基于柔性配体对苯二乙酸的过渡金属配合物的合成、晶体结构及性能研究
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摘要
近几年来,由柔性配体制得的金属配合物由于其结构的多样性和潜在的功能性而受到人们越来越多的关注,其中对苯二乙酸(H_2PDA)就是一个比较典型的柔性二羧酸类配体,它的两个柔性的乙酸基能够形成顺式和反式构型,再加上羧基配位方式的多样性,因此形成的结构更加灵活和多样。为了研究对苯二乙酸的配位特点及它所形成的过渡金属配合物的结构特征和性能,本文以对苯二乙酸为主配体用溶剂法合成了10个未见报道的对苯二乙酸的过渡金属配合物,并通过X-射线单晶衍射、红外光谱、元素分析等手段系统地研究了它们的结构,并对其中一些配合物做了热重分析和一些其他方面的研究。
本论文分为以下五章:
绪论部分首先着重介绍了配位聚合物的研究现状,及它们在气体吸附、催化反应和光学、磁学方面的潜在应用。然后详细介绍了对苯二乙酸在国内外的研究概况。
第二章描述了以对苯二乙酸为主配体,2,2’-联吡啶为第二配体分别与铜盐、锌盐、镉盐反应得到的五个配合物[Cu(PDA)(2,2’-bpy)]·5H_2O(1)、[Cu_2(PDA)_(1.5)(2,2’-bpy)_2](ClO_4)·5H_2O(2)、[Zn_2(PDA)(2,2’-bpy)_2Cl_2](3)、[Cd(PDA)_(0.5)(2,2’-bpy)Cl](H_2PDA)(4)和[Cd_2(PDA)_2(2,2’-bpy)_2]·2H_2O(5)。配合物1~4都属于Triclinic晶系,P-1空间群。配合物1的中心铜离子的配位环境为六配位的八面体构型;配合物2中存在两种配位环境的铜离子,一种为五配位的金字塔构型,另一种为六配位的八面体构型;配合物3中的锌离子的配位环境是五配位的金字塔构型;配合物4中镉离子的配位环境是六配位的八面体构型。配合物5属于Monoclinic晶系,P2/c空间群,中心镉离子的配位环境为六配位的八面体构型。
配合物1通过配位键形成一维链状结构,通过π-π堆积作用和氢键作用而形成三维超分子结构。配合物2中对苯二乙酸用不同的配位模式通过配位键连接铜离子形成一维的阶梯状链状结构,而后又通过丰富的氢键和π-π堆积作用形成三维超分子结构。配合物3是个双核的配合物,π-π堆积作用在其形成三维超分子结构的过程中发挥了很大的作用。配合物4和5都是镉的一维链状配合物,不同的是配合物4中是对苯二乙酸和氯离子作为桥联配体交替连接镉离子而形成一维链,而配合物5中只有对苯二乙酸作为桥联配体把相邻的镉离子连接起来。配合物4中有游离的对苯二乙酸分子,配合物5中含有结晶水分子,氢键作用和π-π堆积作用使它们形成了三维的超分子结构。
第三章描述了以对苯二乙酸为主配体,邻菲啰啉为第二配体分别与铜盐、镍盐反应得到的四个配合物[Cu(PDA)(phen)]·2H_2O(6)、[Cu(HPDA)_2(phen)(H_2O)](7)、[Cu(PDA)(phen)_2]·(H_2PDA)(8)、[Ni(PDA)(phen)(H_2O)]_2(9)。配合物6和7都属于Monoclinic晶系,P21/c空间群,中心铜离子的配位环境也都为五配位的变形的金字塔构型。配合物8属于Triclinic晶系,P-1空间群,中心铜离子的配位环境为六配位的八面体构型。配合物9属于Monoclinic晶系P2(1)/n空间群,其中心镍离子的配位环境为六配位的八面体构型。
配合物6为一维的链状结构,通过氢键作用和超分子作用力而形成三维的超分子结构。配合物7和8都是单核结构,通过氢键作用和π-π堆积作用而形成三维的超分子结构。配合物9是个双核结构,对苯二乙酸采用顺式构型把两个镍离子连接起来形成一个环状结构,氢键作用把一个个环状结构连接成一维链,π-π堆积作用和分子间的范德华力又使它们形成了三维的超分子结构。
第四章描述了对苯二乙酸,DMF和铜盐反应形成的配位聚合物[Cu(PDA)(DMF)](10),它属于Triclinic晶系,P-1空间群,中心铜离子的配位环境为五配位的金字塔构型。配合物10是一个二维层状结构,具有大小为11.608×12.134 (A|°)的孔洞。配合物10的热重分析表明,该化合物具有较好的热稳定性。
第五章总结了本论文的研究成果,也指出了研究的不足之处,并对以后的研究工作提出了要求和期望。
In recent years, much attention has been paid to the complexes based on flexible ligands due to their versatile and novel structures and potential applications. 1, 4-Phenylenediacetic acid (H_2PDA) is one of the typical flexible ligands. It has two flexible acetates, resulting in trans- and cis-configuration. And the coordination modes of carboxylates are also complicated. So the complex structures based on H_2PDA are more versatile and novel. In order to research the relationship between their structures and properties, in this dissertation, we synthesized ten unreported transition metal complexes by liquid method. These complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, IR. We also studied the thermal decomposition behaviors and other facet of some complexes among them.
There are five chapters in this dissertation:
In the introduction, I firstly introduce the research status of coordination polymers, and their potential applications in gas storage, selective catalysis, nonlinear optical and magnetism. Secondly, the study condition of H_2PDA is introduced concisely at home and abroad.
In the second chapter, the synthesis, crystal structures and other properties of complexes [Cu(PDA)(2,2’-bpy)]·5H_2O(1)、[Cu_2(PDA)_(1.5)(2,2’-bpy)_2](ClO_4)·5H_2O(2)、[Zn_2(PDA)(2,2’-bpy)_2Cl_2](3)、[Cd(PDA)_(0.5)(2,2’-bpy)Cl](H_2PDA)(4) and [Cd_2(PDA)_2(2,2’-bpy)_2]·2H_2O(5) which were synthesized by H_2PDA, 2,2’-bipyridine and transition metal salts are described. The complexes 1~4 belong to Triclinic crystal system, P-1 space group. The central copper ions in complex 1 are six-coordinated with a distorted octahedral geometry; there are two kinds of copper ions in complex 2, one is five-coordinated with a nearly pyramid geometry, the other is six-coordinated with a distorted octahedral geometry; The central zinc ions in complex 3 is five-coordinated with a nearly pyramid geometry; The central cadmium ions in complex 4 are six-coordinated with a distorted octahedral geometry. The complex 5 belongs to Monoclinic crystal system, P2/c space group, the central cadmium ions are six-coordinated with a distorted octahedral geometry just like in complex 4.
Complex 1 forms a 1D chain structure by coordination bonds and complicated hydrogen bonds andπ-πstacking interactions make this complex a 3D supramolecular structure. In complex 2, H_2PDA with different coordination modes connect copper ions via coordination bonds to form a one-dimensional ladder-like chain. Abundant hydrogen bonds andπ-πstacking interactions result in the formation of a 3D supramolecular structure. Complex 3 is a dimer andπ-πstacking interactions play an important role in the formation of 3D supramolecular structure. Complex 4 and 5 both are 1D chain-like structures of cadmium, the difference is that in complex 4, Cd (II) ions are alternately bridged by PDA ligands and chloride ions into 1D chains but in complex 5 only PDA ligands act as bridge-ligand to connect Cd (II) ions together. In complex 4, there are free H_2PDA molecules and in complex 5 there are crystallographically independent water molecules. The hydrogen bonds andπ-πstacking interactions make them form 3D supramolecular structures.
In the third chapter, I describe the synthesis, crystal structures and other properties of complexes [Cu(PDA)(phen)]·2H_2O(6)、[Cu(HPDA)_2(phen)(H_2O)](7)、[Cu(PDA)(phen)_2]·(H_2PDA)(8)、[Ni(PDA)(phen)(H_2O)]_2(9) which were synthesized by H_2PDA, 1,10-phenanthroline and corresponding metallic salts. The complexes 6 and 7 belong to Monoclinic crystal system, P21/c space group, and the central copper ions are both five-coordinated with a distorted pyramid geometry. Complex 8 belongs to Triclinic crystal system, P-1 space group and the central copper ions are six-coordinated with a distorted octahedral geometry. Complex 9 belongs to Monoclinic crystal system, P2(1)/n space group, the central nickel ions are six-coordinated with a nearly octahedral geometry.
Complex 6 forms a 1D chain structure by coordination bonds and complicated hydrogen bonds andπ-πstacking interactions result in the formation of a 3D supramolecular structure. Complex 7 and 8 both are mononuclear complexes, forming 3D supramolecules structures via hydrogen bonds andπ-πstacking interactions. Complex 9 is a dimer and two Ni(Ⅱ) ions are linked by two PDA ligands with cis-configuration, resulting in a cyclic structure. The cyclic structures are linked one by one through hydrogen bonds into 1D chains andπ-πstacking interactions between 1,10-phenanthroline molecules of adjacent dimer bring the formation of a 3D supramolecular network.
In the fourth chapter, I describe the synthesis, crystal structure and thermal property of a coordination polymer [Cu(PDA)(DMF)](10). It belongs to Triclinic crystal system, P-1 space group and the central copper ions are five-coordinated with a nearly pyramid geometry. It is a two-dimensional square network with the caves’size being 11.608×12.134 (A|°). Thermogravimetric analysis indicates this complex have good thermal stability.
In the fifth chapter, I summarize the achievements and defects systematically in the dissertation, and put forward proposals and expectations in the future.
本论文分为以下五章:
绪论部分首先着重介绍了配位聚合物的研究现状,及它们在气体吸附、催化反应和光学、磁学方面的潜在应用。然后详细介绍了对苯二乙酸在国内外的研究概况。
第二章描述了以对苯二乙酸为主配体,2,2’-联吡啶为第二配体分别与铜盐、锌盐、镉盐反应得到的五个配合物[Cu(PDA)(2,2’-bpy)]·5H_2O(1)、[Cu_2(PDA)_(1.5)(2,2’-bpy)_2](ClO_4)·5H_2O(2)、[Zn_2(PDA)(2,2’-bpy)_2Cl_2](3)、[Cd(PDA)_(0.5)(2,2’-bpy)Cl](H_2PDA)(4)和[Cd_2(PDA)_2(2,2’-bpy)_2]·2H_2O(5)。配合物1~4都属于Triclinic晶系,P-1空间群。配合物1的中心铜离子的配位环境为六配位的八面体构型;配合物2中存在两种配位环境的铜离子,一种为五配位的金字塔构型,另一种为六配位的八面体构型;配合物3中的锌离子的配位环境是五配位的金字塔构型;配合物4中镉离子的配位环境是六配位的八面体构型。配合物5属于Monoclinic晶系,P2/c空间群,中心镉离子的配位环境为六配位的八面体构型。
配合物1通过配位键形成一维链状结构,通过π-π堆积作用和氢键作用而形成三维超分子结构。配合物2中对苯二乙酸用不同的配位模式通过配位键连接铜离子形成一维的阶梯状链状结构,而后又通过丰富的氢键和π-π堆积作用形成三维超分子结构。配合物3是个双核的配合物,π-π堆积作用在其形成三维超分子结构的过程中发挥了很大的作用。配合物4和5都是镉的一维链状配合物,不同的是配合物4中是对苯二乙酸和氯离子作为桥联配体交替连接镉离子而形成一维链,而配合物5中只有对苯二乙酸作为桥联配体把相邻的镉离子连接起来。配合物4中有游离的对苯二乙酸分子,配合物5中含有结晶水分子,氢键作用和π-π堆积作用使它们形成了三维的超分子结构。
第三章描述了以对苯二乙酸为主配体,邻菲啰啉为第二配体分别与铜盐、镍盐反应得到的四个配合物[Cu(PDA)(phen)]·2H_2O(6)、[Cu(HPDA)_2(phen)(H_2O)](7)、[Cu(PDA)(phen)_2]·(H_2PDA)(8)、[Ni(PDA)(phen)(H_2O)]_2(9)。配合物6和7都属于Monoclinic晶系,P21/c空间群,中心铜离子的配位环境也都为五配位的变形的金字塔构型。配合物8属于Triclinic晶系,P-1空间群,中心铜离子的配位环境为六配位的八面体构型。配合物9属于Monoclinic晶系P2(1)/n空间群,其中心镍离子的配位环境为六配位的八面体构型。
配合物6为一维的链状结构,通过氢键作用和超分子作用力而形成三维的超分子结构。配合物7和8都是单核结构,通过氢键作用和π-π堆积作用而形成三维的超分子结构。配合物9是个双核结构,对苯二乙酸采用顺式构型把两个镍离子连接起来形成一个环状结构,氢键作用把一个个环状结构连接成一维链,π-π堆积作用和分子间的范德华力又使它们形成了三维的超分子结构。
第四章描述了对苯二乙酸,DMF和铜盐反应形成的配位聚合物[Cu(PDA)(DMF)](10),它属于Triclinic晶系,P-1空间群,中心铜离子的配位环境为五配位的金字塔构型。配合物10是一个二维层状结构,具有大小为11.608×12.134 (A|°)的孔洞。配合物10的热重分析表明,该化合物具有较好的热稳定性。
第五章总结了本论文的研究成果,也指出了研究的不足之处,并对以后的研究工作提出了要求和期望。
In recent years, much attention has been paid to the complexes based on flexible ligands due to their versatile and novel structures and potential applications. 1, 4-Phenylenediacetic acid (H_2PDA) is one of the typical flexible ligands. It has two flexible acetates, resulting in trans- and cis-configuration. And the coordination modes of carboxylates are also complicated. So the complex structures based on H_2PDA are more versatile and novel. In order to research the relationship between their structures and properties, in this dissertation, we synthesized ten unreported transition metal complexes by liquid method. These complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, IR. We also studied the thermal decomposition behaviors and other facet of some complexes among them.
There are five chapters in this dissertation:
In the introduction, I firstly introduce the research status of coordination polymers, and their potential applications in gas storage, selective catalysis, nonlinear optical and magnetism. Secondly, the study condition of H_2PDA is introduced concisely at home and abroad.
In the second chapter, the synthesis, crystal structures and other properties of complexes [Cu(PDA)(2,2’-bpy)]·5H_2O(1)、[Cu_2(PDA)_(1.5)(2,2’-bpy)_2](ClO_4)·5H_2O(2)、[Zn_2(PDA)(2,2’-bpy)_2Cl_2](3)、[Cd(PDA)_(0.5)(2,2’-bpy)Cl](H_2PDA)(4) and [Cd_2(PDA)_2(2,2’-bpy)_2]·2H_2O(5) which were synthesized by H_2PDA, 2,2’-bipyridine and transition metal salts are described. The complexes 1~4 belong to Triclinic crystal system, P-1 space group. The central copper ions in complex 1 are six-coordinated with a distorted octahedral geometry; there are two kinds of copper ions in complex 2, one is five-coordinated with a nearly pyramid geometry, the other is six-coordinated with a distorted octahedral geometry; The central zinc ions in complex 3 is five-coordinated with a nearly pyramid geometry; The central cadmium ions in complex 4 are six-coordinated with a distorted octahedral geometry. The complex 5 belongs to Monoclinic crystal system, P2/c space group, the central cadmium ions are six-coordinated with a distorted octahedral geometry just like in complex 4.
Complex 1 forms a 1D chain structure by coordination bonds and complicated hydrogen bonds andπ-πstacking interactions make this complex a 3D supramolecular structure. In complex 2, H_2PDA with different coordination modes connect copper ions via coordination bonds to form a one-dimensional ladder-like chain. Abundant hydrogen bonds andπ-πstacking interactions result in the formation of a 3D supramolecular structure. Complex 3 is a dimer andπ-πstacking interactions play an important role in the formation of 3D supramolecular structure. Complex 4 and 5 both are 1D chain-like structures of cadmium, the difference is that in complex 4, Cd (II) ions are alternately bridged by PDA ligands and chloride ions into 1D chains but in complex 5 only PDA ligands act as bridge-ligand to connect Cd (II) ions together. In complex 4, there are free H_2PDA molecules and in complex 5 there are crystallographically independent water molecules. The hydrogen bonds andπ-πstacking interactions make them form 3D supramolecular structures.
In the third chapter, I describe the synthesis, crystal structures and other properties of complexes [Cu(PDA)(phen)]·2H_2O(6)、[Cu(HPDA)_2(phen)(H_2O)](7)、[Cu(PDA)(phen)_2]·(H_2PDA)(8)、[Ni(PDA)(phen)(H_2O)]_2(9) which were synthesized by H_2PDA, 1,10-phenanthroline and corresponding metallic salts. The complexes 6 and 7 belong to Monoclinic crystal system, P21/c space group, and the central copper ions are both five-coordinated with a distorted pyramid geometry. Complex 8 belongs to Triclinic crystal system, P-1 space group and the central copper ions are six-coordinated with a distorted octahedral geometry. Complex 9 belongs to Monoclinic crystal system, P2(1)/n space group, the central nickel ions are six-coordinated with a nearly octahedral geometry.
Complex 6 forms a 1D chain structure by coordination bonds and complicated hydrogen bonds andπ-πstacking interactions result in the formation of a 3D supramolecular structure. Complex 7 and 8 both are mononuclear complexes, forming 3D supramolecules structures via hydrogen bonds andπ-πstacking interactions. Complex 9 is a dimer and two Ni(Ⅱ) ions are linked by two PDA ligands with cis-configuration, resulting in a cyclic structure. The cyclic structures are linked one by one through hydrogen bonds into 1D chains andπ-πstacking interactions between 1,10-phenanthroline molecules of adjacent dimer bring the formation of a 3D supramolecular network.
In the fourth chapter, I describe the synthesis, crystal structure and thermal property of a coordination polymer [Cu(PDA)(DMF)](10). It belongs to Triclinic crystal system, P-1 space group and the central copper ions are five-coordinated with a nearly pyramid geometry. It is a two-dimensional square network with the caves’size being 11.608×12.134 (A|°). Thermogravimetric analysis indicates this complex have good thermal stability.
In the fifth chapter, I summarize the achievements and defects systematically in the dissertation, and put forward proposals and expectations in the future.
引文
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