吡嗪四羧酸稀土配位聚合物的合成、结构及性质研究
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摘要
配位聚合物是有机配体与金属离子(或金属簇)通过超分子自组装方式形成的以配位键结合而成的聚合物。其结构新颖,性质独特,在诸如分子识别、催化、吸附等领域有良好的应用前景。吡嗪四羧酸是含有N、O的多齿有机配体,具有丰富多样的配位方式,易于形成结构新颖的配合物；稀土金属能提供较多的空轨道,其配合物多具有独特的荧光和磁性质。本文选取吡嗪四羧酸与稀土硝酸盐(硝酸镝、硝酸铕、硝酸铽、硝酸钆)分别通过水热法和溶剂挥发法,合成配位聚合物并采用X-射线单晶衍射,X-射线粉末衍射,元素分析、红外光谱、热重分析、荧光分析等技术手段对所得产品进行表征。主要工作如下：
1.以吩嗪为原料,合成了吡嗪四羧酸。
2.以吡嗪四羧酸为配体,硝酸镝、硝酸铽、硝酸铕为中心原子,采用水热合成法得到了配位聚合物(1)-(3)。配合物(1)为三斜晶系,P-1空间群的三维结构配位聚合物。其晶胞参数为：a=9.0069(4)A,b=10.8801(2)A,c=13.246 A,α=68.725(8)°,p=77.990(8)°,γ=88.618(10)°。该配合物中,Dy3+有九配位和八配位两种配位方式,其中九配位的Dy3+直接与吡嗪四羧酸配位,八配位的Dy3+则与羧基、羟基和水形成金属-氧原子簇合物,最后通过羧基的桥式三齿配位方式将两部分结构连接在一起。经IR, XRD等手段表征,配合物(2)和(3)与配合物(1)有相似的结构方式。
3.以同样的配体在室温下分别与硝酸铕、硝酸铽、硝酸钆合成出配位聚合物(4)-(6)。对其结构的相关性与热稳定性、荧光等性质的研究表明：配合物(4)和(6)具有相似的结构,配合物(5)结构与之不同。三者都有较好的热稳定性,但是荧光性能则差别较大。
Coordination polymers are polymeric, supramolecular assemblies of metalions (or metal clusters) and organic ligands linked through coordination bonds. Because of their novel structures and unique physicochemical properties, coordination polymers have potential applications in molecule identification, catalysis, adsorption, etal. Pyrazine tetracarboxylic acid(PTCA) is a polydentate organic ligand containing N,O atoms, which can coordinate to several metal ions and may exhibit various coordination modes. Thus it is a good candidate for synthesizing novel complexes. Because rare earth elements have many empty orbits, they can react coordinately with organic ligands to get complexes with unique fluorescent and magnetic properties.
In this paper, we used PTCA and rare earth nitrates (dysprosium nitrate, europium nitrate, terbium nitrate, gadolinium nitrate) synthesized a series of coordination polymers through hydrothermal method and solvent evaporation method, and characterized them by single-crystal X-ray diffraction, X-ray diffraction, elemental analysis, infrared spectroscopy, thermogravimetric analysis and fluorescence analysis. The main work is listed as follows:
1. PTCA was synthesized starting from phenazine.
2. Three rare earth complexes(1)- (3)have been synthesized by the solvothermal reactions of PTCA with dysprosium nitrate, terbium nitrate and europium nitrate respectively. Complexes (1) is a three-dimensional coordination polymer. It crystallizes in the triclinic system, space group P-l,with a=9.0069(4) (?), b=10.8801 (2) (?), c=13.246 (?),α=68.725 (8)°,β=77.990 (8)°,γ=88.618(10)°. The Dy(Ⅲ) ions in complexes(1) are nine-coordinated and eight-coordinated. The nine-coordinated Dy(Ⅲ) ion coordinated with PTCA directly while the eight-coordinated ones formed a metal-oxygen atoms cluster with carboxyl, hydroxyl and water. The two parts of the structure are connected by carboxyl's bridge tridentate coordination mode. Complexes (2) and (3) have the similar structure tested by IR, XRD etal.
3. Complexes (4)-(6) have been synthesized with the same ligand and europium nitrate, terbium nitrate and gadolinium nitrate respectively at room temperature. Some related tests result show that structure of complex (4) is similar to that of complex (6) while complex (5) has a different structure than them. Furthermore, all the three complexes have better thermal stability, but the fluorescence properties of the large difference.
1.以吩嗪为原料,合成了吡嗪四羧酸。
2.以吡嗪四羧酸为配体,硝酸镝、硝酸铽、硝酸铕为中心原子,采用水热合成法得到了配位聚合物(1)-(3)。配合物(1)为三斜晶系,P-1空间群的三维结构配位聚合物。其晶胞参数为：a=9.0069(4)A,b=10.8801(2)A,c=13.246 A,α=68.725(8)°,p=77.990(8)°,γ=88.618(10)°。该配合物中,Dy3+有九配位和八配位两种配位方式,其中九配位的Dy3+直接与吡嗪四羧酸配位,八配位的Dy3+则与羧基、羟基和水形成金属-氧原子簇合物,最后通过羧基的桥式三齿配位方式将两部分结构连接在一起。经IR, XRD等手段表征,配合物(2)和(3)与配合物(1)有相似的结构方式。
3.以同样的配体在室温下分别与硝酸铕、硝酸铽、硝酸钆合成出配位聚合物(4)-(6)。对其结构的相关性与热稳定性、荧光等性质的研究表明：配合物(4)和(6)具有相似的结构,配合物(5)结构与之不同。三者都有较好的热稳定性,但是荧光性能则差别较大。
Coordination polymers are polymeric, supramolecular assemblies of metalions (or metal clusters) and organic ligands linked through coordination bonds. Because of their novel structures and unique physicochemical properties, coordination polymers have potential applications in molecule identification, catalysis, adsorption, etal. Pyrazine tetracarboxylic acid(PTCA) is a polydentate organic ligand containing N,O atoms, which can coordinate to several metal ions and may exhibit various coordination modes. Thus it is a good candidate for synthesizing novel complexes. Because rare earth elements have many empty orbits, they can react coordinately with organic ligands to get complexes with unique fluorescent and magnetic properties.
In this paper, we used PTCA and rare earth nitrates (dysprosium nitrate, europium nitrate, terbium nitrate, gadolinium nitrate) synthesized a series of coordination polymers through hydrothermal method and solvent evaporation method, and characterized them by single-crystal X-ray diffraction, X-ray diffraction, elemental analysis, infrared spectroscopy, thermogravimetric analysis and fluorescence analysis. The main work is listed as follows:
1. PTCA was synthesized starting from phenazine.
2. Three rare earth complexes(1)- (3)have been synthesized by the solvothermal reactions of PTCA with dysprosium nitrate, terbium nitrate and europium nitrate respectively. Complexes (1) is a three-dimensional coordination polymer. It crystallizes in the triclinic system, space group P-l,with a=9.0069(4) (?), b=10.8801 (2) (?), c=13.246 (?),α=68.725 (8)°,β=77.990 (8)°,γ=88.618(10)°. The Dy(Ⅲ) ions in complexes(1) are nine-coordinated and eight-coordinated. The nine-coordinated Dy(Ⅲ) ion coordinated with PTCA directly while the eight-coordinated ones formed a metal-oxygen atoms cluster with carboxyl, hydroxyl and water. The two parts of the structure are connected by carboxyl's bridge tridentate coordination mode. Complexes (2) and (3) have the similar structure tested by IR, XRD etal.
3. Complexes (4)-(6) have been synthesized with the same ligand and europium nitrate, terbium nitrate and gadolinium nitrate respectively at room temperature. Some related tests result show that structure of complex (4) is similar to that of complex (6) while complex (5) has a different structure than them. Furthermore, all the three complexes have better thermal stability, but the fluorescence properties of the large difference.
引文
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