基于对称席夫碱配体的配位聚合物的合成、晶体结构与性质研究
摘要
配位聚合物既具有新奇的拓扑结构,又具有丰富的光电磁性质,在气体的储存与分离、磁性材料、光学材料、催化剂及催化剂载体等领域具有广泛的应用前景,因此,近年来配位聚合物的设计合成与性质研究已经成为配位化学、材料化学等学科关注的热点课题之一。相比与柔性连接的配体,配位单元之间的刚性连接变形性小,金属导致的配位过程对刚性连接之间的距离与角度影响小,因此,采用刚性配体构筑配位聚合物时配体本身具有较少的不确定因素,从而更有利于增强对目标产物的结构预测性,有利于实现特定配位聚合物的结构调控,是实现“目标分子自组装”的一个重要途经。本文选择了乙酰吡嗪双缩水合肼(L~1)和4-乙酰吡啶双缩水合肼(L~2)两个刚性的对称席夫碱配体,与金属自组装构筑配位聚合物,主要通过调节抗衡离子的种类与配位能力调控产物结构,引入了硫氰酸根离子、硝酸根、氯离子、碘离子,并扩展到具有较大体积、较高电荷数的多酸阴离子,分别获得了具有一维链状、二维层状及三维网状结构的10个配位聚合物,测定了所有配合物的晶体结构,并测定了产物在室温下的固体荧光光谱。主要内容如下:
(1)利用乙酰吡嗪双缩水合肼配体(L~1)分别与AgNO_3、AgNO_3和KSCN、Cd(NO_3)_2·4H_2O和KSCN、Cd(NO_3)_2·4H_2O和KI在室温下自组装,得到了三维网状的配位聚合物{[Ag_2L~1(NO_3)_2]·H_2O}_n (1)和[Ag(L~1)0.5(SCN)]_n (2) ,二维层状配位聚合物[CdL~1(SCN)_2]_n (3)和[CdL~1I_2]_n (4)。
(2)利用4-乙酰吡啶双缩水合肼配体(L~2),分别与Cu(NO_3)_2和KSCN、Cu(NO_3)_2、AgNO_3、ZnCL~2自组装,得到了三维配位聚合物[Cu(L~2)_(0.5)(SCN)]_n (5)、二维配位聚合物{[Cu(L~2)_2(NO_3)_2]·3H_2O}_n (6)、一维配位聚合物{[AgL~2H_2O][AgL~2NO_3](NO_3)(L~2)_(0.5)(H_2O)}_n (7)和[ZnL~2CL~2]_n (8)。
(3)利用4-乙酰吡啶双缩水合肼配体(L~2),室温下分别与Cu(NO_3)_2和H3PW_(12)O_(40)·nH_2O、AgNO_3和H3PMo_(12)O_(40)·nH_2O自组装,得到了两个含有孔洞的多酸基一维配位聚合物{[CuL~2(DMF)3]2 (PW_(12)O_(40))}_n[CuL~2(DMF)_4]_n·nPW_(12)O_(40)·nDMF (9)和{[AgL~2(DMF)]2(PMo_(12)O_(40))]}_n[AgL~2]_n·4nH_2O (10)。
The construction of coordination polymers via self-assembly of predesigned ligands with appropriate metal ions is a subject of current interest. These solid materials are attractive to chemists not only for the variety of topologies and intriguing frameworks, but also for their potential applications in catalysis, photochemistry, electrochromism, sorption, biology and medicine.
The organic ligands containing nitrogen heterocyclic rings, such as pyridine and pyrazine, are excellent ligands and their coordination to metals leads to a variety of coordination complexes. Compared with the flexible ligands, the rigid ligands are particularly attractive for making expectant coordination polymer structures. Herein the chosen ligands, L~1 [bis(1-pyrazinylethylidene)hydrazine] and L~2 [(bis-(1-pyridin-4-yl-ethylidene)-hydrazine)], are easy-to-prepare and the two ligands are one of the shortest imine-based ligand systems. L~1 and L~2 are suitable to assemble different anion dependent coordination polymers with transition-metal ions. As part of our studies on the construction of metal-Schiff base species and POM-based compounds, in this paper we report the synthesis and characterization of ten interesting coordination polymers, including four 1D crystalline arrays, three 2D sheets and three 3D networks. The luminescent properties of L~1, L~2 and 1-10 in the solid were investigated.
(1) Two 3D coordination polymers {[Ag_2L~1(NO_3)_2]·H_2O}_n (1), [Ag(L~1)0.5(SCN)]_n (2) and two 2D coordination polymers [L~1Cd(SCN)_2]_n (3), [L~1CdI_2]_n (4) have been synthesized and structurally characterized using ligand L~1.
(2) One 3D coordination polymer {[CuL~2(SCN)_2]CH3CN}_n (5),one 2D coordination polymer [CuL~22 (NO_3)_2·3H_2O]_n (6) and two 1D chains {[AgL~2][AgL~2NO_3](NO_3)(L~2)_(0.5)(H_2O)_2}_n (7) and [ZnL~2CL~2]_n (8) have been synthesized and structurally characterized using ligand L~2.
(3) Two 1D coordination polymers {[CuL~2(DMF)3]2 (PW_(12)O_(40))}_n[CuL~2(DMF)_4]_n·nPW_(12)O_(40)·nDMF (9) and {[AgL~2(DMF)]2(PMo_(12)O_(40))]}_n[AgL~2]_n·4nH_2O (10) have been synthesized and structurally characterized using ligand L~2 and saturated Keggin type polyoxoanions.
(1)利用乙酰吡嗪双缩水合肼配体(L~1)分别与AgNO_3、AgNO_3和KSCN、Cd(NO_3)_2·4H_2O和KSCN、Cd(NO_3)_2·4H_2O和KI在室温下自组装,得到了三维网状的配位聚合物{[Ag_2L~1(NO_3)_2]·H_2O}_n (1)和[Ag(L~1)0.5(SCN)]_n (2) ,二维层状配位聚合物[CdL~1(SCN)_2]_n (3)和[CdL~1I_2]_n (4)。
(2)利用4-乙酰吡啶双缩水合肼配体(L~2),分别与Cu(NO_3)_2和KSCN、Cu(NO_3)_2、AgNO_3、ZnCL~2自组装,得到了三维配位聚合物[Cu(L~2)_(0.5)(SCN)]_n (5)、二维配位聚合物{[Cu(L~2)_2(NO_3)_2]·3H_2O}_n (6)、一维配位聚合物{[AgL~2H_2O][AgL~2NO_3](NO_3)(L~2)_(0.5)(H_2O)}_n (7)和[ZnL~2CL~2]_n (8)。
(3)利用4-乙酰吡啶双缩水合肼配体(L~2),室温下分别与Cu(NO_3)_2和H3PW_(12)O_(40)·nH_2O、AgNO_3和H3PMo_(12)O_(40)·nH_2O自组装,得到了两个含有孔洞的多酸基一维配位聚合物{[CuL~2(DMF)3]2 (PW_(12)O_(40))}_n[CuL~2(DMF)_4]_n·nPW_(12)O_(40)·nDMF (9)和{[AgL~2(DMF)]2(PMo_(12)O_(40))]}_n[AgL~2]_n·4nH_2O (10)。
The construction of coordination polymers via self-assembly of predesigned ligands with appropriate metal ions is a subject of current interest. These solid materials are attractive to chemists not only for the variety of topologies and intriguing frameworks, but also for their potential applications in catalysis, photochemistry, electrochromism, sorption, biology and medicine.
The organic ligands containing nitrogen heterocyclic rings, such as pyridine and pyrazine, are excellent ligands and their coordination to metals leads to a variety of coordination complexes. Compared with the flexible ligands, the rigid ligands are particularly attractive for making expectant coordination polymer structures. Herein the chosen ligands, L~1 [bis(1-pyrazinylethylidene)hydrazine] and L~2 [(bis-(1-pyridin-4-yl-ethylidene)-hydrazine)], are easy-to-prepare and the two ligands are one of the shortest imine-based ligand systems. L~1 and L~2 are suitable to assemble different anion dependent coordination polymers with transition-metal ions. As part of our studies on the construction of metal-Schiff base species and POM-based compounds, in this paper we report the synthesis and characterization of ten interesting coordination polymers, including four 1D crystalline arrays, three 2D sheets and three 3D networks. The luminescent properties of L~1, L~2 and 1-10 in the solid were investigated.
(1) Two 3D coordination polymers {[Ag_2L~1(NO_3)_2]·H_2O}_n (1), [Ag(L~1)0.5(SCN)]_n (2) and two 2D coordination polymers [L~1Cd(SCN)_2]_n (3), [L~1CdI_2]_n (4) have been synthesized and structurally characterized using ligand L~1.
(2) One 3D coordination polymer {[CuL~2(SCN)_2]CH3CN}_n (5),one 2D coordination polymer [CuL~22 (NO_3)_2·3H_2O]_n (6) and two 1D chains {[AgL~2][AgL~2NO_3](NO_3)(L~2)_(0.5)(H_2O)_2}_n (7) and [ZnL~2CL~2]_n (8) have been synthesized and structurally characterized using ligand L~2.
(3) Two 1D coordination polymers {[CuL~2(DMF)3]2 (PW_(12)O_(40))}_n[CuL~2(DMF)_4]_n·nPW_(12)O_(40)·nDMF (9) and {[AgL~2(DMF)]2(PMo_(12)O_(40))]}_n[AgL~2]_n·4nH_2O (10) have been synthesized and structurally characterized using ligand L~2 and saturated Keggin type polyoxoanions.
引文
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