含N/O配体配位化合物的合成、结构及性能研究
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摘要
通过配位键、氢键、π-π作用等分子间作用构筑而形成的配位化合物,由于其在光学、磁学、选择性催化、分子识别等方面有着广泛的运用前景,已经成为当今配位化学研究的前沿领域之一。本论文有选择性的挑选了一些含N/O元素的有机配体,运用常规溶液法和水热法与金属盐反应得到[Ni(C_10H_26N_6)][ClO_4]_2 (1),Ni(C_10H_26N_6)(MoO_4)·2H_2O (2),[Mn_2(SO_4)_2(BPIB)_2(H_2O)_2]_n (3),Cu_3(C_6NH_4O_2)_6- (C_3NH_6O)_3 (4), Pb(C_8H_5NO_4) (5)五种结构新颖的配位化合物。对这些化合物都进行了单晶X-射线衍射测试,得出了它们的空间结构,并用红外、热重分析、元素分析、荧光分析等技术手段对其性能进行了表征。
化合物(1)是一种由简单的阳离子[Ni(C_10H_26N_6)](2~)和阴离子[ClO_4]-构成的,可以用作模板剂的大环化合物。我们以此为原料,利用大环化合物中金属剩余的配位点,用水做溶剂,运用常规的溶液法合成出了具有一维链状结构的新化合物Ni(C_10H_26N_6)(MoO_4)·2H_2O (2)。而用于制备化合物(3)的配体1,4-双(邻菲咯琳并[4,5-d]咪唑基)苯(H_2BPIB)具有刚性π-π大共轭体系,它的两边都可以连接金属离子。我们用体积比为2:3的H_2O/DMF做混合溶剂,在水热条件下与MnSO_4·H_2O反应得到了具有ths-b (ThSi2 binary)拓扑结构的三维网状化合物[Mn_2(SO4)(2_) (BPIB)_2(H_2O)2]n (3),并对其荧光性质加以了研究。化合物(4)用烟酸做配体与铜盐反应得到的具有螺旋链的三维结构,且有磁学性质。从这个化合物的制备过程与结构分析,可以看出溶剂对配位化合物的制备和结构起着至关重要的作用。化合物(5)使用具有V形空间结构的刚性5-氨基间苯二甲酸做配体,合成出来具有特殊配位方式的三维超分子化合物,主要通过了氢键、弱的Pb…O键作用、π-π作用等分子间作用力连接二维结构而形成的。并对此化合物的荧光性质进行了初步的研究。
The Coordination Compounds constructing with coordination bonds, hydrogen bonds,π-πinteraction have become the coordination chemistry of one of the active fields,the reason is that some of coordination Compounds with novel structures in the optics, magnetics, selective catalysis, molecular recognition have a wide range of application prospects. In this paper, we have selectively chosen some organic ligands which contains N / O elements reaction with metal salts using conventional solution method and hydrothermal method. Finally, we obtained five novel Coordination Compounds,[Ni(C_10H_26N_6)][ClO_4]2 (1), Ni(C_10H_26N_6)(MoO_4)·2H_2O (2), 2H_2O(3), Cu_3(C_6NH_4O_2)6(C_3NH_6O)_3 (4), Pb(C_8H_5NO_4) (5). These compounds have been conducted on single-crystal X-ray diffraction and characterized by infrared spectra, thermal gravimetric analysis, elemental analysis, fluorescence analysis.
The compound [Ni(C_10H_26N_6)][ClO_4]_2 (1) composed of a simple cation [Ni(C_10H_26N_6)](2~) and a anion [ClO_4]_, which can be used as template. From using the remaining sites of the metal macrocyclic compounds, we used conventional water solution synthesis of Na2MoO_4·2H_2O, obtained a new compound Ni(C_10H_26N_6)_(MoO_4)·2H_2O (2) with one-dimensional chain structure. On the other hand, we used 1,4-Bis([1,10]phenanthroline-[5,6-d]i-midazol-2-yl)benzene(H_2BPIB)with conjugated rigidity system as ligand reaction with MnSO_4·H_2O in the volume ratio of 2:3 H_2O/DMF mixed solvent using the hydrothermal reaction method. The fluorescence of the compound [Mn_2(SO_4)_2(BPIB)_2(H_2O)-2]_n (3) with ths-b (ThSi2 binary) topology of three-dimensional network has been carried out. The compound Cu3(C_6NH_4O_2)6 -(C_3NH_6O)3 (4) was constructed by nicotinic acid and Cooper Chloride, which is a three-dimensional helical chain structure with magnetic characterizations. we selected 5 - amino-isophthalic acid with v-shaped rigid special structure as the organic ligands and received a three-dimensional supramolecular compound Pb(C_8H_5NO_4) (5) with special coordination mode, mainly through the hydrogen bonds, weak Pb...O bonds,π-πinteractions among the two-dimensional structures, and the fluorescence properties of this compound was preliminary studied.
化合物(1)是一种由简单的阳离子[Ni(C_10H_26N_6)](2~)和阴离子[ClO_4]-构成的,可以用作模板剂的大环化合物。我们以此为原料,利用大环化合物中金属剩余的配位点,用水做溶剂,运用常规的溶液法合成出了具有一维链状结构的新化合物Ni(C_10H_26N_6)(MoO_4)·2H_2O (2)。而用于制备化合物(3)的配体1,4-双(邻菲咯琳并[4,5-d]咪唑基)苯(H_2BPIB)具有刚性π-π大共轭体系,它的两边都可以连接金属离子。我们用体积比为2:3的H_2O/DMF做混合溶剂,在水热条件下与MnSO_4·H_2O反应得到了具有ths-b (ThSi2 binary)拓扑结构的三维网状化合物[Mn_2(SO4)(2_) (BPIB)_2(H_2O)2]n (3),并对其荧光性质加以了研究。化合物(4)用烟酸做配体与铜盐反应得到的具有螺旋链的三维结构,且有磁学性质。从这个化合物的制备过程与结构分析,可以看出溶剂对配位化合物的制备和结构起着至关重要的作用。化合物(5)使用具有V形空间结构的刚性5-氨基间苯二甲酸做配体,合成出来具有特殊配位方式的三维超分子化合物,主要通过了氢键、弱的Pb…O键作用、π-π作用等分子间作用力连接二维结构而形成的。并对此化合物的荧光性质进行了初步的研究。
The Coordination Compounds constructing with coordination bonds, hydrogen bonds,π-πinteraction have become the coordination chemistry of one of the active fields,the reason is that some of coordination Compounds with novel structures in the optics, magnetics, selective catalysis, molecular recognition have a wide range of application prospects. In this paper, we have selectively chosen some organic ligands which contains N / O elements reaction with metal salts using conventional solution method and hydrothermal method. Finally, we obtained five novel Coordination Compounds,[Ni(C_10H_26N_6)][ClO_4]2 (1), Ni(C_10H_26N_6)(MoO_4)·2H_2O (2), 2H_2O(3), Cu_3(C_6NH_4O_2)6(C_3NH_6O)_3 (4), Pb(C_8H_5NO_4) (5). These compounds have been conducted on single-crystal X-ray diffraction and characterized by infrared spectra, thermal gravimetric analysis, elemental analysis, fluorescence analysis.
The compound [Ni(C_10H_26N_6)][ClO_4]_2 (1) composed of a simple cation [Ni(C_10H_26N_6)](2~) and a anion [ClO_4]_, which can be used as template. From using the remaining sites of the metal macrocyclic compounds, we used conventional water solution synthesis of Na2MoO_4·2H_2O, obtained a new compound Ni(C_10H_26N_6)_(MoO_4)·2H_2O (2) with one-dimensional chain structure. On the other hand, we used 1,4-Bis([1,10]phenanthroline-[5,6-d]i-midazol-2-yl)benzene(H_2BPIB)with conjugated rigidity system as ligand reaction with MnSO_4·H_2O in the volume ratio of 2:3 H_2O/DMF mixed solvent using the hydrothermal reaction method. The fluorescence of the compound [Mn_2(SO_4)_2(BPIB)_2(H_2O)-2]_n (3) with ths-b (ThSi2 binary) topology of three-dimensional network has been carried out. The compound Cu3(C_6NH_4O_2)6 -(C_3NH_6O)3 (4) was constructed by nicotinic acid and Cooper Chloride, which is a three-dimensional helical chain structure with magnetic characterizations. we selected 5 - amino-isophthalic acid with v-shaped rigid special structure as the organic ligands and received a three-dimensional supramolecular compound Pb(C_8H_5NO_4) (5) with special coordination mode, mainly through the hydrogen bonds, weak Pb...O bonds,π-πinteractions among the two-dimensional structures, and the fluorescence properties of this compound was preliminary studied.
引文
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