基于取代三唑配体的过渡金属配合物的合成、结构及性质研究
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摘要
配位聚合物作为一种新型多功能复合晶态材料,受到各国化学家日益广泛的关注,配位聚合物的研究也取得令人瞩目的成绩,大量的研究成果表明,配位聚合物的体系结构取决于构筑模块(有机配体、金属中心、抗衡离子和溶剂分子)和配位共存性。如何合理地选取和设计适当的分子基构筑模块是合成配合物的重要因素之一。我们主要研究含给体取代基的不对称3,5-二取代-1,2,4-三唑类配体构筑的新型配合物的合成、结构及性能。此类配体在增加配位点的同时,进一步增加了骨架三唑配体的长度,可以作为极好的桥连配体,有望获得新颖结构和优良性能的金属有机材料。
本论文设计合成3-氨基-5-乙酸基-1,2,4-三唑(H2trza)配体,并选取3-(2’-吡嗪)-5-(4’-吡啶)-1,2,4-三唑(Hppt)配体,利用这两个配体设计合成了22个未见文献报道的过渡金属配合物,并分别对它们进行元素分析、红外光谱、X-射线单晶衍射、粉末X-射线衍射、热重、荧光光谱、磁学性质等方面的表征和研究。另外从阴离子调控、溶剂的调控以及辅助配体的调控等方面考查它们对所构筑的配合物结构的影响。本论文的工作主要分为以下四个部分：
1.设计并合成了H2trza配体,利用此配体合成了6个过渡金属配合物,结构分析结果显示配合物1-6都是离散的零维分子,通过丰富的氢键作用形成3D超分子网络结构。并研究了辅助配体和金属离子对结构的有序态和无序态的影响,同时也测试了配合物1-6的热稳定性。
2.用Hppt配体合成了6个配合物,利用不同阴离子的镉盐得到化合物7-9,其中7和9是通过卤素离子桥连形成三核镉簇,以此为结构单元通过有机配体连接形成二维结构,不同的卤素离子对最终的结构有导向作用；化合物10、11、12分别呈现零维、三维和一维结构,分析了配体的扭转程度不同对连接方式的影响。并测试了7-10的热稳定性和荧光性能。
3.在Cd/Hppt体系中引入不同的苯羧酸共配体合成了配位聚合物13-16,结构分析表明化合物13是二重穿插的二维波浪形结构；化合物15是二重穿插的三维网络结构；化合物14和16都是复杂的三维结构；并研究了它们的热稳定性和荧光性能。
4.使用Hppt配体和不同的苯羧酸共配体,采用混配策略,合成了配合物17-22,化合物17和19是通过双核单元构筑的新型超分子网络,20和21是两个同构的二维层结构；利用配合物配体的策略得到一个新颖的多聚连锁的配位聚合物22,22是2D→3D的平行穿插网络。此外,对化合物19进行了磁学初步研究,测试了直流变温磁化率,结果表明金属锰离子之间存在反铁磁相互作用,分子间氢键提供可能的磁耦合通道；对化合物20进行了比较详细的磁学分析,测试了直流变温磁化率、变场磁化强度和场冷-零场冷(FC-ZFC),在20中也存在反铁磁相互作用。并研究了化合物17和19的热稳定性及17和21的荧光光谱。
Coordination polymer as a new type of multi-functional composite crystal materials attracts chemist's attention. Coordination polymer research has made outstanding achievements. A large number of research results show that the influence of coordination polymer architecture depends on constructing module (organic ligands, metal center, counter ion, and solvent molecules) and coordination co-existence. How to reasonably choose and design the appropriate molecular base building module is one of the important factors in the synthesis of complexes. We mainly intends to synthesis and choose contain donors asymmetric3,5-disubstituted1,2,4-triazoles ligands and construct coordination polymers by self-assembly. This kind of ligand increasing with coordination sites, further enhancing the skeleton trizole ligand length at the same time, can be used as a very good bridging ligand, which is expected to obtain novel metal organic framework materials with good performance,
In this paper,3-amino-lH-1,2,4-triazole-5-acetate ligand is designed and synthesized and3-(2'-pyrazine)-5-(4'-pyridine)-1,2,4-triazole (Hppt) ligand is choosed. These ligands have been used to react with metal ion to afford twenty-two new complexes. Structures of them have een determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra, and thermogravimetric analysis. Furthermore, photoluminescence and magnetic properties of some complexes were also investigated. We have studied the influence of many factors, such as anionic-controlled and solvent-controlled and auxiliary-controlled the formation of various structural types. The main contributions in this work are blow:
1. We have designed and synthesized Hatrza ligand. Six complexes have been synthesized by the ligand and different metal salts. Complexes1-6are discrete OD structures. These are abundant intermolecular H-bonds in their packing structure. The units were connected as three dimension structure by the intermolecular H-bonds. Also, the thermal stabilities were discussed.
2. Six complexes haved been synthesized by using Hppt ligand and metal salts. The complexes7-9containing Cd(II) ions are2D layer structure. The halogen ions have no the effects of structure. There are large differences on thermostability of them. The complexes10、11and12are0D、3D and ID, respectively. The results show that distorting of ligand influences on coordination mode. And the thermal stabilities and luminescent properties of compounds7-10were carried out.
3. Compounds13-16have been successfully synthesized by the self-assembly of Cd(Ⅱ), Hppt ligand, and carboxylate ligands. Compound13shows a2-fold interpenetrating2D wave-like structure. Compounds14and16are complexity3D net. Compound15reveals a2-fold interpenetrating3D framework. And the thermal stabilities and luminescent properties were carried out and analyzed.
4. Six new complexes17-22have been obtained from the self-assembly of the Hppt ligand with different metal salts, in the presence of coligands. Compounds17and19are new supramolecular architectures. Compound22reveals a novel interesting2D→3D parallel polycatenation network. Compounds20and21are two isomorphic2D net. Different auxiliary ligand has obvious influence on dimension of compounds. Moreover, the magnetic properties of compounds19and20were studied, and they display weak antiferromagnetic character. At the same time, the thermal stabilities of17and19, the luminescent properties of17and21were tested and discussed, respectively.
本论文设计合成3-氨基-5-乙酸基-1,2,4-三唑(H2trza)配体,并选取3-(2’-吡嗪)-5-(4’-吡啶)-1,2,4-三唑(Hppt)配体,利用这两个配体设计合成了22个未见文献报道的过渡金属配合物,并分别对它们进行元素分析、红外光谱、X-射线单晶衍射、粉末X-射线衍射、热重、荧光光谱、磁学性质等方面的表征和研究。另外从阴离子调控、溶剂的调控以及辅助配体的调控等方面考查它们对所构筑的配合物结构的影响。本论文的工作主要分为以下四个部分：
1.设计并合成了H2trza配体,利用此配体合成了6个过渡金属配合物,结构分析结果显示配合物1-6都是离散的零维分子,通过丰富的氢键作用形成3D超分子网络结构。并研究了辅助配体和金属离子对结构的有序态和无序态的影响,同时也测试了配合物1-6的热稳定性。
2.用Hppt配体合成了6个配合物,利用不同阴离子的镉盐得到化合物7-9,其中7和9是通过卤素离子桥连形成三核镉簇,以此为结构单元通过有机配体连接形成二维结构,不同的卤素离子对最终的结构有导向作用；化合物10、11、12分别呈现零维、三维和一维结构,分析了配体的扭转程度不同对连接方式的影响。并测试了7-10的热稳定性和荧光性能。
3.在Cd/Hppt体系中引入不同的苯羧酸共配体合成了配位聚合物13-16,结构分析表明化合物13是二重穿插的二维波浪形结构；化合物15是二重穿插的三维网络结构；化合物14和16都是复杂的三维结构；并研究了它们的热稳定性和荧光性能。
4.使用Hppt配体和不同的苯羧酸共配体,采用混配策略,合成了配合物17-22,化合物17和19是通过双核单元构筑的新型超分子网络,20和21是两个同构的二维层结构；利用配合物配体的策略得到一个新颖的多聚连锁的配位聚合物22,22是2D→3D的平行穿插网络。此外,对化合物19进行了磁学初步研究,测试了直流变温磁化率,结果表明金属锰离子之间存在反铁磁相互作用,分子间氢键提供可能的磁耦合通道；对化合物20进行了比较详细的磁学分析,测试了直流变温磁化率、变场磁化强度和场冷-零场冷(FC-ZFC),在20中也存在反铁磁相互作用。并研究了化合物17和19的热稳定性及17和21的荧光光谱。
Coordination polymer as a new type of multi-functional composite crystal materials attracts chemist's attention. Coordination polymer research has made outstanding achievements. A large number of research results show that the influence of coordination polymer architecture depends on constructing module (organic ligands, metal center, counter ion, and solvent molecules) and coordination co-existence. How to reasonably choose and design the appropriate molecular base building module is one of the important factors in the synthesis of complexes. We mainly intends to synthesis and choose contain donors asymmetric3,5-disubstituted1,2,4-triazoles ligands and construct coordination polymers by self-assembly. This kind of ligand increasing with coordination sites, further enhancing the skeleton trizole ligand length at the same time, can be used as a very good bridging ligand, which is expected to obtain novel metal organic framework materials with good performance,
In this paper,3-amino-lH-1,2,4-triazole-5-acetate ligand is designed and synthesized and3-(2'-pyrazine)-5-(4'-pyridine)-1,2,4-triazole (Hppt) ligand is choosed. These ligands have been used to react with metal ion to afford twenty-two new complexes. Structures of them have een determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra, and thermogravimetric analysis. Furthermore, photoluminescence and magnetic properties of some complexes were also investigated. We have studied the influence of many factors, such as anionic-controlled and solvent-controlled and auxiliary-controlled the formation of various structural types. The main contributions in this work are blow:
1. We have designed and synthesized Hatrza ligand. Six complexes have been synthesized by the ligand and different metal salts. Complexes1-6are discrete OD structures. These are abundant intermolecular H-bonds in their packing structure. The units were connected as three dimension structure by the intermolecular H-bonds. Also, the thermal stabilities were discussed.
2. Six complexes haved been synthesized by using Hppt ligand and metal salts. The complexes7-9containing Cd(II) ions are2D layer structure. The halogen ions have no the effects of structure. There are large differences on thermostability of them. The complexes10、11and12are0D、3D and ID, respectively. The results show that distorting of ligand influences on coordination mode. And the thermal stabilities and luminescent properties of compounds7-10were carried out.
3. Compounds13-16have been successfully synthesized by the self-assembly of Cd(Ⅱ), Hppt ligand, and carboxylate ligands. Compound13shows a2-fold interpenetrating2D wave-like structure. Compounds14and16are complexity3D net. Compound15reveals a2-fold interpenetrating3D framework. And the thermal stabilities and luminescent properties were carried out and analyzed.
4. Six new complexes17-22have been obtained from the self-assembly of the Hppt ligand with different metal salts, in the presence of coligands. Compounds17and19are new supramolecular architectures. Compound22reveals a novel interesting2D→3D parallel polycatenation network. Compounds20and21are two isomorphic2D net. Different auxiliary ligand has obvious influence on dimension of compounds. Moreover, the magnetic properties of compounds19and20were studied, and they display weak antiferromagnetic character. At the same time, the thermal stabilities of17and19, the luminescent properties of17and21were tested and discussed, respectively.
引文
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