d～（10）金属与芳香二酸、二亚胺混合配体配合物的研究
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摘要
采用水热法，以对苯二甲酸(H_2bdc)、邻苯二甲酸(H_2phth)为第一配体，二齿螯合配体1，10-邻菲哕啉(phen)、2，2′-联吡啶(2，2′-bipy)及桥联配体4，4′-联吡啶(4，4′-bipy)为第二配体，设计合成了6个未见报道的配合物。其中配合物[Zn(2，2′-bipy)(H_2O)(phth)]_2(1)，[Zn(2，2′-bipy)(H_2O)(phth)]_2·2H_2O(2)，[Cd(2，2′-bipy)(H_2O)_2(phth)]_n(3)是邻苯二甲酸与d~(10)金属形成的配合物；配合物[CaZn_4(μ_3-OH)_2(2，2′-bipy)_2(bdc)_4](4)，[CaZn_4(μ_3-OH)_2(phen)_2(bdc)_4](5)，[CaZn_2(4，4′-bipy)(bdc)_3](6)是碱土-过渡金属杂核聚合物。对所分离的配合物，用元素分析和红外光谱进行了表征；用单晶X-射线衍射技术测定了它们的晶体结构；对配合物1，2，4，5，用热分析方法研究了它们的热稳定性，还研究了它们的光发射性质。主要研究结果如下：
1、配合物1，3，4，5，6均属于三斜晶系，P-1空间群，配合物2属于单斜晶系，P2(1)／n空间群。
2、配合物1，2，4，5，6的中心离子Zn(Ⅱ)有四配位四面体构型(1，4，5，6)、五配位变形四方锥构型(4，5)和六配位变形八面体构型(2)；配合物3的中心离子Cd(Ⅱ)是六配位变形八面体构型。配合物中苯二甲酸根的配位方式多种多样，有单齿桥联配位、双齿桥联或螯合、单齿双桥联等配位方式。二酸不同的配位方式影响配合物的结构。配合物1，2通过邻苯二甲酸不同的桥联模式形成双核结构，配合物3通过邻苯二甲酸单单桥联形成1D链状结构，配合物4，5，6是八连接3D结构。
3、配合物热稳定性研究表明，所有配合物都先失去结晶溶剂水分子，再失去CO或CO_2，配位的邻菲啰啉或2，2′-联吡啶的分解温度在140～500℃。配合物1，4在相对较低的温度下发生分解，而且分解也较为彻底。其它配合物相对较为稳定。
4、配合物1，2，4，5固态的光发射性质研究表明，配合物在330～370nm光激发下，均有荧光发射，最大发射光谱分别出现在515nm，550nm，531nm和482nm处。配合物结构和配体的不同，发射光谱的位置和强度不同。结果表明它们是潜在的固体发光材料。
Six compounds (1～6) were synthesized by hydrothermal reaction, using terephthalic acid (H_2bdc), phthalic acid (H_2phth) as the first ligand and the bidentate chelating ligands 1, 10-phenanthroline(phen) or 2, 2'-bipyridine (2, 2'-bipy) and bridging ligand 4, 4'-bipyridine (4, 4'-bipy) as the second ligand. [Zn(2, 2'-bipy)(H_2O)(phth)]_2 (1), [Zn(2,2'-bipy)(H_2O)(phth)]_2·2H_2O (2), [Cd(2, 2'-bipy)(H_2O)_2(phth)]_n (3) are d~(10) metals compounds containing phth ligand. [CaZn_4(μ_3-OH)_2(2,2'-bipy)_2(bdc)_4] (4), [CaZn_4-(μ_3-OH)_2(phen)_2(bdc)_4] (5), [CaZn_2(4, 4'-bipy)(bdc)_3] (6) are alkaline earth-transition heterometal complexes. All the compounds were characterized by the IR and element analyses. The crystal structures of these compounds were determined by X-ray single crystal diffraction method. Futhermore, the thermal stability was analysized by the TG and DSC, and the fluorescent properties were studied for compounds 1, 2,4, 5. The main results are as following:
1. Compounds 1, 3, 4, 5, 6 are crystallized in triclinic crystal system and P-1 space group. Compound 2 is monoclinic crystal system, and P2(1)/n space group.
2. The central metal atom Zn(II) in compounds 1, 2, 4, 5, 6 has a distored tetrahedron(l, 4, 5, 6), distorted square pyramidal(4, 5) and distorted octahedronal(2) coordination geometry, respectively; Cd(II) in 3 is six coordinated and a distorted octahedron coordination geometry. The coordination modes of dicarboxylic acid ligands within these compounds are diverse, including monodentate, bridging bidentate, chelating bidentate, chelating and monodentate double bridging as well. Due to the multi-coordination mode of diacid ligands, the structures of these compounds are different and various. The compounds 1, 2 are binuclear complex through phth different bridge modes. The compounds 3 hold 1D chain through phth monodentate bridging. Compounds 4, 5, 6 have eight-connected 3D network structure.
3. The results of thermal analyses for the compounds show that all compounds lose crystallized H_2O firstly, and then CO or CO_2 were released. The decomposition temperatures of the coordination ligands phen and 2, 2'-bipy range from 140 to 500℃. Compounds 1, 4 begin to decompose more completely at the relatively lower temperatures. The others are more standable relatively.
4. The compounds 1, 2, 4, 5 at the solid state show fluorescent emission bands around 515 nm, 550 nm, 531 nm and 482 nm, resectively, under 330～370 nm light excitation. The intensity and location of emission spectra are influence by the kind of ligand and the structure of compands. The result means that the compounds are potential solid luminescent material.
1、配合物1，3，4，5，6均属于三斜晶系，P-1空间群，配合物2属于单斜晶系，P2(1)／n空间群。
2、配合物1，2，4，5，6的中心离子Zn(Ⅱ)有四配位四面体构型(1，4，5，6)、五配位变形四方锥构型(4，5)和六配位变形八面体构型(2)；配合物3的中心离子Cd(Ⅱ)是六配位变形八面体构型。配合物中苯二甲酸根的配位方式多种多样，有单齿桥联配位、双齿桥联或螯合、单齿双桥联等配位方式。二酸不同的配位方式影响配合物的结构。配合物1，2通过邻苯二甲酸不同的桥联模式形成双核结构，配合物3通过邻苯二甲酸单单桥联形成1D链状结构，配合物4，5，6是八连接3D结构。
3、配合物热稳定性研究表明，所有配合物都先失去结晶溶剂水分子，再失去CO或CO_2，配位的邻菲啰啉或2，2′-联吡啶的分解温度在140～500℃。配合物1，4在相对较低的温度下发生分解，而且分解也较为彻底。其它配合物相对较为稳定。
4、配合物1，2，4，5固态的光发射性质研究表明，配合物在330～370nm光激发下，均有荧光发射，最大发射光谱分别出现在515nm，550nm，531nm和482nm处。配合物结构和配体的不同，发射光谱的位置和强度不同。结果表明它们是潜在的固体发光材料。
Six compounds (1～6) were synthesized by hydrothermal reaction, using terephthalic acid (H_2bdc), phthalic acid (H_2phth) as the first ligand and the bidentate chelating ligands 1, 10-phenanthroline(phen) or 2, 2'-bipyridine (2, 2'-bipy) and bridging ligand 4, 4'-bipyridine (4, 4'-bipy) as the second ligand. [Zn(2, 2'-bipy)(H_2O)(phth)]_2 (1), [Zn(2,2'-bipy)(H_2O)(phth)]_2·2H_2O (2), [Cd(2, 2'-bipy)(H_2O)_2(phth)]_n (3) are d~(10) metals compounds containing phth ligand. [CaZn_4(μ_3-OH)_2(2,2'-bipy)_2(bdc)_4] (4), [CaZn_4-(μ_3-OH)_2(phen)_2(bdc)_4] (5), [CaZn_2(4, 4'-bipy)(bdc)_3] (6) are alkaline earth-transition heterometal complexes. All the compounds were characterized by the IR and element analyses. The crystal structures of these compounds were determined by X-ray single crystal diffraction method. Futhermore, the thermal stability was analysized by the TG and DSC, and the fluorescent properties were studied for compounds 1, 2,4, 5. The main results are as following:
1. Compounds 1, 3, 4, 5, 6 are crystallized in triclinic crystal system and P-1 space group. Compound 2 is monoclinic crystal system, and P2(1)/n space group.
2. The central metal atom Zn(II) in compounds 1, 2, 4, 5, 6 has a distored tetrahedron(l, 4, 5, 6), distorted square pyramidal(4, 5) and distorted octahedronal(2) coordination geometry, respectively; Cd(II) in 3 is six coordinated and a distorted octahedron coordination geometry. The coordination modes of dicarboxylic acid ligands within these compounds are diverse, including monodentate, bridging bidentate, chelating bidentate, chelating and monodentate double bridging as well. Due to the multi-coordination mode of diacid ligands, the structures of these compounds are different and various. The compounds 1, 2 are binuclear complex through phth different bridge modes. The compounds 3 hold 1D chain through phth monodentate bridging. Compounds 4, 5, 6 have eight-connected 3D network structure.
3. The results of thermal analyses for the compounds show that all compounds lose crystallized H_2O firstly, and then CO or CO_2 were released. The decomposition temperatures of the coordination ligands phen and 2, 2'-bipy range from 140 to 500℃. Compounds 1, 4 begin to decompose more completely at the relatively lower temperatures. The others are more standable relatively.
4. The compounds 1, 2, 4, 5 at the solid state show fluorescent emission bands around 515 nm, 550 nm, 531 nm and 482 nm, resectively, under 330～370 nm light excitation. The intensity and location of emission spectra are influence by the kind of ligand and the structure of compands. The result means that the compounds are potential solid luminescent material.
引文
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