2'-bipy)和桥连配体(4,4'-bipy和Bpe),实现了对配位聚合物维度的调控(1D,2D,3D)。在该组配合物中出现了新的“M”型构型,它属于降低维数的因素。另外,桥连辅助配体属于拓展维度和稳定结构的因素,封端辅助配体属于典型的降低维数的因素。通过这一系列不同维度配合物的调控验证了柔性配体的分子构型以及刚性辅助配体的种类对最终结构维度的重要影响。除此之外对荧光的研究发现,刚性辅助配体的选择促进了配合物的红移现象,其中引入封端配体的红移小,引入桥连配体的红移大。
4.基于柔性三齿配体H3cpbda,分别与金属离子Mn2+和Zn2+通过不同的反应方法以及溶剂体系分别合成了两组疏途同晶结构,先前关于疏途同晶现象的报道中虽然晶体的结构相同,但是宏观的晶体形貌(形状和尺寸)完全不同。本文中的两组实验方案均得到了相似的晶体形貌及产率。这是由于本文选取的柔性配体H3cpbda能够更好的适应外界溶剂及环境,在结晶过程中形成了形貌相似。说明晶体的宏观形貌的变化不仅与溶剂体系有关,它还与选择的配体种类有关。
本文的研究内容为如何调控配合物的超分子异构和异质同晶现象,定向的合成不同结构和性能的配位聚合物提供了理论依据,具有非常重要的意义。
Coordination polymers not only have variform charming structures, such as1D,2D,3D structures and novel interpenetrating or intertwine structures, but also possess various functions. Design and construction of the metal-organic frameworks (MOFs) have become an attractive prospect for their potential applications in gas absorption, separation, molecular sensing, and catalysis. As we known, the porous shape, dimensions and function groups are key factors for the applications of MOFs, and lots of factors can influence the final structure of MOFs, such as pH values, solvents temperature and so on. Therefore, the targeted design and assembly coordination polymers or MOFs is still a great challenge, which is urgent need to be intensive researched. Besides, the rational selection of metal cations and organic ligands with suitable shape, size, symmetry, functional groups and flexibility is considered to be a pivotal role to construct MOFs
In this dissertation, the1,3-bis(4'-carboxyl phenoxy)benzoic acid (H3cpbda) is choosen as main building block, and successfully construct17coordination polymers. H3cpbda react with different transition metal ions, result various supramolecular isomers and isomorphor. When a series of rigid N-donor ligand is introduced to the react systerm, five vari-dimension coordination polymers are synthesized. The properties and influence factor are intensively discussed. The major contents of this dissertation are listed as follows:
(1) H3cpbda reacts with Mn2+, and results a series of supramolecular isomers, by changing the solvent systerms, temperature and reactors. The "T" and "Y" shaped configurations of cpbda3" lead to rectangle and parallelogram shaped1D channel in structures。 The solvent void volumes of complex6>1>4>3are according with the solvent molecular size (H2O
(2) Hacpbda react with Mn2+and Co2+, and result two groups of isomorphors, by changing the solvent systerms. In the3D structures group, the solvents voids volume of complex6>7>8。Besides, in the2D structures group, the porous size and the solvents voids volume of complex9<10<11. Both the two groups are according with the solvent molecular size (DMF
(3) Along with the Cd+and H3cpbda, four rigid N-donor ligands are introduced, and five complexes with different dimensions are successfully constructed. The phen and2,2'-bipy are terminal ligands, which are adverse to increase the dimension of coordination polymers. However,4,4'-bipy and bpe are bridged ligands, tend to assembly high dimension MOFs. Besides, the new type of "M" molecular configuration is a factor to decrease the dimension. The fluorescence researches find that the red shifts are brought out by the introductions of rigid N-donor ligands. The red shift of terminal N-donor ligand is litter than bridged N-donor ligand.
(4) Using various synthesis methods, resulting same crystal products. According to the literature, the synthesis methods can bring out the variform crystal morphologies (crystal size and shape). However, the various synthesis ways of complexe in this dissertation are get the similar crystal morphologies and productive rate. It's must bescause of the flexible ligand H3cpbda can adapt the solvent environment and tend to form the similar crystal morphologies.
The research of this dissertation provide the theoretical basis for assembly of supramolecular isomers and isomorphors with different structures and functions.
引文
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