由柔性双功能配体构筑的配位聚合物
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摘要
本论文主要研究由柔性配体构筑的金属-有机配位聚合物的合成与结构表征,旨在合成新颖的具有互穿与螺旋结构特征的配位聚合物,并在合成研究的基础上,探讨特殊结构化合物的合成条件对产物结构的影响作用。
研究体系主要包括柔性二羧酸配体构筑的配位聚合物,柔性二吡啶配体构筑的配位聚合物,及柔性二吡啶与二羧酸混合配体构筑的配位聚合物。利用单晶X-射线衍射等多种表征手段对系列合成产物的结构与相关性能进行表征及测试。论文具体内容包括由柔性二羧酸配体与不同过渡金属合成的配位聚合物(第二章),由柔性二吡啶配体与不同的过渡金属备的配位聚合物(第三章),由柔性二吡啶与二羧酸混合配体和不同金属合成的配位聚合物(第四章)。论文还阐述了上述化合物的合成条件与方法,有机配体对结构的影响,热稳定性以及特殊结构形成的原因,为柔性配体配位聚合物的进一步研究奠定了基础。
Metal-organic coordination polymer has been a focus of material chemistry as a kind of newly-identified functional molecule-based material. According to the principle of the crystal engineering, it is possible to control the structure of the coordination polymer at a certain extent, at the same time, coordination polymer can be endowed with some properties, such as optics, electric, magnetism, enantio-separation and catalysis, by selecting functional metals or ligands with functional groups. As the properties of the coordination polymers is determined by their chemical constituents and framework topologies, seeking the coordination polymers with the novel topology has been considered as the exploiting the functional properties of the coordination polymers. Therefore, it has been a challengeable work to rationally design and synthesize the coordination polymers with predetermined structures. Latest years, many research groups at home and abroad get a lot of great fruits in design, synthesis and functional development according to the principle of the crystal engineering. However, the synthesis mechanism is still not known due to the terrible complexity of the synthesis-chemistry in coordination polymer, especially, in the coordination polymers constructed with the flexible ligands. So it is need to deeply research and accumulate abundant experimental facts, finally to achieve the aims of molecular design and directional synthesis. It is difficult to predict and control the framework constructed with flexible ligands, in result, it has been put little attention. In fact, it is possible to construct the novel structures with the flexible ligands because the distances and angles between functional groups and forms of linkers of flexible ligands can be adjusted to fit the coordination surroundings, not to mention the flexible ligands with the aromatic rings. The flexible ligands with aromatic rings have enough rigidity to prevent the bindingsites from coordinating to one single metal center that may results to some novel structures with large pores; and these ligands have flexible units which can entangle or entwine, as a result, it is prone to form interpenetrating or helical structures. So these properties of the flexible ligand can lead to some novle structural coordination polymers.
On the base of above paragraghs, we synthesized some interpenetrating and helical coordination polymers after rationally designing the flexible ligands and metals according to the principle of the crystal engineering. In the mean time, we studied the mainly factors on the synthesis of coordination polymers via changing the metal ions to adjust the inorganic components or ligands to adjust the framework components. In this paper, we synthesized some coordination polymers with novel structures using two different flexible ligands.
In chapter two, we synthesized a series of coordination polymers using the O-bondingsites flexible ligand----4,4’-oxybis(benzoicacid)(H2oba). Compound 1 exhibits a 2-D layer structure via the oba ligands linking the1-D chains Fe(R-CO2)3]∞; Compound 2 is a 3-D network via the oba ligands supporting the [Mn(OH)]nn+ inorganic layers with 4-, 8-rings windows formed with the Mn2+ and the hydroxy; Compound 3 is a 3-D supramolecular structure via the hydrongen-bond interaction linking the 2-D layers which are formed through the oba ligands bridging the [Zn(CO2)2(H2O)]n chains; Compound 4 displays a 3-D fivefold interpenetrating framework, and the individual network is formed by the same-vertexes helix which is constructed with the oba liands connecting the“paddle-wheel”structures Cu2(-CO2)4; Compound 5 is a 3-D chiral network with several helical chanals through two different coordinating-mode oba ligands linking the Zn2+ ions; Compound 6 reveals the formation of 3-D network via ligands linking the [Co4(CO2)8(EtOH)2] chains.
In chapter three, we synthesized a series of coordination polymers with novel structure using the flexible pyridyl ligand----1,3-bis(4-pyridyl)propane(bpp). Compounds 7 and 8 display 1-D“zigzag”chains through the ligands bridging the metal; Compounds 9 and 10 with 1-D helical structures exhibit 3-D supramolecular framework via theπ-πinteractions; Compound 11 shows 1-D chains; Compound 12 reveals the formation of 2-D layer structure; Compound 13 is a self-interpenetrating framework which is constructed with the bpp bridging the trimeric Second Building Units [Zn3O3N6]; Compound 14 displays 3-D fourfold interpenetrating diamondlike framework with helical chains in a, b, c axes in individual network. It shows that flexible bpp ligand is prone to construct the interpenetrating and helical frameworks, and it is possible to construct the structures with large pores in virtue of the large ligand.
On the base of above, we chose the bpp and H2oba as the mixed ligands to synthesize a series of coordination polymers with novel structures in chapter 4. Compound 15 reveals the formation of a 2-D layer with helical chains, and forms 3-D supramolecular structure via the van der Waals interactions; Compound 16 exhibits a double-layer structure via two-fold interpenetrating layers with helix; The helical chains in compound 15 and 16 are both constructed by two different ligands alternately bonding the metal ions. Compound 17 shows a threefold interpenetrating framework of a 2-D layers which is constituted with the single metal and two ligands, and exhibits two kinds of different helical chains in two directions in individual network---- one is constructed by two different ligands alternately bonding the metal atoms, the other is constructed by two different segments alternately bonding the metal atoms which contain two same ligands. Compound 18 is a threefold interpenetrating framework of a 2-D layers with two kinds of helical chains which is constituted with two different metals and two ligands, and the two helical chains are both constructed by two different segments alternately bonding the metal atoms which contain two same ligands. Moreover, we characterized the properties. The results show that compound 15, 16 are antiferromagnetic and compound 17, 18 exhibit good fluorescence. Furthermore, it is rare that two ligands, especially two different segments which contain two same ligands, link metals alternately to form the helix.
研究体系主要包括柔性二羧酸配体构筑的配位聚合物,柔性二吡啶配体构筑的配位聚合物,及柔性二吡啶与二羧酸混合配体构筑的配位聚合物。利用单晶X-射线衍射等多种表征手段对系列合成产物的结构与相关性能进行表征及测试。论文具体内容包括由柔性二羧酸配体与不同过渡金属合成的配位聚合物(第二章),由柔性二吡啶配体与不同的过渡金属备的配位聚合物(第三章),由柔性二吡啶与二羧酸混合配体和不同金属合成的配位聚合物(第四章)。论文还阐述了上述化合物的合成条件与方法,有机配体对结构的影响,热稳定性以及特殊结构形成的原因,为柔性配体配位聚合物的进一步研究奠定了基础。
Metal-organic coordination polymer has been a focus of material chemistry as a kind of newly-identified functional molecule-based material. According to the principle of the crystal engineering, it is possible to control the structure of the coordination polymer at a certain extent, at the same time, coordination polymer can be endowed with some properties, such as optics, electric, magnetism, enantio-separation and catalysis, by selecting functional metals or ligands with functional groups. As the properties of the coordination polymers is determined by their chemical constituents and framework topologies, seeking the coordination polymers with the novel topology has been considered as the exploiting the functional properties of the coordination polymers. Therefore, it has been a challengeable work to rationally design and synthesize the coordination polymers with predetermined structures. Latest years, many research groups at home and abroad get a lot of great fruits in design, synthesis and functional development according to the principle of the crystal engineering. However, the synthesis mechanism is still not known due to the terrible complexity of the synthesis-chemistry in coordination polymer, especially, in the coordination polymers constructed with the flexible ligands. So it is need to deeply research and accumulate abundant experimental facts, finally to achieve the aims of molecular design and directional synthesis. It is difficult to predict and control the framework constructed with flexible ligands, in result, it has been put little attention. In fact, it is possible to construct the novel structures with the flexible ligands because the distances and angles between functional groups and forms of linkers of flexible ligands can be adjusted to fit the coordination surroundings, not to mention the flexible ligands with the aromatic rings. The flexible ligands with aromatic rings have enough rigidity to prevent the bindingsites from coordinating to one single metal center that may results to some novel structures with large pores; and these ligands have flexible units which can entangle or entwine, as a result, it is prone to form interpenetrating or helical structures. So these properties of the flexible ligand can lead to some novle structural coordination polymers.
On the base of above paragraghs, we synthesized some interpenetrating and helical coordination polymers after rationally designing the flexible ligands and metals according to the principle of the crystal engineering. In the mean time, we studied the mainly factors on the synthesis of coordination polymers via changing the metal ions to adjust the inorganic components or ligands to adjust the framework components. In this paper, we synthesized some coordination polymers with novel structures using two different flexible ligands.
In chapter two, we synthesized a series of coordination polymers using the O-bondingsites flexible ligand----4,4’-oxybis(benzoicacid)(H2oba). Compound 1 exhibits a 2-D layer structure via the oba ligands linking the1-D chains Fe(R-CO2)3]∞; Compound 2 is a 3-D network via the oba ligands supporting the [Mn(OH)]nn+ inorganic layers with 4-, 8-rings windows formed with the Mn2+ and the hydroxy; Compound 3 is a 3-D supramolecular structure via the hydrongen-bond interaction linking the 2-D layers which are formed through the oba ligands bridging the [Zn(CO2)2(H2O)]n chains; Compound 4 displays a 3-D fivefold interpenetrating framework, and the individual network is formed by the same-vertexes helix which is constructed with the oba liands connecting the“paddle-wheel”structures Cu2(-CO2)4; Compound 5 is a 3-D chiral network with several helical chanals through two different coordinating-mode oba ligands linking the Zn2+ ions; Compound 6 reveals the formation of 3-D network via ligands linking the [Co4(CO2)8(EtOH)2] chains.
In chapter three, we synthesized a series of coordination polymers with novel structure using the flexible pyridyl ligand----1,3-bis(4-pyridyl)propane(bpp). Compounds 7 and 8 display 1-D“zigzag”chains through the ligands bridging the metal; Compounds 9 and 10 with 1-D helical structures exhibit 3-D supramolecular framework via theπ-πinteractions; Compound 11 shows 1-D chains; Compound 12 reveals the formation of 2-D layer structure; Compound 13 is a self-interpenetrating framework which is constructed with the bpp bridging the trimeric Second Building Units [Zn3O3N6]; Compound 14 displays 3-D fourfold interpenetrating diamondlike framework with helical chains in a, b, c axes in individual network. It shows that flexible bpp ligand is prone to construct the interpenetrating and helical frameworks, and it is possible to construct the structures with large pores in virtue of the large ligand.
On the base of above, we chose the bpp and H2oba as the mixed ligands to synthesize a series of coordination polymers with novel structures in chapter 4. Compound 15 reveals the formation of a 2-D layer with helical chains, and forms 3-D supramolecular structure via the van der Waals interactions; Compound 16 exhibits a double-layer structure via two-fold interpenetrating layers with helix; The helical chains in compound 15 and 16 are both constructed by two different ligands alternately bonding the metal ions. Compound 17 shows a threefold interpenetrating framework of a 2-D layers which is constituted with the single metal and two ligands, and exhibits two kinds of different helical chains in two directions in individual network---- one is constructed by two different ligands alternately bonding the metal atoms, the other is constructed by two different segments alternately bonding the metal atoms which contain two same ligands. Compound 18 is a threefold interpenetrating framework of a 2-D layers with two kinds of helical chains which is constituted with two different metals and two ligands, and the two helical chains are both constructed by two different segments alternately bonding the metal atoms which contain two same ligands. Moreover, we characterized the properties. The results show that compound 15, 16 are antiferromagnetic and compound 17, 18 exhibit good fluorescence. Furthermore, it is rare that two ligands, especially two different segments which contain two same ligands, link metals alternately to form the helix.
引文
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