过渡金属—脂肪族羟基多羧酸配位聚合物及钨钒金属氧簇的合成与表征
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摘要
本论文主要利用中温水热方法合成了钨钒金属氧簇化合物和脂肪族羟基多羧酸类配位聚合物等一系列无机/有机杂化材料,对它们进行了X?射线单晶结构测定以及相关的性能表征。在合成配位聚合物方面,作者对脂肪族羟基多羧酸与含氮有机配体的混和体系进行了重点的研究,发现了柠檬酸的两种新配位模式,并合成了三种具有新结构的配位聚合物;在非经典金属氧簇研究方面,作者主要着眼于钨钒体系,合成出了首例三帽单支撑结构的钨钒Keggin簇。
1、选用过渡金属盐?柠檬酸?4,4’?bpy体系合成了三个配位聚合物Ni_2(H_2cit)_2(4,4’-bpy) 1、Zn4(cit)_2(4,4’-bpy)_2(H_2O)2-3H_2O 2、Co_3(Hcit)_2(4,4’-bpy)_4(_2H_2O)-4H_2O 3,其中1和2中的柠檬酸配体展示出新的配位模式。对它们的合成条件进行了较详细研究,发现不同金属对合成条件的要求具有显著的差别。
2、选用过渡金属盐-苹果酸-含氮配体体系合成了两个配位化合物Zn(C_4H_4O_5)(4,4’-bpy)-2H_2O 4、Cd(C_4H_2O_4)(2,2’-bpy)_H_2O 5其中化合物4的结构中包含类似正方形的四核水簇,而化合物5则是由苹果酸发生原位脱水反应生成的,它的合成为有关苹果酸原位配体生成反应的研究又提供了新的依据。
3、利用常温结晶方法合成了一个由锌-酒石酸构成的具有分立结构的配位化合物[Zn_2(C_4H_4O_6)_2(4H_2O)]_2-12H_2O 6,但它并没有按我们的设计思路生成多维结构。
4、在中温水热条件下,合成了两个非经典结构的金属氧簇化合物{PW_5~VW_4~(VI)V_3~(IV)O_(40)(V~(IV)O)_3[Cu(en)_2]}[Cu(phen)_2]_3·4H_2O 7、(H_3N(CH_2)_2NH_3) [V4O10] 8其中,化合物7是首例具有三帽单支撑结构的钨钒Keggin簇。
在上述化合物中,1、2、4、6、7是首次合成的,化合物5的结构虽然已被人报道,但我们却利用不同的反应物在原位生成条件下得到了同样的结构。
Recently, many coordination compounds with special performances and various structures have been of great interests due to their potential applications as optical materials, superconductor, magnetic, ion exchange, separation and catalyst. Polyoxometalates (POMs) have been attracted extensive attention for many years owing to their interesting structural diversity and various potential applications in different areas such as catalysis, sorption, electrical conductivity, magnetism, photochemistry, medicine and material science. More and more researchers and groups focus their attentions on decorating and fine-tuning POMs at molecular level by capping and supporting them in order to explore their performances and various potential applications. In this paper, the hydroxylpolycarboxylic acids (citric acid, malic acid and tartaric acid) and N-heterocyclic organic ligands have been employed to act as building blocks, and six coordination compounds (1?6)have been got; we also synthesis two POMs (7,8)under hydrothermal condition. Among them, the structures of compound 1、2、4、 6、7 are novel. On the bases of X-ray structural analyses, some compounds have been characterized by IR, XPS, EPR and fluorescence spectra. The thermal analyses and magnetic properties of some compounds have also been studied, which would take a role in the explorations of structures and functions for the compounds.
1、We choose transition metal-citric acid-4,4’?bpy as starting materials and obtained three coordination compounds(1?3) under hydrothermal condition: In Ni_2(H_2cit)_2(4,4’_bpy) (1), the wave chains which is constructed by citric acid ligands and Ni2+ are connected with 4,4’-bpy to form a 2D structure, and the coordination mode of citric acid is novel; Zn_4(cit)_2(4,4’-bpy)_2(H_2O)_2-3H_2O(2) is 3D structure which is constructed by citric acid and 4,4’?bpy, and the citric acid in 2 exhibits novel coordination modes; Co_3(Hcit)_2(4,4’-bpy)_4(2H_2O)-4H_2O(3) is 3D structure, but unfortunately, it has been reported before.
2、Two coordination compounds have been synthesized in d10 metal?malic acid-N-heterocyclic organic ligands reaction system. Zn(C_4H_4O_5)(4,4’-bpy)-2H_2O(4) displays two-dimensional network constructed by malic ligand, 4,4’?bpy acts as terminal ligand alternatively extrude out two sides of the 2-D sheet which is containing a tetramer water cluster. For Cd(C4H2O4)(2,2’-bpy)-H_2O(5), the fumarate, which is obtained from the in situ dehydration reaction of malic acid, links Cd atoms to form 1?D zigzag chain with 2,2’?bpy extruding out of one side of the chain as terminal ligand, the structure of 5 has been reported before by fumarate as the starting material.
3、[Zn_2(C_4H_4O_6)_2(4H_2O)]2-12H_2O (6) has been obtained at room temperature, which is contained two dinuclear compounds and twelve lattice water molecular. The two planes of the two dinuclear compounds are vertical approximately, and water molecular distributes around them.
4、We try to synthesis some coordination compounds building with POMs, but a tri-capped mono-supporting Keggin structure tungstovanadophosphate{PW_5~VW_4~(VI)V_3~(IV)O_(40)(V~(IV)O)_3[Cu(en)_2]}[Cu(phen)_2]_3·4H_2O(7) and a vanadium cluster (H_3N(CH_2)2NH_3) [V4O10] (8)were obtained. They both can be further linked to form three-dimensional supramolecular networks through extensive hydrogen bonding.
1、选用过渡金属盐?柠檬酸?4,4’?bpy体系合成了三个配位聚合物Ni_2(H_2cit)_2(4,4’-bpy) 1、Zn4(cit)_2(4,4’-bpy)_2(H_2O)2-3H_2O 2、Co_3(Hcit)_2(4,4’-bpy)_4(_2H_2O)-4H_2O 3,其中1和2中的柠檬酸配体展示出新的配位模式。对它们的合成条件进行了较详细研究,发现不同金属对合成条件的要求具有显著的差别。
2、选用过渡金属盐-苹果酸-含氮配体体系合成了两个配位化合物Zn(C_4H_4O_5)(4,4’-bpy)-2H_2O 4、Cd(C_4H_2O_4)(2,2’-bpy)_H_2O 5其中化合物4的结构中包含类似正方形的四核水簇,而化合物5则是由苹果酸发生原位脱水反应生成的,它的合成为有关苹果酸原位配体生成反应的研究又提供了新的依据。
3、利用常温结晶方法合成了一个由锌-酒石酸构成的具有分立结构的配位化合物[Zn_2(C_4H_4O_6)_2(4H_2O)]_2-12H_2O 6,但它并没有按我们的设计思路生成多维结构。
4、在中温水热条件下,合成了两个非经典结构的金属氧簇化合物{PW_5~VW_4~(VI)V_3~(IV)O_(40)(V~(IV)O)_3[Cu(en)_2]}[Cu(phen)_2]_3·4H_2O 7、(H_3N(CH_2)_2NH_3) [V4O10] 8其中,化合物7是首例具有三帽单支撑结构的钨钒Keggin簇。
在上述化合物中,1、2、4、6、7是首次合成的,化合物5的结构虽然已被人报道,但我们却利用不同的反应物在原位生成条件下得到了同样的结构。
Recently, many coordination compounds with special performances and various structures have been of great interests due to their potential applications as optical materials, superconductor, magnetic, ion exchange, separation and catalyst. Polyoxometalates (POMs) have been attracted extensive attention for many years owing to their interesting structural diversity and various potential applications in different areas such as catalysis, sorption, electrical conductivity, magnetism, photochemistry, medicine and material science. More and more researchers and groups focus their attentions on decorating and fine-tuning POMs at molecular level by capping and supporting them in order to explore their performances and various potential applications. In this paper, the hydroxylpolycarboxylic acids (citric acid, malic acid and tartaric acid) and N-heterocyclic organic ligands have been employed to act as building blocks, and six coordination compounds (1?6)have been got; we also synthesis two POMs (7,8)under hydrothermal condition. Among them, the structures of compound 1、2、4、 6、7 are novel. On the bases of X-ray structural analyses, some compounds have been characterized by IR, XPS, EPR and fluorescence spectra. The thermal analyses and magnetic properties of some compounds have also been studied, which would take a role in the explorations of structures and functions for the compounds.
1、We choose transition metal-citric acid-4,4’?bpy as starting materials and obtained three coordination compounds(1?3) under hydrothermal condition: In Ni_2(H_2cit)_2(4,4’_bpy) (1), the wave chains which is constructed by citric acid ligands and Ni2+ are connected with 4,4’-bpy to form a 2D structure, and the coordination mode of citric acid is novel; Zn_4(cit)_2(4,4’-bpy)_2(H_2O)_2-3H_2O(2) is 3D structure which is constructed by citric acid and 4,4’?bpy, and the citric acid in 2 exhibits novel coordination modes; Co_3(Hcit)_2(4,4’-bpy)_4(2H_2O)-4H_2O(3) is 3D structure, but unfortunately, it has been reported before.
2、Two coordination compounds have been synthesized in d10 metal?malic acid-N-heterocyclic organic ligands reaction system. Zn(C_4H_4O_5)(4,4’-bpy)-2H_2O(4) displays two-dimensional network constructed by malic ligand, 4,4’?bpy acts as terminal ligand alternatively extrude out two sides of the 2-D sheet which is containing a tetramer water cluster. For Cd(C4H2O4)(2,2’-bpy)-H_2O(5), the fumarate, which is obtained from the in situ dehydration reaction of malic acid, links Cd atoms to form 1?D zigzag chain with 2,2’?bpy extruding out of one side of the chain as terminal ligand, the structure of 5 has been reported before by fumarate as the starting material.
3、[Zn_2(C_4H_4O_6)_2(4H_2O)]2-12H_2O (6) has been obtained at room temperature, which is contained two dinuclear compounds and twelve lattice water molecular. The two planes of the two dinuclear compounds are vertical approximately, and water molecular distributes around them.
4、We try to synthesis some coordination compounds building with POMs, but a tri-capped mono-supporting Keggin structure tungstovanadophosphate{PW_5~VW_4~(VI)V_3~(IV)O_(40)(V~(IV)O)_3[Cu(en)_2]}[Cu(phen)_2]_3·4H_2O(7) and a vanadium cluster (H_3N(CH_2)2NH_3) [V4O10] (8)were obtained. They both can be further linked to form three-dimensional supramolecular networks through extensive hydrogen bonding.
引文
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