含二咪唑配体的配位聚合物的合成、结构和性质研究
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摘要
在第一章中,比较全面的介绍了功能配位聚合物的基本概念、发展过程、应用价值、及影响配合物结构的因素等。最后,指明了本课题的选题意义,概括了本研究工作所取得的成果。
在第二章中,利用4,4'-六氟异丙基邻苯二甲酸(H4hfpdpt)与1,4-二(1-咪唑基)丁烷配体(biim-4)在溶剂热的条件下合成了4个金属配合物:[Cd(Hhfpdpt)(Hbiim-4)(biim-4)_(0.5)(H_2O)]·2H_2O (1), [Cd_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (2), [Mn_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (3)和[Zn_2(hfpdpt)(biim-4)_(1.5)]·(CH_3CH_2OH) (4)。化合物1具有(4,5)连接拓扑的超分子结构,而化合物2具有(5,6)连接拓扑的三维结构。化合物3与化合物2具有相同的(5,6)连接的拓扑,然而它们唯一的不同在于hfpdpt上羧基的配位模式。化合物4展示了一个罕见的3D→3D的自穿结构。对化合物1,2和4的热稳定性、光学性质进行了讨论。
在第三章中,利用1,5-二(1-咪唑基)戊烷配体(biim-5)作为中性配体通过溶剂热的方法合成了5个配合物: [Co(o-BDC)(biim-5)] (5), [Co(m-BDC)(biim-5)]·H_2O (6), [Co(5-OH-m-BDC)(biim-5)] (7), [Co(DL-Cam)(biim-5)]·4H_2O (8)和[Co(BTCA)_(0.5)(biim-5)] (9)。化合物5展现出了二维的63-hcb拓扑。化合物6展现出了不常见的4-连接的二维双层结构。化合物7展示了一个二维的sql网络结构,这个二维的层进一步被羧基上的O原子和羟基之间存在的分子间氢键连接形成一个三维超分子结构。化合物8是一个含有四核水簇的二维层状结构。化合物9是一个相对比较复杂的(3,4)连接的三维化合物,其拓扑符号为(83)2(85·10)。对这些化合物的热稳定性进行了研究。
在第四章中,利用2,2’–二(1–咪唑基)乙醚配体(BIE)作为中性配体与多元羧酸通过溶剂热的方法合成了13个配合物:[Ni(p-BDC)(BIE)] (10), [Cu(p-BDC)(BIE)] (11), [Cu(o-BDC)(BIE)] (12), [Cu_5(m-BDC)_4(μ3-O)_2(BIE)_2(H_2O)_2] (13), [Co(OX)(BIE)] (14), [Cu_3(1,3,5-BTC)_2(BIE)_2(H_2O)_3] (15), [Cu(1,2,4,5-btec)_(0.5)(BIE)] (16), [Co_2(1,2,4,5-btec)(BIE)_2]·H_2O (17), [Co_2(OA)(BIE)_2]·1.5H_2O (18), [Zn_2(OA)(BIE)_2]·2.5H_2O (19), [Cd(OA)_(0.5)(BIE)(H_2O)]·H_2O (20), [Zn_2(hfpdpt)(BIE)_2]·H_2O (21)和[Cd(1,2,3,4-btec)_(0.5)(BIE)(H_2O)] (22)。化合物10-12为44-sql层。化合物13中含有五核Cu簇,其结构可以简化为α-Po拓扑。化合物14为63-hcb层。而化合物15为罕见的二维自穿结构。化合物16则为不常见的Kagomé拓扑。化合物17为少见的含有平面四边形4-连接点的(3,4)连接的拓扑,其拓扑符号为(83)2(85·10)。化合物18和19几乎是同构的,它们具有相同的(32·62·72)(32·4·62·7)2拓扑。而化合物20则含有两种手性层,其拓扑符号为(52·64)(53·62·7)2。化合物21含有一个假对称中心,其结构为三维孔道结构。化合物22则展示了一个一维链状结构。对这些化合物的结构进行了描述,并对他们的热稳定性和光学性质进行了研究。
第五章是结论。
In the first chapter, the concepts, the histories, the potential applications of coordination polymers, and the factors affecting the structures of the compounds are concisely introduced. At the end of this chapter, we pointed out that the importance of the search project and summarized the important results obtained in the thesis.
In the second chapter, four new coordination polymers based on hfpdpt anion and biim-4 ligand, namely [Cd(Hhfpdpt)(Hbiim-4)(biim-4)_(0.5)(H_2O)]·2H_2O (1), [Cd_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (2), [Mn_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (3), and [Zn_2(hfpdpt)(biim-4)_(1.5)]·(CH_3CH_2OH) (4), where H4hfpdpt = 4,4’-(hexafluoroisopropylidene)diphthalic acid, biim-4 = 1,4-bis(imidazolyl)butane, were synthesized under hydrothermal conditions. Compound 1 displays a 3D supramolecular structure, with a (4,5)-connected topology, while compound 2 has a 3D (5,6)-connected topology. 3 has the same (5,6)-connected topology as that of 2, however, the only difference of these two compounds is the coordination modes of the hfpdpt anion. Compound 4 exhibits a rare 3D→3D self-penetrating framework. The thermogravimetric and luminescent properties were also investigated for compounds 1, 2 and 4.
In the third chapter, five new coordination polymers based on biim-5 ligand, namely [Co(o-BDC)(biim-5)] (5), [Co(m-BDC)(biim-5)]·H_2O (6), [Co(5-OH-m-BDC)(biim-5)] (7), [Co(DL-Cam)(biim-5)]·4H_2O (8), and [Co(BTCA)_(0.5)(biim-5)] (9), where biim-5 = 1,5-bis(imidazolyl)pentane, H_2o-BDC = 1,2-benzenedicarboxylic acid, H_2m-BDC = 1,3-benzenedicarboxylic acid, H_25-OH-m-BDC = 5-OH-1,3-benzenedicarboxylic acid, H_2DL-Cam = DL-camphoric acid, and H4BTCA = 1,2,3,4-butanetetracarboxylic acid, were synthesized under hydrothermal conditions. Compound 5 displays a 2D 63-hcb-net. Compound 6 exhibits an uncommon 4-connected 2D layer. Compound 7 has a 2D sql net, this net is further extended by hydrogen bonds between the carboxylate O atoms and the hydroxyl groups into a 3D supramolecular framework. 8 is a 2D layer containing water tetramer. Compound 9 is relatively complex 3D framework with a rare (3,4)-connected topology. The thermal stabilities these five compounds were studied by thermogravimetric analysis.
In the fourth chapter, reactions of 2,2’-bis(1-imidazolyl)ether (BIE) with different polycarboxylic acids produce thirteen new coordination polymers, namely [Ni(p-BDC)(BIE)] (10), [Cu(p-BDC)(BIE)] (11), [Cu(o-BDC)(BIE)] (12), [Cu_5(m-BDC)4(μ3-O)_2(BIE)_2(H_2O)_2] (13), [Co(OX)(BIE)] (14), [Cu3(1,3,5-BTC)_2(BIE)_2(H_2O)3] (15), [Cu(1,2,4,5-btec)_(0.5)(BIE)] (16), [Co_2(1,2,4,5-btec)(BIE)_2]·H_2O (17), [Co_2(OA)(BIE)_2]·1.5H_2O (18), [Zn_2(OA)(BIE)_2]·2.5H_2O (19), [Cd(OA)_(0.5)(BIE)(H_2O)]·H_2O (20), [Zn_2(hfpdpt)(BIE)_2]·H_2O (21), and [Cd(1,2,3,4-btec)_(0.5)(BIE)(H_2O)] (22), where H_(2p)-bdc = 1,4-benzenedicarboxylic acid, H_2o-bdc = 1,2-benzenedicarboxylic acid, H_2m-bdc = 1,3-benzenedicarboxylic acid, H_2OX = oxalic acid, H31,3,5-BTC = 1,3,5-benzenetricarboxylic acid, H41,2,4,5-btec = 1,2,4,5-benzenetetracarboxylic acid, H4OA = 4,4’-oxidiphthalic acid, H4hfpdpt = 4,4’-(hexafluoroisopropylidene)diphthalic acid, and H41,2,3,4-btec = 1,2,3,4-benzenetetracarboxylic acid, were synthesized under hydrothermal conditions. Compounds 10-12 are 44-sql layers. 13 exhibits anα-Po topology based on pentanuclear Cu(II) cluster. Compound 14 displays a 63-hcb layer, while 15 is a rare self-penetrating 2D network. Compound 16 is a unique Kagométopology. Compound 17 shows a rare 3,4-connected (83)2(85·10) topology with 3-connected nodes and square-planar 4-connected node. The crystal structures of 18 and 19 are close to being isostructural with a scarce (32·62·72)(32·4·62·7)2 topology. 20 contains two kinds of chiral layers, one left-handed and the other right-handed, with a unique topological type of (52·64)(53·62·7)2. Compound 21, related by a pseudo-centre of inversion, possesses a 3D porous framework. 22 shows a 1D chain structure. The structures of 10-22 are described. The thermal stabilities and the luminescent properties of 19-22 are also discussed in detail.
The fifth chapter is the conclusions.
在第二章中,利用4,4'-六氟异丙基邻苯二甲酸(H4hfpdpt)与1,4-二(1-咪唑基)丁烷配体(biim-4)在溶剂热的条件下合成了4个金属配合物:[Cd(Hhfpdpt)(Hbiim-4)(biim-4)_(0.5)(H_2O)]·2H_2O (1), [Cd_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (2), [Mn_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (3)和[Zn_2(hfpdpt)(biim-4)_(1.5)]·(CH_3CH_2OH) (4)。化合物1具有(4,5)连接拓扑的超分子结构,而化合物2具有(5,6)连接拓扑的三维结构。化合物3与化合物2具有相同的(5,6)连接的拓扑,然而它们唯一的不同在于hfpdpt上羧基的配位模式。化合物4展示了一个罕见的3D→3D的自穿结构。对化合物1,2和4的热稳定性、光学性质进行了讨论。
在第三章中,利用1,5-二(1-咪唑基)戊烷配体(biim-5)作为中性配体通过溶剂热的方法合成了5个配合物: [Co(o-BDC)(biim-5)] (5), [Co(m-BDC)(biim-5)]·H_2O (6), [Co(5-OH-m-BDC)(biim-5)] (7), [Co(DL-Cam)(biim-5)]·4H_2O (8)和[Co(BTCA)_(0.5)(biim-5)] (9)。化合物5展现出了二维的63-hcb拓扑。化合物6展现出了不常见的4-连接的二维双层结构。化合物7展示了一个二维的sql网络结构,这个二维的层进一步被羧基上的O原子和羟基之间存在的分子间氢键连接形成一个三维超分子结构。化合物8是一个含有四核水簇的二维层状结构。化合物9是一个相对比较复杂的(3,4)连接的三维化合物,其拓扑符号为(83)2(85·10)。对这些化合物的热稳定性进行了研究。
在第四章中,利用2,2’–二(1–咪唑基)乙醚配体(BIE)作为中性配体与多元羧酸通过溶剂热的方法合成了13个配合物:[Ni(p-BDC)(BIE)] (10), [Cu(p-BDC)(BIE)] (11), [Cu(o-BDC)(BIE)] (12), [Cu_5(m-BDC)_4(μ3-O)_2(BIE)_2(H_2O)_2] (13), [Co(OX)(BIE)] (14), [Cu_3(1,3,5-BTC)_2(BIE)_2(H_2O)_3] (15), [Cu(1,2,4,5-btec)_(0.5)(BIE)] (16), [Co_2(1,2,4,5-btec)(BIE)_2]·H_2O (17), [Co_2(OA)(BIE)_2]·1.5H_2O (18), [Zn_2(OA)(BIE)_2]·2.5H_2O (19), [Cd(OA)_(0.5)(BIE)(H_2O)]·H_2O (20), [Zn_2(hfpdpt)(BIE)_2]·H_2O (21)和[Cd(1,2,3,4-btec)_(0.5)(BIE)(H_2O)] (22)。化合物10-12为44-sql层。化合物13中含有五核Cu簇,其结构可以简化为α-Po拓扑。化合物14为63-hcb层。而化合物15为罕见的二维自穿结构。化合物16则为不常见的Kagomé拓扑。化合物17为少见的含有平面四边形4-连接点的(3,4)连接的拓扑,其拓扑符号为(83)2(85·10)。化合物18和19几乎是同构的,它们具有相同的(32·62·72)(32·4·62·7)2拓扑。而化合物20则含有两种手性层,其拓扑符号为(52·64)(53·62·7)2。化合物21含有一个假对称中心,其结构为三维孔道结构。化合物22则展示了一个一维链状结构。对这些化合物的结构进行了描述,并对他们的热稳定性和光学性质进行了研究。
第五章是结论。
In the first chapter, the concepts, the histories, the potential applications of coordination polymers, and the factors affecting the structures of the compounds are concisely introduced. At the end of this chapter, we pointed out that the importance of the search project and summarized the important results obtained in the thesis.
In the second chapter, four new coordination polymers based on hfpdpt anion and biim-4 ligand, namely [Cd(Hhfpdpt)(Hbiim-4)(biim-4)_(0.5)(H_2O)]·2H_2O (1), [Cd_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (2), [Mn_2(hfpdpt)(biim-4)_(0.5)(H_2O)_2]·0.5H_2O (3), and [Zn_2(hfpdpt)(biim-4)_(1.5)]·(CH_3CH_2OH) (4), where H4hfpdpt = 4,4’-(hexafluoroisopropylidene)diphthalic acid, biim-4 = 1,4-bis(imidazolyl)butane, were synthesized under hydrothermal conditions. Compound 1 displays a 3D supramolecular structure, with a (4,5)-connected topology, while compound 2 has a 3D (5,6)-connected topology. 3 has the same (5,6)-connected topology as that of 2, however, the only difference of these two compounds is the coordination modes of the hfpdpt anion. Compound 4 exhibits a rare 3D→3D self-penetrating framework. The thermogravimetric and luminescent properties were also investigated for compounds 1, 2 and 4.
In the third chapter, five new coordination polymers based on biim-5 ligand, namely [Co(o-BDC)(biim-5)] (5), [Co(m-BDC)(biim-5)]·H_2O (6), [Co(5-OH-m-BDC)(biim-5)] (7), [Co(DL-Cam)(biim-5)]·4H_2O (8), and [Co(BTCA)_(0.5)(biim-5)] (9), where biim-5 = 1,5-bis(imidazolyl)pentane, H_2o-BDC = 1,2-benzenedicarboxylic acid, H_2m-BDC = 1,3-benzenedicarboxylic acid, H_25-OH-m-BDC = 5-OH-1,3-benzenedicarboxylic acid, H_2DL-Cam = DL-camphoric acid, and H4BTCA = 1,2,3,4-butanetetracarboxylic acid, were synthesized under hydrothermal conditions. Compound 5 displays a 2D 63-hcb-net. Compound 6 exhibits an uncommon 4-connected 2D layer. Compound 7 has a 2D sql net, this net is further extended by hydrogen bonds between the carboxylate O atoms and the hydroxyl groups into a 3D supramolecular framework. 8 is a 2D layer containing water tetramer. Compound 9 is relatively complex 3D framework with a rare (3,4)-connected topology. The thermal stabilities these five compounds were studied by thermogravimetric analysis.
In the fourth chapter, reactions of 2,2’-bis(1-imidazolyl)ether (BIE) with different polycarboxylic acids produce thirteen new coordination polymers, namely [Ni(p-BDC)(BIE)] (10), [Cu(p-BDC)(BIE)] (11), [Cu(o-BDC)(BIE)] (12), [Cu_5(m-BDC)4(μ3-O)_2(BIE)_2(H_2O)_2] (13), [Co(OX)(BIE)] (14), [Cu3(1,3,5-BTC)_2(BIE)_2(H_2O)3] (15), [Cu(1,2,4,5-btec)_(0.5)(BIE)] (16), [Co_2(1,2,4,5-btec)(BIE)_2]·H_2O (17), [Co_2(OA)(BIE)_2]·1.5H_2O (18), [Zn_2(OA)(BIE)_2]·2.5H_2O (19), [Cd(OA)_(0.5)(BIE)(H_2O)]·H_2O (20), [Zn_2(hfpdpt)(BIE)_2]·H_2O (21), and [Cd(1,2,3,4-btec)_(0.5)(BIE)(H_2O)] (22), where H_(2p)-bdc = 1,4-benzenedicarboxylic acid, H_2o-bdc = 1,2-benzenedicarboxylic acid, H_2m-bdc = 1,3-benzenedicarboxylic acid, H_2OX = oxalic acid, H31,3,5-BTC = 1,3,5-benzenetricarboxylic acid, H41,2,4,5-btec = 1,2,4,5-benzenetetracarboxylic acid, H4OA = 4,4’-oxidiphthalic acid, H4hfpdpt = 4,4’-(hexafluoroisopropylidene)diphthalic acid, and H41,2,3,4-btec = 1,2,3,4-benzenetetracarboxylic acid, were synthesized under hydrothermal conditions. Compounds 10-12 are 44-sql layers. 13 exhibits anα-Po topology based on pentanuclear Cu(II) cluster. Compound 14 displays a 63-hcb layer, while 15 is a rare self-penetrating 2D network. Compound 16 is a unique Kagométopology. Compound 17 shows a rare 3,4-connected (83)2(85·10) topology with 3-connected nodes and square-planar 4-connected node. The crystal structures of 18 and 19 are close to being isostructural with a scarce (32·62·72)(32·4·62·7)2 topology. 20 contains two kinds of chiral layers, one left-handed and the other right-handed, with a unique topological type of (52·64)(53·62·7)2. Compound 21, related by a pseudo-centre of inversion, possesses a 3D porous framework. 22 shows a 1D chain structure. The structures of 10-22 are described. The thermal stabilities and the luminescent properties of 19-22 are also discussed in detail.
The fifth chapter is the conclusions.
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