A new dinuclear centrosymmetric complex [LaL（HL）（H2O）3]2（2H2O （H2L = 3-nitrophthalic acid, NPA） was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The com...A new dinuclear centrosymmetric complex [LaL（HL）（H2O）3]2（2H2O （H2L = 3-nitrophthalic acid, NPA） was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1^- with a = 8.1549（16）, b = 8.8856（18）, c = 15.277（3）A,α= 100.93（3）,α= 90.81（3）, γ= 104.56（3）°, V = 1049.8（4）A^3, Z = 1,μ= 2.125 mm^-1, Dc=1.994 g/cm^3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates（2-） coordinate with the La3＋ ions in a bridging mode, and two monohydrogen- 3-nitrophthates（1-） and three waters in terminal ways, respectively. Each La^3＋ ion is nine-coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C-H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.展开更多
A 2D coordination polymer, [Co（NPA）（H_2 O）_2]_n（1, H_2 NPA = 3-nitrophthalic acid）, has been synthesized by solvothermal method and characterized by single-crystal X-ray diffraction analysis, FT-IR spectroscopy,...A 2D coordination polymer, [Co（NPA）（H_2 O）_2]_n（1, H_2 NPA = 3-nitrophthalic acid）, has been synthesized by solvothermal method and characterized by single-crystal X-ray diffraction analysis, FT-IR spectroscopy, elemental analysis, thermogravimetric analysis and powder X-ray diffraction. Complex 1 crystallizes in orthorhombic space group Pbca with a = 7.2261（2）, b = 14.6450（5）, c = 19.6671（7） ？, V = 2081.31（11） ？~3, Z = 8, C_8 H_7 CoNO_8, M_r = 304.08, D_c = 1.941 mg/m^3, μ = 1.686 mm^（-1）, S = 1.054, F（000） = 1224, the final R = 0.0248 and wR = 0.0603 for 1834 observed reflections（I 〉 2σ（I））. The crystal structural analysis demonstrates that the Co（Ⅱ） ions in 1 are linked by single and double μ_2-1,3-bridging carboxylate bridges, forming a 2D layer structure. Moreover, magnetic property of 1 was also discussed.展开更多
Two complexes, [Cd（nphth）（2,2＇-bipy）（H20）]2.2H20 （1） and [Cd（nphth）（4,4＇- bipy）（H20）], （2） （nphth = 3-nitrophthalate, 2,2＇-bipy = 2,2＇-bipyridine, 4,4＇-bipy = 4,4＇-bipyridine）, were synthesized...Two complexes, [Cd（nphth）（2,2＇-bipy）（H20）]2.2H20 （1） and [Cd（nphth）（4,4＇- bipy）（H20）], （2） （nphth = 3-nitrophthalate, 2,2＇-bipy = 2,2＇-bipyridine, 4,4＇-bipy = 4,4＇-bipyridine）, were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in triclinic with space group Pi, a = 0.7599（4）, b = 1.0551（6）, c = 1.2448（6） nm, α = 88.96（2）, β = 75.40（2）, γ= 76.76（2）°, V= 0.9393（9） nm3, Z = 1, Dc = 1.816 Mg/m3, F（000） = 512, μ = 1.217 mm-1, S = 0.946, the final R = 0.0238 and wR = 0.0631, Complex 2 crystallizes in monoclinic, space group P21/c, a = 0.737（5）, b = 2.338（1）, c = 1.0030（6） nm, β = 96：359（9）°, V= 1.803（2） nm3, Z = 4, Dc = 1.826 Mg/m3, F （000） = 984,μ = 1.260 mm-1, S = 1.016, the final R = 0.0455 and wR = 0.1007. Complex 1 exhibits a discrete cyclic binuclear structure and complex 2 possesses a 2D layer structure with cyclic binuclear unit. The fluorescent spectrum study shows that complex 1 exhibits fluorescent emission in the solid state at room temperature.展开更多
3-甲基-7-硝基苯酞是嘧啶水杨酸类除草剂环酯草醚的一个重要中间体,以3-硝基邻苯二甲酸、乙酸酐和丙二酸二乙酯为原料,经脱水缩合、Knoevenagel反应、水解脱羧及硼氢化钠还原合成.考察了各步反应溶剂、反应温度、反应时间和原料配比等...3-甲基-7-硝基苯酞是嘧啶水杨酸类除草剂环酯草醚的一个重要中间体,以3-硝基邻苯二甲酸、乙酸酐和丙二酸二乙酯为原料,经脱水缩合、Knoevenagel反应、水解脱羧及硼氢化钠还原合成.考察了各步反应溶剂、反应温度、反应时间和原料配比等因素对反应收率的影响.在最佳优化反应条件下,反应总收率为57.8%,产品质量分数为98.8%,其结构经红外IR和氢谱核磁1 H NMR分析确证.该工艺路线简单、经济、合理并适合于工业化生产.展开更多
基金This work was supported by the Beijing Talent Fund for Young Sci-Tech Researchers (No. H013610050112)
文摘A new dinuclear centrosymmetric complex [LaL（HL）（H2O）3]2（2H2O （H2L = 3-nitrophthalic acid, NPA） was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1^- with a = 8.1549（16）, b = 8.8856（18）, c = 15.277（3）A,α= 100.93（3）,α= 90.81（3）, γ= 104.56（3）°, V = 1049.8（4）A^3, Z = 1,μ= 2.125 mm^-1, Dc=1.994 g/cm^3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates（2-） coordinate with the La3＋ ions in a bridging mode, and two monohydrogen- 3-nitrophthates（1-） and three waters in terminal ways, respectively. Each La^3＋ ion is nine-coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C-H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.
基金supported financially by the Scientific Research Program Funded by Shaanxi Provincial Education Department(No.16JK1598,16JK1612,17JK0606)the Natural Science Foundation of Shaanxi Province(No.2017JQ2009)
文摘A 2D coordination polymer, [Co（NPA）（H_2 O）_2]_n（1, H_2 NPA = 3-nitrophthalic acid）, has been synthesized by solvothermal method and characterized by single-crystal X-ray diffraction analysis, FT-IR spectroscopy, elemental analysis, thermogravimetric analysis and powder X-ray diffraction. Complex 1 crystallizes in orthorhombic space group Pbca with a = 7.2261（2）, b = 14.6450（5）, c = 19.6671（7） ？, V = 2081.31（11） ？~3, Z = 8, C_8 H_7 CoNO_8, M_r = 304.08, D_c = 1.941 mg/m^3, μ = 1.686 mm^（-1）, S = 1.054, F（000） = 1224, the final R = 0.0248 and wR = 0.0603 for 1834 observed reflections（I 〉 2σ（I））. The crystal structural analysis demonstrates that the Co（Ⅱ） ions in 1 are linked by single and double μ_2-1,3-bridging carboxylate bridges, forming a 2D layer structure. Moreover, magnetic property of 1 was also discussed.
基金supported by the National Natural Science Foundation of China(21371088)the Education Department of Fujian Province(No.JK2012048,JA12310,JB12207)
文摘Two complexes, [Cd（nphth）（2,2＇-bipy）（H20）]2.2H20 （1） and [Cd（nphth）（4,4＇- bipy）（H20）], （2） （nphth = 3-nitrophthalate, 2,2＇-bipy = 2,2＇-bipyridine, 4,4＇-bipy = 4,4＇-bipyridine）, were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in triclinic with space group Pi, a = 0.7599（4）, b = 1.0551（6）, c = 1.2448（6） nm, α = 88.96（2）, β = 75.40（2）, γ= 76.76（2）°, V= 0.9393（9） nm3, Z = 1, Dc = 1.816 Mg/m3, F（000） = 512, μ = 1.217 mm-1, S = 0.946, the final R = 0.0238 and wR = 0.0631, Complex 2 crystallizes in monoclinic, space group P21/c, a = 0.737（5）, b = 2.338（1）, c = 1.0030（6） nm, β = 96：359（9）°, V= 1.803（2） nm3, Z = 4, Dc = 1.826 Mg/m3, F （000） = 984,μ = 1.260 mm-1, S = 1.016, the final R = 0.0455 and wR = 0.1007. Complex 1 exhibits a discrete cyclic binuclear structure and complex 2 possesses a 2D layer structure with cyclic binuclear unit. The fluorescent spectrum study shows that complex 1 exhibits fluorescent emission in the solid state at room temperature.
文摘3-甲基-7-硝基苯酞是嘧啶水杨酸类除草剂环酯草醚的一个重要中间体,以3-硝基邻苯二甲酸、乙酸酐和丙二酸二乙酯为原料,经脱水缩合、Knoevenagel反应、水解脱羧及硼氢化钠还原合成.考察了各步反应溶剂、反应温度、反应时间和原料配比等因素对反应收率的影响.在最佳优化反应条件下,反应总收率为57.8%,产品质量分数为98.8%,其结构经红外IR和氢谱核磁1 H NMR分析确证.该工艺路线简单、经济、合理并适合于工业化生产.
