羧酸及多金属氧酸盐超分子化合物的结构及电、光分析
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摘要
本文以羧酸类配体、多金属氧酸盐和过渡金属为原料,采用水热合成的方法合成了一系列的化合物。测定了其结构并对其结构进行了表征。具体结论如下:
(1)在水热条件下合成了金属-有机配位聚合物: [Co(BDC)(phen)- (H2O)]n·3nH2O(H2BDC=terephthalic acid, phen=1,10- phenanthroline),并通过元素分析,IR光谱,TG和单晶X-射线衍射对其进行了表征。结构表明该化合物属于三斜晶系:P-1(2)空间群组;晶胞参数a=9.795(5) A,b=10.752(5) A,c=11.271(5) A,α=75.903(5)o,β=65.306(5) o,γ=86.042(5) o,V=1045.3(9) A3,C_(20)H_(22)CoN_2O_8,Mr =477.13, Dc = 1.908 g/cm~3,μ(MoKα) = 1.637 mm~(-1), F(000) = 620, Z = 2, R1 = 0.1586,wR2 = 0.3906。该化合物表现出Z字连状结构。
(2)以水热合成的方法合成了标题化合物:[C_4H_(12)N_2]_3[PMo_(12)O_(40)]。通过IR,元素分析等方法对化合物进行了表征。晶体解析数据:a=17.8862A, b=17.8862 A, c= 23.543 A,α=90°,β= 90°,γ=120°, V=6522.62 A3, Z=6, R1=0.0384, wR2= 0.1020。该化合物包含keggin结构的PMo12O40阴离子,里面包含了长短交替的Mo-O(Mo)键。在这个晶胞单元里每个Keeggin结构阴离子包含有三个哌嗪。以该化合物为修饰剂的本体修饰碳糊电极(APM-CPE)对抗坏血酸氧化有很好的电催化活性。
(3)在水热条件下,制备了一个新的含有混合配体的配位聚合物:[Mn(2,3-Pydc)2(phen)]n·nH2O (2,3-Pydc= pyridine-2,3-dicarboxylic acid. phen= 1,10-phen anthroline),并且通过元素分析,红外光谱,热重分析,荧光分析和单晶X-衍射对其进行了表征。X射线晶体结构分析表明该化合物属于单斜晶系,MnC_(24)H_(27)N_5O_9,P2(1)/n, a=11.5852(16)A, b=12.0162(17)?,c=13.2157(19)A,α=90.00°,β=108.947(2)°,γ=90.00°。在化合物1中,两个相邻的Mn(II)离子连接两个Phen配体和两个2,3-Pydc配体构成一个双核的[Mn_2(2,3-Pydc)2(phen)]单元,其中Mn-Mn键长为8.226(9) ?。两个相连双核单元通过2,3-pydc配体中3-羰基上的两个O原子进一步连接成网状结构。
In this article, a series of polymers with carboxylic acid and POMs has been hydrothermally synthesized and structurally characterized. The conclusion was arrived as follows:
(1)A metal-organic coordination polymer [Co(phen)(BDC)(H_2O)]n·3nH_2O(H_2BDC= terephthalic acid, phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in triclinic,space group P-1(2) with a=9.795(5) A,b=10.752(5)A, c=11.271(5)A,α=75.903(5)o,β=65.306(5)o,γ=86.042(5)o,V=1045.3(9)A3,C_(20)H_(22)CoN_2O_8,Mr=477.13, Dc = 1.908 g/cm~3,μ(MoKα) =1.637mm~(-1),F(000)=620,Z=2,R1=0.1586,wR2=0.3906. It exhibits a one-dimensional zigzag chain-like structure.
(2)The title compound, [C_4H_(12)N_2]_3[PMo_12O40], was synthesized from the hydrothermal reaction and characterized by IR, elemental analysis and signal crystal x-ray diffraction. Crystal data: a=17.8862A, b=17.8862 A, c= 23.543 A,α=90°,β= 90°,γ=120°, V=6522.62 A3, Z=6, R1=0.0384, wR2= 0.1020.It has a PMo12O40 anion of keggin structure, which contains the strong alternating short (mean 1.875 A) and long (mean 1.926 A) Mo–O(Mo) bonds. In the unit cell, each keggin anion is surrounded by three piperazine. The bulk-modified carbon paste electrode(APM-CPE) using this compound as modifier shows a good electrocatalytic activity toward the oxidation of ascorbic acid(AA) .
(3)Two new coordination polymers with mixed ligands, [M(2,3-Pydc)(phen)]n·nH+2O (M=Mn and Co; 2,3-Pydc= pyridine-2,3- dicarboxylicacid.phen=1,10-phenanthroline) were prepared under hydrothermal conditions and characterized by element alanalyses, IR spectra and single crystal X-ray diffraction analysis.X-ray crystal structural analyses reveal that 1 and 2 are isomorphic and belong to the monoclinic system. MnC_(19)H_(15)N_3O_5,P2(1)/n, a=11.5852(16)A, b=12.0162(17)A, c=13.2157(19)A,α=90.00,β=108.947(2)γ=90.00 for 1;and CoC19H15N3O5, P2(1)/n, a=11.1987(7) A, b=12.121(7) A, c=12.808(7) A,α=90.00,β=110.037(9),γ=90.00 for 2. In the structures of 1 and 2, The two adjacent Mn(II) ions together with two Phen ligands and two 2,3-Pydc ligands construct a dinuclear [Mn2(2,3-Pydc)2(phen)2] subunit with the Mn-Mn distance of 8.226(9) A. Furthermore, two adjacent binuclear subunits are connected by two oxygen atoms of the 3-carboxyl group of 2,3-pydc ligand to form a network structure.
(1)在水热条件下合成了金属-有机配位聚合物: [Co(BDC)(phen)- (H2O)]n·3nH2O(H2BDC=terephthalic acid, phen=1,10- phenanthroline),并通过元素分析,IR光谱,TG和单晶X-射线衍射对其进行了表征。结构表明该化合物属于三斜晶系:P-1(2)空间群组;晶胞参数a=9.795(5) A,b=10.752(5) A,c=11.271(5) A,α=75.903(5)o,β=65.306(5) o,γ=86.042(5) o,V=1045.3(9) A3,C_(20)H_(22)CoN_2O_8,Mr =477.13, Dc = 1.908 g/cm~3,μ(MoKα) = 1.637 mm~(-1), F(000) = 620, Z = 2, R1 = 0.1586,wR2 = 0.3906。该化合物表现出Z字连状结构。
(2)以水热合成的方法合成了标题化合物:[C_4H_(12)N_2]_3[PMo_(12)O_(40)]。通过IR,元素分析等方法对化合物进行了表征。晶体解析数据:a=17.8862A, b=17.8862 A, c= 23.543 A,α=90°,β= 90°,γ=120°, V=6522.62 A3, Z=6, R1=0.0384, wR2= 0.1020。该化合物包含keggin结构的PMo12O40阴离子,里面包含了长短交替的Mo-O(Mo)键。在这个晶胞单元里每个Keeggin结构阴离子包含有三个哌嗪。以该化合物为修饰剂的本体修饰碳糊电极(APM-CPE)对抗坏血酸氧化有很好的电催化活性。
(3)在水热条件下,制备了一个新的含有混合配体的配位聚合物:[Mn(2,3-Pydc)2(phen)]n·nH2O (2,3-Pydc= pyridine-2,3-dicarboxylic acid. phen= 1,10-phen anthroline),并且通过元素分析,红外光谱,热重分析,荧光分析和单晶X-衍射对其进行了表征。X射线晶体结构分析表明该化合物属于单斜晶系,MnC_(24)H_(27)N_5O_9,P2(1)/n, a=11.5852(16)A, b=12.0162(17)?,c=13.2157(19)A,α=90.00°,β=108.947(2)°,γ=90.00°。在化合物1中,两个相邻的Mn(II)离子连接两个Phen配体和两个2,3-Pydc配体构成一个双核的[Mn_2(2,3-Pydc)2(phen)]单元,其中Mn-Mn键长为8.226(9) ?。两个相连双核单元通过2,3-pydc配体中3-羰基上的两个O原子进一步连接成网状结构。
In this article, a series of polymers with carboxylic acid and POMs has been hydrothermally synthesized and structurally characterized. The conclusion was arrived as follows:
(1)A metal-organic coordination polymer [Co(phen)(BDC)(H_2O)]n·3nH_2O(H_2BDC= terephthalic acid, phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in triclinic,space group P-1(2) with a=9.795(5) A,b=10.752(5)A, c=11.271(5)A,α=75.903(5)o,β=65.306(5)o,γ=86.042(5)o,V=1045.3(9)A3,C_(20)H_(22)CoN_2O_8,Mr=477.13, Dc = 1.908 g/cm~3,μ(MoKα) =1.637mm~(-1),F(000)=620,Z=2,R1=0.1586,wR2=0.3906. It exhibits a one-dimensional zigzag chain-like structure.
(2)The title compound, [C_4H_(12)N_2]_3[PMo_12O40], was synthesized from the hydrothermal reaction and characterized by IR, elemental analysis and signal crystal x-ray diffraction. Crystal data: a=17.8862A, b=17.8862 A, c= 23.543 A,α=90°,β= 90°,γ=120°, V=6522.62 A3, Z=6, R1=0.0384, wR2= 0.1020.It has a PMo12O40 anion of keggin structure, which contains the strong alternating short (mean 1.875 A) and long (mean 1.926 A) Mo–O(Mo) bonds. In the unit cell, each keggin anion is surrounded by three piperazine. The bulk-modified carbon paste electrode(APM-CPE) using this compound as modifier shows a good electrocatalytic activity toward the oxidation of ascorbic acid(AA) .
(3)Two new coordination polymers with mixed ligands, [M(2,3-Pydc)(phen)]n·nH+2O (M=Mn and Co; 2,3-Pydc= pyridine-2,3- dicarboxylicacid.phen=1,10-phenanthroline) were prepared under hydrothermal conditions and characterized by element alanalyses, IR spectra and single crystal X-ray diffraction analysis.X-ray crystal structural analyses reveal that 1 and 2 are isomorphic and belong to the monoclinic system. MnC_(19)H_(15)N_3O_5,P2(1)/n, a=11.5852(16)A, b=12.0162(17)A, c=13.2157(19)A,α=90.00,β=108.947(2)γ=90.00 for 1;and CoC19H15N3O5, P2(1)/n, a=11.1987(7) A, b=12.121(7) A, c=12.808(7) A,α=90.00,β=110.037(9),γ=90.00 for 2. In the structures of 1 and 2, The two adjacent Mn(II) ions together with two Phen ligands and two 2,3-Pydc ligands construct a dinuclear [Mn2(2,3-Pydc)2(phen)2] subunit with the Mn-Mn distance of 8.226(9) A. Furthermore, two adjacent binuclear subunits are connected by two oxygen atoms of the 3-carboxyl group of 2,3-pydc ligand to form a network structure.
引文
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