金属叠氮/甲酸分子基磁性配合物研究
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摘要
构筑具有潜在应用价值的新型分子基磁性材料,研究磁性和结构的关系,已成为当今材料化学和配位化学中的热点课题之一。然而,如何通过桥连配体将自旋载体在特定的固体形态中排列使之拥有期望的磁学性能依旧是十分具有挑战性的任务。叠氮和甲酸在配位模式和磁传导性能上有很多相似点,在过去的二三十年中,数以千计具有有趣结构和特殊磁性的叠氮／甲酸金属配合物被合成报道。这些配合物的磁性依赖于自旋载体的种类和具体配合物的结构,而共配体以及合成条件则主要决定了配合物的结构。为了实现分子基磁性材料的定向合成和可控组装,并有效调控其结构与性能,还需要做大量的探索工作。
为探索分子基磁性材料的构筑条件,并进一步调控其结构与性能,发展多功能的分子基磁性固体,本文通过一系列桥连配体与自旋载体的选择及合成条件的调变,构筑了系列新颖的配合物并详细研究了其合成、结构、磁性及磁构关系等,取得系列成果。具体结果如下：
一、取代羧酸为共配体的金属叠氮铜配合物的构筑与性质。通过选取一系列结构相关并具有不同非配位基团的羧酸为辅助配体得到九个叠氮铜配合物。结构分析表明这些配合物都是基于syn,Syn羧基/EO叠氮混配的铜单元,辅助配体的非配位基团对叠氮离子的配位方式有着重要的影响。磁性研究表明,混配的syn,syn羧酸/EO叠氮在铜离子之间传递铁磁耦合,并与Cu-N-Cu的角度关系不大。高连接模式的叠氮如,μ-1,1.3和μ-1,1,3,3模式对配合物中长程磁有序的形成具有重要的作用。
二、杂环羧酸为共配体的金属甲酸配合物的构筑与性质。作为最小的有机羧酸,甲酸有多样的桥连模式并能有效传递磁耦合,而被广泛用于分子基磁性材料的构筑,并且甲酸和叠氮在配位模式和磁传导特征上有诸多相似之处。本文以杂环羧酸为共配体构筑了系列具有独特结构和磁行为的金属甲酸配合物。与金属叠氮化物不同,金属甲酸配合物中容易出现螺旋和多孔结构。磁性研究表明,尽管在配合物中甲酸主要传递反铁磁耦合,但在一些配合物中展示出亚铁磁和自旋倾斜的弱铁磁行为。
三、3d-3d异金属配合物的构筑与性质。由于不同3d金属离子的配位构型和半径的差异,在水热条件下某些多齿配体可以利用不同的配位齿的选择性与不同的金属离子配位。本文在在一锅反应中进行两种或多种金属离子的组装得到一系列3d-3d异金属配合物。两种金属的引入丰富了金属叠氮／甲酸配合物的种类和结构。磁性研究表明异金属的配合物和同金属配合物有很大不同,并且配合物的磁性可以通过金属离子种类的改变而进行调节。这为在异金属3d-3d配合物中通过金属离子的改变来调控其磁行为乃至定向设计合成提供了新的方法。
四、3d-4f异金属配合物的构筑与性质。镧系4f金属有更大的离子半径,并且某些4f离子还具有较高的磁各向异性,也是分子基磁性材料研究的热点。本文利用4f离子取代由2-吡啶基甲醇配体构筑的过渡金属配合物中的部分过渡金属离子,得到了一系列3d-4f的异金属配合物。结构分析表明叠氮／甲酸将双立方烷结构的3d-4f簇连接成一维链结构,而没有叠氮／甲酸存在时则得到基于立方烷结构的3d-4f簇合物。4f金属的引入改变了离子之间的磁相互作用,并显著加强了一维链体系的各向异性和单链磁体行为。
The construction of new molecule-based magnetic materials has become a fascinating subject in the fields of material and coordination chemistry for magneto-structural correlations as well as the development of new molecule-based materials. However, the rational arrangement of spin carriers in the solid state with desired properties by bridging ligands is still a great challenge. Azide and formate have similar coordination modes and transfer analogous interactions associated with it. In the past two decades, dozens of metal-azido/formate complexes with peculiar structures and magnetic properties have been reported. The co-ligands and synthesis condition are the primary factors in determining the structures of the complexes. In our efforts to construct new molecule-based magnetic materials and investigate the magneto-structural correlations, in this dissertation, a series of new magnetic complexes have been successfully obtained by the selection of suitable bridging ligands and spin carriers under different contitions, and structure and magnetic properties as well as the magneto-structural correlations were investigated. The main points are summarized as follows:
1、The copper-azido complexes with substituted carboxylate as co-ligand have been synthesized and studied. By using a series of structurally related carboxylate with different uncoordinated substituents as co-ligand, nine new azido-copper complexes were obtained. Structural analysis indicated the structures were based on the syn,syn carboxylate/EO azido mixed coordinating copper units and the coordination modes of the azido anions were affected greatly by the uncoordinating groups of the co-ligand. Magnetic study revealed that the syn,syn carboxylate/EO azido mixed bridges transfer ferromagnetic interactions between copper ions nearly irrelevent to the size of Cu-N-Cu angles, and azido ligands acting as high connecting mode such asμ-1,1,3 andμ-1,1,3,3 were significant in constructing complexes with long-range magnetic order.
2、The metal-formate complexes with heterocyclic carboxylate as co-ligand have been synthesized and studied. As the smallest carboxylate, formate displaying multiple bridging modes and being able to mediate magnetic coupling effectively between metal ions, has been well used in preparing molecular magnetic materials. The more important thing is that it has similarity with azide both in coordination modes and transferring magnetic coupling. By using our experience in preparing metal-azido complexes with carboxylate as co-ligand, we constructed a series of complexes with interesting structure and magnetic behaviors by using formate and different heterocyclic carboxylate as bridging ligands. Different from the metal-azido complexes, the formate tends to give helix and porous structures. Magnetic study revealed that dominating anti-ferromagnetic interactions were conducted by formate, and in some cases homospin ferrimagnetism and spin canting companying with the anti-ferromagnetic interactions.
3、Heterometallic 3d-3d complexes have been synthesized and studied. In the hydrothermal condition the assembling two or more kinds of metal ions in one pot give birth to series of heterometallic 3d-3d complexes. The polydentate ligands used coordinate to different kinds of metal ions using its different coordinated group for the variety of the 3d metal ions in coordination geometry and ionic radius. The introducing of two kinds of metal ions enriches the metal-azido/formate complexes. Magnetic study revealed that the magnetism of those complexes were distinct from the homometallic ones. And the magnetism can be tuned by varying the kinds of spin carriers. The successes of the magnetic control in the heterometallic 3d-3d complexes give us a new way to achieve "designing synthesis" and enrich the study of magneto-structural correlations.
4、Heterometallic 3d-4f complexes have been synthesized and studied. Using the 4f ions to partly substitute the 3d ions in some structure constructed by the ligand 2-Hydroxymethylpyridine brings series of 3d-4f homometallic complexes. The lanthanide 4f ions with large radius and, in some cases, high magnetic anisotropy bring novel srtucrure and amusing magnetic behavior. The azido/formate link dicubane-like 3d-4f clusters giving a 1D chain. And without azido/formate two cubane based cluster was separated. The introducing of the 4f ions not only change the magnetic interactions between metal ions but also enhance the anisotropy and single chain magnet behaviors of the 1D chain.
为探索分子基磁性材料的构筑条件,并进一步调控其结构与性能,发展多功能的分子基磁性固体,本文通过一系列桥连配体与自旋载体的选择及合成条件的调变,构筑了系列新颖的配合物并详细研究了其合成、结构、磁性及磁构关系等,取得系列成果。具体结果如下：
一、取代羧酸为共配体的金属叠氮铜配合物的构筑与性质。通过选取一系列结构相关并具有不同非配位基团的羧酸为辅助配体得到九个叠氮铜配合物。结构分析表明这些配合物都是基于syn,Syn羧基/EO叠氮混配的铜单元,辅助配体的非配位基团对叠氮离子的配位方式有着重要的影响。磁性研究表明,混配的syn,syn羧酸/EO叠氮在铜离子之间传递铁磁耦合,并与Cu-N-Cu的角度关系不大。高连接模式的叠氮如,μ-1,1.3和μ-1,1,3,3模式对配合物中长程磁有序的形成具有重要的作用。
二、杂环羧酸为共配体的金属甲酸配合物的构筑与性质。作为最小的有机羧酸,甲酸有多样的桥连模式并能有效传递磁耦合,而被广泛用于分子基磁性材料的构筑,并且甲酸和叠氮在配位模式和磁传导特征上有诸多相似之处。本文以杂环羧酸为共配体构筑了系列具有独特结构和磁行为的金属甲酸配合物。与金属叠氮化物不同,金属甲酸配合物中容易出现螺旋和多孔结构。磁性研究表明,尽管在配合物中甲酸主要传递反铁磁耦合,但在一些配合物中展示出亚铁磁和自旋倾斜的弱铁磁行为。
三、3d-3d异金属配合物的构筑与性质。由于不同3d金属离子的配位构型和半径的差异,在水热条件下某些多齿配体可以利用不同的配位齿的选择性与不同的金属离子配位。本文在在一锅反应中进行两种或多种金属离子的组装得到一系列3d-3d异金属配合物。两种金属的引入丰富了金属叠氮／甲酸配合物的种类和结构。磁性研究表明异金属的配合物和同金属配合物有很大不同,并且配合物的磁性可以通过金属离子种类的改变而进行调节。这为在异金属3d-3d配合物中通过金属离子的改变来调控其磁行为乃至定向设计合成提供了新的方法。
四、3d-4f异金属配合物的构筑与性质。镧系4f金属有更大的离子半径,并且某些4f离子还具有较高的磁各向异性,也是分子基磁性材料研究的热点。本文利用4f离子取代由2-吡啶基甲醇配体构筑的过渡金属配合物中的部分过渡金属离子,得到了一系列3d-4f的异金属配合物。结构分析表明叠氮／甲酸将双立方烷结构的3d-4f簇连接成一维链结构,而没有叠氮／甲酸存在时则得到基于立方烷结构的3d-4f簇合物。4f金属的引入改变了离子之间的磁相互作用,并显著加强了一维链体系的各向异性和单链磁体行为。
The construction of new molecule-based magnetic materials has become a fascinating subject in the fields of material and coordination chemistry for magneto-structural correlations as well as the development of new molecule-based materials. However, the rational arrangement of spin carriers in the solid state with desired properties by bridging ligands is still a great challenge. Azide and formate have similar coordination modes and transfer analogous interactions associated with it. In the past two decades, dozens of metal-azido/formate complexes with peculiar structures and magnetic properties have been reported. The co-ligands and synthesis condition are the primary factors in determining the structures of the complexes. In our efforts to construct new molecule-based magnetic materials and investigate the magneto-structural correlations, in this dissertation, a series of new magnetic complexes have been successfully obtained by the selection of suitable bridging ligands and spin carriers under different contitions, and structure and magnetic properties as well as the magneto-structural correlations were investigated. The main points are summarized as follows:
1、The copper-azido complexes with substituted carboxylate as co-ligand have been synthesized and studied. By using a series of structurally related carboxylate with different uncoordinated substituents as co-ligand, nine new azido-copper complexes were obtained. Structural analysis indicated the structures were based on the syn,syn carboxylate/EO azido mixed coordinating copper units and the coordination modes of the azido anions were affected greatly by the uncoordinating groups of the co-ligand. Magnetic study revealed that the syn,syn carboxylate/EO azido mixed bridges transfer ferromagnetic interactions between copper ions nearly irrelevent to the size of Cu-N-Cu angles, and azido ligands acting as high connecting mode such asμ-1,1,3 andμ-1,1,3,3 were significant in constructing complexes with long-range magnetic order.
2、The metal-formate complexes with heterocyclic carboxylate as co-ligand have been synthesized and studied. As the smallest carboxylate, formate displaying multiple bridging modes and being able to mediate magnetic coupling effectively between metal ions, has been well used in preparing molecular magnetic materials. The more important thing is that it has similarity with azide both in coordination modes and transferring magnetic coupling. By using our experience in preparing metal-azido complexes with carboxylate as co-ligand, we constructed a series of complexes with interesting structure and magnetic behaviors by using formate and different heterocyclic carboxylate as bridging ligands. Different from the metal-azido complexes, the formate tends to give helix and porous structures. Magnetic study revealed that dominating anti-ferromagnetic interactions were conducted by formate, and in some cases homospin ferrimagnetism and spin canting companying with the anti-ferromagnetic interactions.
3、Heterometallic 3d-3d complexes have been synthesized and studied. In the hydrothermal condition the assembling two or more kinds of metal ions in one pot give birth to series of heterometallic 3d-3d complexes. The polydentate ligands used coordinate to different kinds of metal ions using its different coordinated group for the variety of the 3d metal ions in coordination geometry and ionic radius. The introducing of two kinds of metal ions enriches the metal-azido/formate complexes. Magnetic study revealed that the magnetism of those complexes were distinct from the homometallic ones. And the magnetism can be tuned by varying the kinds of spin carriers. The successes of the magnetic control in the heterometallic 3d-3d complexes give us a new way to achieve "designing synthesis" and enrich the study of magneto-structural correlations.
4、Heterometallic 3d-4f complexes have been synthesized and studied. Using the 4f ions to partly substitute the 3d ions in some structure constructed by the ligand 2-Hydroxymethylpyridine brings series of 3d-4f homometallic complexes. The lanthanide 4f ions with large radius and, in some cases, high magnetic anisotropy bring novel srtucrure and amusing magnetic behavior. The azido/formate link dicubane-like 3d-4f clusters giving a 1D chain. And without azido/formate two cubane based cluster was separated. The introducing of the 4f ions not only change the magnetic interactions between metal ions but also enhance the anisotropy and single chain magnet behaviors of the 1D chain.
引文
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