金属叠氮配合物和多核金属簇化合物的合成、结构与磁性研究
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摘要
结构独特的分子基磁性材料因其重要的性质和潜在应用前景已经成为材料化学和无机化学领域中最为热门的课题之一。以叠氮桥为主要磁交换通道的叠氮金属化合物由于在磁性方面的优异性质引起了人们极大的兴趣。目前,尽管上千种结构新颖、磁性功能各异的叠氮金属配合物被报导,但叠氮同羧酸桥一起构筑的磁性化合物的例子鲜有报导。这可能是由于合成上电荷竞争,且磁耦合方式经常抵消。因此要构筑叠氮-羧酸化合物,特别是铁磁体将是很具挑战性的工作。具有单分子磁体行为的多核金属簇合物由于呈现出慢磁弛豫、量子隧穿、相干涉等奇特的磁现象,在高密度信息存储、量子计算机和自旋电子学等领域具有潜在的应用前景而受到研究者的密切关注。到目前,尽管有两百多例单分子磁体、近千个高核金属簇合物被报导,但无论是在其广度还是深度上都有很大的不足。尤其是在簇核数的增加、分子的磁各向异性和基念自旋值的增大,Blocking温度的升高,加深对磁交换机理的理解、调控结构实现对磁性能的改进等方面的深入研究显得尤为迫切。本论文主要开展了两方面的工作,对四个叠氮金属磁性化合物和二十个多核金属簇合物的合成、结构及磁性进行了研究,具体如下:
第一章简要介绍本论文工作的研究背景与相关概念,并对叠氮磁性化合物和多核金属簇合物的研究现状进行了简要的总结和评述。在此基础上阐明了本论文的选题依据和目的,以及所取得的主要进展。
第二章研究了金属叠氮配合物。以刚性的有机羧酸为辅助配体,水热条件下成功构筑了四个金属叠氮配合物(1-4),解析了它们的晶体结构,并研究了它们的磁性。晶体结构分析表明,在这些配合物中,叠氮桥主要采取了铁磁耦合方式的桥连模式:化合物分别具有三维、一维、零维和二维结构。磁性研究表明化合物总体上分别呈现铁磁、铁磁、铁磁和反铁磁行为,其中1和3为铁磁体,而且DFT理论计算完美地解释了2和3中细微的结构变化对磁性质的影响。配合物1为第一个叠氮/羧酸铁磁体。
第三章研究了多核Fe-Ln簇合物。通过溶剂热法,把稀土离子引入大Fe~Ⅲ体系,合成了十个Fe-Ln簇合物(5-14),解析了它们的晶体结构,并研究了部分化合物的磁性。结构表明它们都是具有十六核的Fe_(12)Ln_4结构的化合物;而磁性研究表明Fe-O核内存在竞争的反铁磁和铁磁耦合作用,从而产生了S=8的基态自旋值,而且部分稀土离子的单离子磁各向异性诱导出了化合物的磁各向异性,呈现出了慢磁弛豫现象。Fe_(12)Ln_4是目前最大的Fe-Ln簇。
第四章研究了多核铁簇合物。主要通过溶剂热法,构筑了七个铁簇化合物(15-21),解析了它们的晶体结构。结构表明它们分别为Fe_8棒、Fe_8轮、Fe_8簇、Fe_8簇、具有交替[Fe_3]和[FeNa_2]单元的一维链、以[Fe_6]轮为基元的一维链和以[Fe_(20)]簇为基元的二维网络。磁性研究表明在21中,[Fe_(20)]单元内反铁磁耦合导致了自旋阻挫,产生了S=5的基态自旋值。21中的[Fe_(20)]单元是目前最大的铁簇单元。
第五章研究了多核锰簇合物。通过溶剂热法,构筑了三个锰化合物(22-24),解析了它们的晶体结构,并研究了其中化合物24的磁性。结构分析表明它们分别是Mn_(12)簇、Mn_(12)簇和以[Mn_(12)]簇为基元的二维网络。磁性研究表明在24中,[Mn_(12)]簇内存在较强的反铁磁耦合,而且在2.4 K以下才出现交流信号。结构的调控使22-24中Mn~Ⅲ的易轴取向实现了簇内平行/晶格内垂直(22)到簇内平行/晶格内平行(23和24)的转变。
The investigation of molecule-based magnetic materials with fascinating structures has become one of the most active fields in materials and inorganic chemistry for their interesting properties and potential application. Azido-metal compounds in which azido bridges provide the magnetic exchange pathways have evoked researchers' considerable interest because of their unusual magnetic properties. So far, over a thousand azido-metal complexes, with novel structures and diverse magnetic properties, have been reported. However, azido/carboxylate compounds which consist of azido and carboxylate bridges have seldom been reported, probably due to competition of charge from synthesis and offset of couplings from magnetism. So, to construct azido/carboxylate compounds, especially ferromagnet, is a challenging task. Because their unique phenomena of slow relaxation of magnetization, quantum tunnel effects and phase interference make them very promising for applications in high density information storage, quantum computing and molecular spintronics, polynuclear cluster compounds with single molecule magnet (SMM) behaviors attract researchers' great attentions. Up to till, over two hundred SMMs and a thousand polynuclear metal clusters have been reported, but there are still lots of shortages in width and depth. It is urgent to carry out more profound investigation from several aspects: increasing nuclearity, heightening magnetic anisotropy and spin ground state, enhancing the blocking temperature, apprehending mechanism of magnetic exchange, improving magnetic properties through tune of structure. This thesis, containing two parts, has studied the syntheses, structures and magnetic properties of four azido-metal magnetic complexes and twenty polynuclear cluster compounds. The concrete contents consisting of five chapters are as follows:
In chapter 1, a brief introduction of the background and relative concepts of this work are presented. The progresses of azido magnetic compound and polynuclear metal cluster are concisely reviewed, and the research significance and main results of this thesis are also summarized.
In chapter 2, four azido-metal complexes are described. Under hydrothermal condition, four azido-metal complexes (1-4) have been constructed from rigid organic carboxylate ligands. Their structural characterizations show that azido anions mainly takes on ferromagnetic bridging modes in all the compounds, and their overall strutures are 3D, 1D, 0D and 2D, respectively. The studies of magnetic properties indicate that global ferromagnetic, ferromagnetic, ferromagnetic and antiferromagnetic behaviors are observed, respectively, in which complexes 1 and 3 are long-range ordered ferromagnets, moreover, for 2 and 3, DFT calculations have perfectly explained the alteration of structures effecting on the magnetic properties. Complex 1 is the first ferromagnet in azido/carboxylate system.
In chapter 3, the syntheses, structures and magnetic properties of Fe-Ln clusters are studied. By incorporation of Ln~Ⅲinto Fe~Ⅲsystem, ten Fe-Ln clusters (5-14) are obtained under solvothermal conditions. X-ray single crystal diffractions indicate that they have hexadeca-nuclear Fe_(12)Ln_4 topology. Magnetic measurement demonstrate that competitive antiferromagnetic and ferromagnetic couplings in Fe-O core result in spin ground state of S = 8. Moreover, molecular magnetic anisotropy has been induced from single-ion magnetic anisotropy of Sm~Ⅲ, and exhibited slow relaxation of magnetization. These Fe_(12)Ln_4 clusters are the largest cluster in Fe-Ln system.
In chapter 4, the syntheses, structures and magnetic properties of Fe~Ⅲclusters are investigated. Seven Fe~Ⅲcompounds (15-21) are prepared solvothermally, and which are structurally characterized by X-ray single crystal diffraction. Their crystal structures can be described as Fe_8 rod, Fe_8 wheel, Fe_8 cluster, Fe_8 cluster, 1D alternating [Fe_3] and [FeNa_2] chain, 1D [Fe_6] wheel chain and 2D sheet based on [Fe_(20)] cluster, respectively. Magnetic measurement of 21 indicate that competitive antiferromagnetic couplings result in spin frustration in [Fe_(20)] unit, which produce a spin ground state of S = 5. The [Fe_(20)] unit in 21 is the largest iron unit.
In chapter 5, the syntheses, structures and magnetic properties of Mn clusters are discussed. Three Mn complexes (22-24) are obtained from solvothermal conditions, and their structures are Mn_(12) cluster, Mn_(12) cluster and 2D network based on [Mn_(12)] unit, respectively. For 24, the study of magnetic properties demonstrate that couplings in [Mn_(12)] unit are strongly antiferromagnetic, and ac signals can be detected below 2.4 K. Structural modifications in 22-24 have made the easy-axial directions of Mn~Ⅲions shifted from parallel in cluster/vertical in crystal lattice (22) to parallel in cluster/parallel in crystal lattice (23 and 24).
第一章简要介绍本论文工作的研究背景与相关概念,并对叠氮磁性化合物和多核金属簇合物的研究现状进行了简要的总结和评述。在此基础上阐明了本论文的选题依据和目的,以及所取得的主要进展。
第二章研究了金属叠氮配合物。以刚性的有机羧酸为辅助配体,水热条件下成功构筑了四个金属叠氮配合物(1-4),解析了它们的晶体结构,并研究了它们的磁性。晶体结构分析表明,在这些配合物中,叠氮桥主要采取了铁磁耦合方式的桥连模式:化合物分别具有三维、一维、零维和二维结构。磁性研究表明化合物总体上分别呈现铁磁、铁磁、铁磁和反铁磁行为,其中1和3为铁磁体,而且DFT理论计算完美地解释了2和3中细微的结构变化对磁性质的影响。配合物1为第一个叠氮/羧酸铁磁体。
第三章研究了多核Fe-Ln簇合物。通过溶剂热法,把稀土离子引入大Fe~Ⅲ体系,合成了十个Fe-Ln簇合物(5-14),解析了它们的晶体结构,并研究了部分化合物的磁性。结构表明它们都是具有十六核的Fe_(12)Ln_4结构的化合物;而磁性研究表明Fe-O核内存在竞争的反铁磁和铁磁耦合作用,从而产生了S=8的基态自旋值,而且部分稀土离子的单离子磁各向异性诱导出了化合物的磁各向异性,呈现出了慢磁弛豫现象。Fe_(12)Ln_4是目前最大的Fe-Ln簇。
第四章研究了多核铁簇合物。主要通过溶剂热法,构筑了七个铁簇化合物(15-21),解析了它们的晶体结构。结构表明它们分别为Fe_8棒、Fe_8轮、Fe_8簇、Fe_8簇、具有交替[Fe_3]和[FeNa_2]单元的一维链、以[Fe_6]轮为基元的一维链和以[Fe_(20)]簇为基元的二维网络。磁性研究表明在21中,[Fe_(20)]单元内反铁磁耦合导致了自旋阻挫,产生了S=5的基态自旋值。21中的[Fe_(20)]单元是目前最大的铁簇单元。
第五章研究了多核锰簇合物。通过溶剂热法,构筑了三个锰化合物(22-24),解析了它们的晶体结构,并研究了其中化合物24的磁性。结构分析表明它们分别是Mn_(12)簇、Mn_(12)簇和以[Mn_(12)]簇为基元的二维网络。磁性研究表明在24中,[Mn_(12)]簇内存在较强的反铁磁耦合,而且在2.4 K以下才出现交流信号。结构的调控使22-24中Mn~Ⅲ的易轴取向实现了簇内平行/晶格内垂直(22)到簇内平行/晶格内平行(23和24)的转变。
The investigation of molecule-based magnetic materials with fascinating structures has become one of the most active fields in materials and inorganic chemistry for their interesting properties and potential application. Azido-metal compounds in which azido bridges provide the magnetic exchange pathways have evoked researchers' considerable interest because of their unusual magnetic properties. So far, over a thousand azido-metal complexes, with novel structures and diverse magnetic properties, have been reported. However, azido/carboxylate compounds which consist of azido and carboxylate bridges have seldom been reported, probably due to competition of charge from synthesis and offset of couplings from magnetism. So, to construct azido/carboxylate compounds, especially ferromagnet, is a challenging task. Because their unique phenomena of slow relaxation of magnetization, quantum tunnel effects and phase interference make them very promising for applications in high density information storage, quantum computing and molecular spintronics, polynuclear cluster compounds with single molecule magnet (SMM) behaviors attract researchers' great attentions. Up to till, over two hundred SMMs and a thousand polynuclear metal clusters have been reported, but there are still lots of shortages in width and depth. It is urgent to carry out more profound investigation from several aspects: increasing nuclearity, heightening magnetic anisotropy and spin ground state, enhancing the blocking temperature, apprehending mechanism of magnetic exchange, improving magnetic properties through tune of structure. This thesis, containing two parts, has studied the syntheses, structures and magnetic properties of four azido-metal magnetic complexes and twenty polynuclear cluster compounds. The concrete contents consisting of five chapters are as follows:
In chapter 1, a brief introduction of the background and relative concepts of this work are presented. The progresses of azido magnetic compound and polynuclear metal cluster are concisely reviewed, and the research significance and main results of this thesis are also summarized.
In chapter 2, four azido-metal complexes are described. Under hydrothermal condition, four azido-metal complexes (1-4) have been constructed from rigid organic carboxylate ligands. Their structural characterizations show that azido anions mainly takes on ferromagnetic bridging modes in all the compounds, and their overall strutures are 3D, 1D, 0D and 2D, respectively. The studies of magnetic properties indicate that global ferromagnetic, ferromagnetic, ferromagnetic and antiferromagnetic behaviors are observed, respectively, in which complexes 1 and 3 are long-range ordered ferromagnets, moreover, for 2 and 3, DFT calculations have perfectly explained the alteration of structures effecting on the magnetic properties. Complex 1 is the first ferromagnet in azido/carboxylate system.
In chapter 3, the syntheses, structures and magnetic properties of Fe-Ln clusters are studied. By incorporation of Ln~Ⅲinto Fe~Ⅲsystem, ten Fe-Ln clusters (5-14) are obtained under solvothermal conditions. X-ray single crystal diffractions indicate that they have hexadeca-nuclear Fe_(12)Ln_4 topology. Magnetic measurement demonstrate that competitive antiferromagnetic and ferromagnetic couplings in Fe-O core result in spin ground state of S = 8. Moreover, molecular magnetic anisotropy has been induced from single-ion magnetic anisotropy of Sm~Ⅲ, and exhibited slow relaxation of magnetization. These Fe_(12)Ln_4 clusters are the largest cluster in Fe-Ln system.
In chapter 4, the syntheses, structures and magnetic properties of Fe~Ⅲclusters are investigated. Seven Fe~Ⅲcompounds (15-21) are prepared solvothermally, and which are structurally characterized by X-ray single crystal diffraction. Their crystal structures can be described as Fe_8 rod, Fe_8 wheel, Fe_8 cluster, Fe_8 cluster, 1D alternating [Fe_3] and [FeNa_2] chain, 1D [Fe_6] wheel chain and 2D sheet based on [Fe_(20)] cluster, respectively. Magnetic measurement of 21 indicate that competitive antiferromagnetic couplings result in spin frustration in [Fe_(20)] unit, which produce a spin ground state of S = 5. The [Fe_(20)] unit in 21 is the largest iron unit.
In chapter 5, the syntheses, structures and magnetic properties of Mn clusters are discussed. Three Mn complexes (22-24) are obtained from solvothermal conditions, and their structures are Mn_(12) cluster, Mn_(12) cluster and 2D network based on [Mn_(12)] unit, respectively. For 24, the study of magnetic properties demonstrate that couplings in [Mn_(12)] unit are strongly antiferromagnetic, and ac signals can be detected below 2.4 K. Structural modifications in 22-24 have made the easy-axial directions of Mn~Ⅲions shifted from parallel in cluster/vertical in crystal lattice (22) to parallel in cluster/parallel in crystal lattice (23 and 24).
引文
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