Two complexes CuLCl（H2O） 1 and Ni（L）2 2 （HL = 2-carboxy-1,10-phenanthroline） have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n...Two complexes CuLCl（H2O） 1 and Ni（L）2 2 （HL = 2-carboxy-1,10-phenanthroline） have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n with a = 7.985（2）, b = 16.067（3）, c = 9.694（2） A, β = 98.189（30）°, V= 1231.0（4） A^3, Z = 4, Dc = 1.836 g/cm^3,μ =1.998 mm^-1, F（000） = 684, the final R = 0.0301 and wR = 0.0810. The structure of 2 （C26H14N4NiO10） adopts an orthorhombic system, space group Pbea with a = 9.410（2）, b = 23.2410（5）, c = 23.8680（5） A, V = 5219.9（18） A^3, Z = 8, Mr = 601.12, Dc = 1,530 g/cm^3,μ = 0.809 mm^-1, F（000） = 2448, the final R = 0.0448 and wR = 0.1427. The Cu center of complex 1 exhibits a square pyramidal coordination environment with one oxygen and two nitrogen atoms from deprotonated 2-carboxy-1,10-phenanthroline, one oxygen atom from water and one chloride ion. The Ni center of complex 2 assumes a distorted octahedral coordination geometry consisting of two oxygen atoms and four nitrogen atoms of two deprotonated 2-carboxy-1,10-phenanthroline molecules. Supramolecular assembly has been found via noncovalent bonds, such as hydrogen bonds and π-π stacking interactions.展开更多
A new ID coordination polymer, [Cda（L1）2（L2）2].H2O （1, H2L1 = 4-（carboxy- methoxy）benzoic acid and L2 = 2-（4-fluorophenyl）-I H-imidazo[4,5-f][1,10]phenanthroline）, has been hydrothermally synthesized and cha...A new ID coordination polymer, [Cda（L1）2（L2）2].H2O （1, H2L1 = 4-（carboxy- methoxy）benzoic acid and L2 = 2-（4-fluorophenyl）-I H-imidazo[4,5-f][1,10]phenanthroline）, has been hydrothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.985（5）, b = 10.768（5）, c = 12.512（5） A, a = 68.959（5）, β = 80.354（5）, γ = 79.663（5）°, V= 1227.4（10） A3, Z = 1, C56H36Cd2F2N8O11, Mr = 1259.73, Dc = 1.704 g/cm3, F（000） = 630, μ（MoKa） = 0.949 mm-1, R = 0.0261 and wR = 0.0655. The L1 anions link the neighboring Cd（II） atoms to form a 1D double chain structure. The L2 ligands are alternately located on both sides of the double chains. More interestingly, the lateral L2 ligands from adjacent double chains are paired to furnish strong π-π interactions, yielding a 2D supramolecular layer. N-H...O, O-H...N and O-H...O hydrogen bonds further stabilize the structure of 1. The luminescent property of 1 was studied in solid state at room temperature.展开更多
An unusual two-dimensional supramolecular complex, namely, [Cd2（Cl）4（L）2]（1）, has been synthesized by 2-（1 H-imidazo[4,5-f][1,10]phenanthrolin-2-yl）phenol（L） and CdCl2·2.5H2O under hydrothermal conditio...An unusual two-dimensional supramolecular complex, namely, [Cd2（Cl）4（L）2]（1）, has been synthesized by 2-（1 H-imidazo[4,5-f][1,10]phenanthrolin-2-yl）phenol（L） and CdCl2·2.5H2O under hydrothermal conditions. The compound was characterized by elemental analysis, TG and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 10.151（2）, b = 14.119（3）, c = 14.744（3） ？, α = 115.744（4）, β = 108.063（4）, γ = 93.371（4）o, V = 1762.7（7） A°^3, Z = 2, C（38）H（24）Cd2Cl4N8O2, Mr = 991.25, Dc = 1.868 g/cm^3, F（000） = 976, μ（Mo Ka） = 1.560 mm^-1, R = 0.0639 and w R = 0.1307. In 1, two Cd（II） atoms are bridged by two chroline atoms to give a dimer. Neighboring dimers are linked by N–H···Cl hydrogen bonds to afford supramolecular chains, which are further joined together by π-π interactions to result in a supramolecular layer. In addition, luminescent property and thermal behavior of compound 1 have been studied.展开更多
In this work, a new Cd（Ⅱ） dimeric compound, [Cd（Cl）2（L）（H2O）]2 （1, L = 2-（4- fluorophenyl）-lH-imidazo[4,5-f][1,10]phenanthroline）, has been achieved under hydrothermal conditions. The structure of compoun...In this work, a new Cd（Ⅱ） dimeric compound, [Cd（Cl）2（L）（H2O）]2 （1, L = 2-（4- fluorophenyl）-lH-imidazo[4,5-f][1,10]phenanthroline）, has been achieved under hydrothermal conditions. The structure of compound 1 was determined by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 8.944（2）, b = 18.781（5）, c = 10.904（3） A, β = 91.392（4）°, V = 1831.2（8） A^3, Z = 2, C3sH26Cd2F2C14Cl4N8O2, Mr = 1031.27, Dc = 1.870 g/cm3, F（000） = 1016, μ（MoKα） = 1.513 mm^-1, R = 0.0532 and wR = 0.1407. Each Cd（ll） atom is in an octahedral coordination sphere, completed by two nitrogen atoms from one L ligand, two chlorine anions, and one water oxygen atom. Two chlorine anions bridge two Cd（Ⅱ） atoms to give a dimer [Cd（Cl）2（L）（H2O）]2. Adjacent dimers are stacked by one type of π…π interactions among L ligands to generate a 1D supramolecular chain. Further, the 1D supramolecular chains are stacked by another type of π…π interactions among L ligands to give a 2D supramolecular layer. Finally, the luminescent property of 1 has been studied in solid state at room temperature.展开更多
A novel ligand N - ethyl - 1,10 - phenanthroline - 2 - methanamine and its Ni(Ⅱ)complex have been synthesized.The crystal structure of the complex has been determined by X - ray diffraction method.The Ni(Ⅱ)is five -...A novel ligand N - ethyl - 1,10 - phenanthroline - 2 - methanamine and its Ni(Ⅱ)complex have been synthesized.The crystal structure of the complex has been determined by X - ray diffraction method.The Ni(Ⅱ)is five - coordi - nated by three nitrogen atoms from the ligand and two Cl - anions in a distorted trigonal bipyramidal environment:the N(2),Cl(1)and Cl(2)in equatorial plane;the N(1)and N(3)in axial positions.The UV - spectra and IR - spectra of the ligand and its Ni(Ⅱ)complex were recorded and discussed.The thermodynamic properties of the ligand with various bivalent metals were studied by potentiometric titrations and the order of the stability constants is in a - greement with the Irving - Williams order in coordination chemistry.CCDC:221750.展开更多
以1,10-菲咯啉-5,6-二酮为原料,合成了标题化合物。通过质谱、1H N M R对其进行了表征。X-射线单晶衍射测试进一步确定了化合物的结构,结果表明：化合物为单斜晶系,空间群P 21/n,晶胞参数：a=1.1492（5）nm,b=1.2622（6）nm,c=1.2506（5...以1,10-菲咯啉-5,6-二酮为原料,合成了标题化合物。通过质谱、1H N M R对其进行了表征。X-射线单晶衍射测试进一步确定了化合物的结构,结果表明：化合物为单斜晶系,空间群P 21/n,晶胞参数：a=1.1492（5）nm,b=1.2622（6）nm,c=1.2506（5）nm,α=90.00°,β=100.354（12）°,γ=90.00°,V=1.784nm 3,Z=4,D c=1.274m-3,μ=0.082m m-1,最终偏离因子：R=0.0467,w R=0.1386。展开更多
研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,...研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,溶剂DMF用量为15 m L,反应时间为8 h;氨基化反应的优化反应条件:投料质量比为1:6,反应温度为180℃、时间为2.0 h。该工艺具有原料易得、工艺简单、环境友好等特点,为2-氨基-1,10-邻菲罗啉的合成提供了一条简便的合成路线。展开更多
基金This work was supported by the National Natural Science Foundation of China (No. 20671055)the Ministry of Science and Technology,China through 973-Project (No. 2002CB613301)
文摘Two complexes CuLCl（H2O） 1 and Ni（L）2 2 （HL = 2-carboxy-1,10-phenanthroline） have been synthesized and characterized by single-crystal X-ray crystallography. The structure of 1 has a monoclinic space group P21/n with a = 7.985（2）, b = 16.067（3）, c = 9.694（2） A, β = 98.189（30）°, V= 1231.0（4） A^3, Z = 4, Dc = 1.836 g/cm^3,μ =1.998 mm^-1, F（000） = 684, the final R = 0.0301 and wR = 0.0810. The structure of 2 （C26H14N4NiO10） adopts an orthorhombic system, space group Pbea with a = 9.410（2）, b = 23.2410（5）, c = 23.8680（5） A, V = 5219.9（18） A^3, Z = 8, Mr = 601.12, Dc = 1,530 g/cm^3,μ = 0.809 mm^-1, F（000） = 2448, the final R = 0.0448 and wR = 0.1427. The Cu center of complex 1 exhibits a square pyramidal coordination environment with one oxygen and two nitrogen atoms from deprotonated 2-carboxy-1,10-phenanthroline, one oxygen atom from water and one chloride ion. The Ni center of complex 2 assumes a distorted octahedral coordination geometry consisting of two oxygen atoms and four nitrogen atoms of two deprotonated 2-carboxy-1,10-phenanthroline molecules. Supramolecular assembly has been found via noncovalent bonds, such as hydrogen bonds and π-π stacking interactions.
基金Supported by Jilin Province Science and Technology Development projects (No. 201105085)
文摘A new ID coordination polymer, [Cda（L1）2（L2）2].H2O （1, H2L1 = 4-（carboxy- methoxy）benzoic acid and L2 = 2-（4-fluorophenyl）-I H-imidazo[4,5-f][1,10]phenanthroline）, has been hydrothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.985（5）, b = 10.768（5）, c = 12.512（5） A, a = 68.959（5）, β = 80.354（5）, γ = 79.663（5）°, V= 1227.4（10） A3, Z = 1, C56H36Cd2F2N8O11, Mr = 1259.73, Dc = 1.704 g/cm3, F（000） = 630, μ（MoKa） = 0.949 mm-1, R = 0.0261 and wR = 0.0655. The L1 anions link the neighboring Cd（II） atoms to form a 1D double chain structure. The L2 ligands are alternately located on both sides of the double chains. More interestingly, the lateral L2 ligands from adjacent double chains are paired to furnish strong π-π interactions, yielding a 2D supramolecular layer. N-H...O, O-H...N and O-H...O hydrogen bonds further stabilize the structure of 1. The luminescent property of 1 was studied in solid state at room temperature.
基金Supported by the National Natural Science Foundation of China(No.21607051)
文摘An unusual two-dimensional supramolecular complex, namely, [Cd2（Cl）4（L）2]（1）, has been synthesized by 2-（1 H-imidazo[4,5-f][1,10]phenanthrolin-2-yl）phenol（L） and CdCl2·2.5H2O under hydrothermal conditions. The compound was characterized by elemental analysis, TG and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 10.151（2）, b = 14.119（3）, c = 14.744（3） ？, α = 115.744（4）, β = 108.063（4）, γ = 93.371（4）o, V = 1762.7（7） A°^3, Z = 2, C（38）H（24）Cd2Cl4N8O2, Mr = 991.25, Dc = 1.868 g/cm^3, F（000） = 976, μ（Mo Ka） = 1.560 mm^-1, R = 0.0639 and w R = 0.1307. In 1, two Cd（II） atoms are bridged by two chroline atoms to give a dimer. Neighboring dimers are linked by N–H···Cl hydrogen bonds to afford supramolecular chains, which are further joined together by π-π interactions to result in a supramolecular layer. In addition, luminescent property and thermal behavior of compound 1 have been studied.
基金Supported by the Science and Technology Research Projects of the Education Committee of Jilin Province(No.2013206)
文摘In this work, a new Cd（Ⅱ） dimeric compound, [Cd（Cl）2（L）（H2O）]2 （1, L = 2-（4- fluorophenyl）-lH-imidazo[4,5-f][1,10]phenanthroline）, has been achieved under hydrothermal conditions. The structure of compound 1 was determined by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 8.944（2）, b = 18.781（5）, c = 10.904（3） A, β = 91.392（4）°, V = 1831.2（8） A^3, Z = 2, C3sH26Cd2F2C14Cl4N8O2, Mr = 1031.27, Dc = 1.870 g/cm3, F（000） = 1016, μ（MoKα） = 1.513 mm^-1, R = 0.0532 and wR = 0.1407. Each Cd（ll） atom is in an octahedral coordination sphere, completed by two nitrogen atoms from one L ligand, two chlorine anions, and one water oxygen atom. Two chlorine anions bridge two Cd（Ⅱ） atoms to give a dimer [Cd（Cl）2（L）（H2O）]2. Adjacent dimers are stacked by one type of π…π interactions among L ligands to generate a 1D supramolecular chain. Further, the 1D supramolecular chains are stacked by another type of π…π interactions among L ligands to give a 2D supramolecular layer. Finally, the luminescent property of 1 has been studied in solid state at room temperature.
文摘A novel ligand N - ethyl - 1,10 - phenanthroline - 2 - methanamine and its Ni(Ⅱ)complex have been synthesized.The crystal structure of the complex has been determined by X - ray diffraction method.The Ni(Ⅱ)is five - coordi - nated by three nitrogen atoms from the ligand and two Cl - anions in a distorted trigonal bipyramidal environment:the N(2),Cl(1)and Cl(2)in equatorial plane;the N(1)and N(3)in axial positions.The UV - spectra and IR - spectra of the ligand and its Ni(Ⅱ)complex were recorded and discussed.The thermodynamic properties of the ligand with various bivalent metals were studied by potentiometric titrations and the order of the stability constants is in a - greement with the Irving - Williams order in coordination chemistry.CCDC:221750.
文摘以1,10-菲咯啉-5,6-二酮为原料,合成了标题化合物。通过质谱、1H N M R对其进行了表征。X-射线单晶衍射测试进一步确定了化合物的结构,结果表明：化合物为单斜晶系,空间群P 21/n,晶胞参数：a=1.1492（5）nm,b=1.2622（6）nm,c=1.2506（5）nm,α=90.00°,β=100.354（12）°,γ=90.00°,V=1.784nm 3,Z=4,D c=1.274m-3,μ=0.082m m-1,最终偏离因子：R=0.0467,w R=0.1386。
文摘研究了以1,10-邻菲罗啉为原料,经氧化和氯代反应合成2-氯-1,10-邻菲罗啉,再经氨基化反应得到目标产物2-氨基-1,10-邻菲罗啉,化合物结构经核磁共振仪、红外分光光度计和质谱仪确认。结果表明,氯代反应的优化反应条件:投料比为1 g:2 m L,溶剂DMF用量为15 m L,反应时间为8 h;氨基化反应的优化反应条件:投料质量比为1:6,反应温度为180℃、时间为2.0 h。该工艺具有原料易得、工艺简单、环境友好等特点,为2-氨基-1,10-邻菲罗啉的合成提供了一条简便的合成路线。
