设计并合成能用于识别铜离子的荧光探针N′-(喹啉-2-亚甲基)-7-二乙胺基-3-甲酰肼-香豆素(FKBA),通过质谱、红外光谱、元素分析、~1 H NMR、^(13) C NMR等方法对该荧光探针FKBA进行表征;采用荧光光谱法和紫外-可见光谱法对FKBA与金属离...设计并合成能用于识别铜离子的荧光探针N′-(喹啉-2-亚甲基)-7-二乙胺基-3-甲酰肼-香豆素(FKBA),通过质谱、红外光谱、元素分析、~1 H NMR、^(13) C NMR等方法对该荧光探针FKBA进行表征;采用荧光光谱法和紫外-可见光谱法对FKBA与金属离子的相互作用进行了研究。结果表明FKBA对Cu^(2+)有良好的选择性和灵敏度。向含有FKBA的溶液中加入Cu^(2+),其吸收峰发生红移,且强度增大。而向该溶液中,加入Al ^(3+),Ag^+,Ba^(2+),Cd^(2+),Ca^(2+),Co^(3+),Fe^(3+),Cr^(3+),Hg^(2+),Mg^(2+),K^+,Mn^(2+),Ni ^(2+),Na^+,Zn^(2+)和Pb^(2+)等其他16种金属离子时,FKBA的紫外吸收仅发生细微的变化。FKBA作为化学传感器对Cu^(2+)的选择性是通过与一系列与环保和生物功能相关的金属离子相互作用得到验证。FKBA中加入Cu^(2+)时,FKBA的荧光强度明显猝灭,其他16种金属离子对FKBA的荧光强度几乎没有影响。不同的金属离子分别与Cu^(2+)共存时FKBA的荧光光谱猝灭程度相同,说明FKBA具有良好的抗干扰能力。向FKBA中加入EDTA,FKBA的荧光强度得到恢复。FKBA中加入Cu^(2+),溶液颜色变成棕色,加入EDTA后又恢复到初始颜色。说明FKBA的荧光减弱不是Cu^(2+)催化FKBA分解而是FKBA与Cu^(2+)络合。在酸性环境中,FKBA的希夫碱结构不稳定,部分FKBA分解成其他的荧光物质。据IUPAC(cDL=3Sb/m)测得检测限为0.13μmol·L^(-1)。对实际样品中的Cu^(2+)浓度进行分析,表明FKBA可作为荧光传感器用于实际样品的Cu^(2+)检测。展开更多
Co-crystallization of pztcH_4 with 4,4＇-bipyridine（4,4＇-bipy） in pH = 3-4 and 1-2 gave two new binary molecular adducts： [（4,4＇-bipy H2）（pztc H2）]（1） and [（4,4＇-bipy H2）（pztcH3）（Cl）]·4H2O（2）,...Co-crystallization of pztcH_4 with 4,4＇-bipyridine（4,4＇-bipy） in pH = 3-4 and 1-2 gave two new binary molecular adducts： [（4,4＇-bipy H2）（pztc H2）]（1） and [（4,4＇-bipy H2）（pztcH3）（Cl）]·4H2O（2）, respectively. Compounds 1 and 2 have been characterized by IR, elemental analysis, NMR and X-ray single-crystal diffraction. Compound 1 crystallizes in triclinic, space group P1 with a = 5.7752（12）, b = 7.9126（16）, c = 9.4492（19） ？, α = 97.49（3）, β = 107.71（3）, γ = 94.52（3）o, V = 404.62（14） A^3, Z = 1, μ = 0.137 mm^1, Dc = 1.692 Mg/m^3, C18H12N4O8, Mr = 412.32, F（000） = 212, S = 1.025, R = 0.0360 and wR = 0.0973. Compound 2 crystallizes in monoclinic, space group C2/c with a = 17.093（3）, b = 7.7665（16）, c = 18.414（4） A, β = 113.36（3）o, V = 2244.1（8） A^3, Z = 4, μ = 0.244 mm^-1, Dc = 1.542 Mg/m^3, C18H21ClN4O12, Mr = 520.84, F（000） = 1080, S = 1.021, R = 0.0343 and wR = 0.0978. In compound 1, pztc H22- anions self-formed 2-D sheets by strong Oacid-H···Oacidhydrogen bonds, which are further extended to form a 3-D supramolecular network bridged with 4,4？-bipy via N-H···Oacid interactions. In compound 2, besides the 1-D chain constructed by pztc H3-itself through strong H-bond Oacid-H···Oacid, the other chain is constructed with 4,4？-bipy H22＋, Cl-anion and water molecules by moderate H-bonds and Ow-H···Cl and N-H···Ow. The two chains are linked with μ3-connected water molecules resulting from the combination of strong synthon-assisted H-bonding Oacid-H···Ow to afford an interlaced 3-D network.展开更多
Reactions of piperidine derivatives 4-(aminomethyl)piperidine(4-AMPD) and 1-methylpiperidin-4-amine(1-MPDA) with semi-conductive metal iodine SbI3 and PbI2 in concentrated HI aqueous solution afforded two one-dimensio...Reactions of piperidine derivatives 4-(aminomethyl)piperidine(4-AMPD) and 1-methylpiperidin-4-amine(1-MPDA) with semi-conductive metal iodine SbI3 and PbI2 in concentrated HI aqueous solution afforded two one-dimensional(1 D) chain compounds [(4-AMPD)SbI5]n(1), [(1-MPDA)SbI5]n(2) and a two-dimensional(2 D) single layered organicinorganic hybrid material [(1-MPDA)PbI4]n(3), which were confirmed by X-ray single-crystal diffraction, infrared(IR) spectroscopy and powder X-ray diffraction(PXRD). Simultaneously, compounds 1~3 exhibit strong emission peaks at 600 nm for 1 and 2 and 570 nm for 3, which were originated from their inorganic moieties.展开更多
8-Hydroxyquinoline salt of pyrazine-2,3,5,6-tetracarboxylic acid [HQ]2[H2pztc]· 2H2O （1） was prepared and characterized by single-crystal X-ray diffraction, NMR, IR, TGA, elemental analysis and fluorescent meas...8-Hydroxyquinoline salt of pyrazine-2,3,5,6-tetracarboxylic acid [HQ]2[H2pztc]· 2H2O （1） was prepared and characterized by single-crystal X-ray diffraction, NMR, IR, TGA, elemental analysis and fluorescent measurements. Compound 1 crystallizes in orthorhombic, space group Pbcn with a = 9.953（3）, b = 15.966（3）, c = 16.081（5） A, V = 2555.5（13） A3, Z = 4, μ = 0.122 mm^-1, Dc = 1.514 Mg/m3, T= 296（2） K, C26H22N4O12, Mr = 582.48, F（000） = 1208, S = 1.006, R = 0.0448 and wR = 0.1149. Compound 1 has a three-dimensional （3D） network, in which pyra- zine-2,3,5,6-tetracarboxylic acids build up two-dimensional （2D） sheets and 8-hydroxyquinoline cations and water molecules act as pillars to connect the 2D sheets into an extended 3D network through strong intermolecular hydrogen bonding and π…π stacking interactions. Especially, a very short O-H…O hydrogen bond （O…O 2.470（2） A） between two neighboring [H2pztc] anions was observed.展开更多
3-Carboxy-2-pyrazinehydroxamic acid was prepared by a one pot reaction starting from pyrazine-2,3-dicarboxylic anhydride with a high yield, and characterized by IR, Mass spectrum, 1H NMR and 13C NMR spectra and single...3-Carboxy-2-pyrazinehydroxamic acid was prepared by a one pot reaction starting from pyrazine-2,3-dicarboxylic anhydride with a high yield, and characterized by IR, Mass spectrum, 1H NMR and 13C NMR spectra and single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with a=4.8659（10）, b=7.4233（15）, c=11.602（2）, α=96.904（2）, β=92.422（3）, γ=107.454（2）°, V=395.51（14）3 , Z=2, Dc=1.689g/cm3 , F（000）=208, μ（MoKα）=0.149 mm-1 , the final R=0.0473 and wR=0.1306 for 2853 observed reflections （I〉2σ （I））. A three-dimensional framework was assembled through intermolecular hydrogen bonding between water and 3-carboxy-2-pyrazine-carbohydroxamic acid molecules.展开更多
文摘设计并合成能用于识别铜离子的荧光探针N′-(喹啉-2-亚甲基)-7-二乙胺基-3-甲酰肼-香豆素(FKBA),通过质谱、红外光谱、元素分析、~1 H NMR、^(13) C NMR等方法对该荧光探针FKBA进行表征;采用荧光光谱法和紫外-可见光谱法对FKBA与金属离子的相互作用进行了研究。结果表明FKBA对Cu^(2+)有良好的选择性和灵敏度。向含有FKBA的溶液中加入Cu^(2+),其吸收峰发生红移,且强度增大。而向该溶液中,加入Al ^(3+),Ag^+,Ba^(2+),Cd^(2+),Ca^(2+),Co^(3+),Fe^(3+),Cr^(3+),Hg^(2+),Mg^(2+),K^+,Mn^(2+),Ni ^(2+),Na^+,Zn^(2+)和Pb^(2+)等其他16种金属离子时,FKBA的紫外吸收仅发生细微的变化。FKBA作为化学传感器对Cu^(2+)的选择性是通过与一系列与环保和生物功能相关的金属离子相互作用得到验证。FKBA中加入Cu^(2+)时,FKBA的荧光强度明显猝灭,其他16种金属离子对FKBA的荧光强度几乎没有影响。不同的金属离子分别与Cu^(2+)共存时FKBA的荧光光谱猝灭程度相同,说明FKBA具有良好的抗干扰能力。向FKBA中加入EDTA,FKBA的荧光强度得到恢复。FKBA中加入Cu^(2+),溶液颜色变成棕色,加入EDTA后又恢复到初始颜色。说明FKBA的荧光减弱不是Cu^(2+)催化FKBA分解而是FKBA与Cu^(2+)络合。在酸性环境中,FKBA的希夫碱结构不稳定,部分FKBA分解成其他的荧光物质。据IUPAC(cDL=3Sb/m)测得检测限为0.13μmol·L^(-1)。对实际样品中的Cu^(2+)浓度进行分析,表明FKBA可作为荧光传感器用于实际样品的Cu^(2+)检测。
基金supported by the National Natural Science Foundation of China(No.21571094)
文摘Co-crystallization of pztcH_4 with 4,4＇-bipyridine（4,4＇-bipy） in pH = 3-4 and 1-2 gave two new binary molecular adducts： [（4,4＇-bipy H2）（pztc H2）]（1） and [（4,4＇-bipy H2）（pztcH3）（Cl）]·4H2O（2）, respectively. Compounds 1 and 2 have been characterized by IR, elemental analysis, NMR and X-ray single-crystal diffraction. Compound 1 crystallizes in triclinic, space group P1 with a = 5.7752（12）, b = 7.9126（16）, c = 9.4492（19） ？, α = 97.49（3）, β = 107.71（3）, γ = 94.52（3）o, V = 404.62（14） A^3, Z = 1, μ = 0.137 mm^1, Dc = 1.692 Mg/m^3, C18H12N4O8, Mr = 412.32, F（000） = 212, S = 1.025, R = 0.0360 and wR = 0.0973. Compound 2 crystallizes in monoclinic, space group C2/c with a = 17.093（3）, b = 7.7665（16）, c = 18.414（4） A, β = 113.36（3）o, V = 2244.1（8） A^3, Z = 4, μ = 0.244 mm^-1, Dc = 1.542 Mg/m^3, C18H21ClN4O12, Mr = 520.84, F（000） = 1080, S = 1.021, R = 0.0343 and wR = 0.0978. In compound 1, pztc H22- anions self-formed 2-D sheets by strong Oacid-H···Oacidhydrogen bonds, which are further extended to form a 3-D supramolecular network bridged with 4,4？-bipy via N-H···Oacid interactions. In compound 2, besides the 1-D chain constructed by pztc H3-itself through strong H-bond Oacid-H···Oacid, the other chain is constructed with 4,4？-bipy H22＋, Cl-anion and water molecules by moderate H-bonds and Ow-H···Cl and N-H···Ow. The two chains are linked with μ3-connected water molecules resulting from the combination of strong synthon-assisted H-bonding Oacid-H···Ow to afford an interlaced 3-D network.
基金Financially supported by the National Natural Science Foundation of China(No.21571094,21661021,21865015)the Graduate Student Creativity Funding of Jiangxi Province(No.YC2015-S008)
文摘Reactions of piperidine derivatives 4-(aminomethyl)piperidine(4-AMPD) and 1-methylpiperidin-4-amine(1-MPDA) with semi-conductive metal iodine SbI3 and PbI2 in concentrated HI aqueous solution afforded two one-dimensional(1 D) chain compounds [(4-AMPD)SbI5]n(1), [(1-MPDA)SbI5]n(2) and a two-dimensional(2 D) single layered organicinorganic hybrid material [(1-MPDA)PbI4]n(3), which were confirmed by X-ray single-crystal diffraction, infrared(IR) spectroscopy and powder X-ray diffraction(PXRD). Simultaneously, compounds 1~3 exhibit strong emission peaks at 600 nm for 1 and 2 and 570 nm for 3, which were originated from their inorganic moieties.
基金supported by the National Natural Science Foundation of China(No.21162015)Science Foundation of State Key Laboratory of Structural Chemistry(No.20100009)
文摘8-Hydroxyquinoline salt of pyrazine-2,3,5,6-tetracarboxylic acid [HQ]2[H2pztc]· 2H2O （1） was prepared and characterized by single-crystal X-ray diffraction, NMR, IR, TGA, elemental analysis and fluorescent measurements. Compound 1 crystallizes in orthorhombic, space group Pbcn with a = 9.953（3）, b = 15.966（3）, c = 16.081（5） A, V = 2555.5（13） A3, Z = 4, μ = 0.122 mm^-1, Dc = 1.514 Mg/m3, T= 296（2） K, C26H22N4O12, Mr = 582.48, F（000） = 1208, S = 1.006, R = 0.0448 and wR = 0.1149. Compound 1 has a three-dimensional （3D） network, in which pyra- zine-2,3,5,6-tetracarboxylic acids build up two-dimensional （2D） sheets and 8-hydroxyquinoline cations and water molecules act as pillars to connect the 2D sheets into an extended 3D network through strong intermolecular hydrogen bonding and π…π stacking interactions. Especially, a very short O-H…O hydrogen bond （O…O 2.470（2） A） between two neighboring [H2pztc] anions was observed.
基金supported by the National Natural Science Foundation of China (No. 20861007)Science Foundation of State Key Laboratory of Structural Chemistry (No. 20100009)Science and Technology Research Projects in Department of Education of Jiangxi Province (No. GJJ08026)
文摘3-Carboxy-2-pyrazinehydroxamic acid was prepared by a one pot reaction starting from pyrazine-2,3-dicarboxylic anhydride with a high yield, and characterized by IR, Mass spectrum, 1H NMR and 13C NMR spectra and single-crystal X-ray diffraction. It crystallizes in triclinic, space group Pī with a=4.8659（10）, b=7.4233（15）, c=11.602（2）, α=96.904（2）, β=92.422（3）, γ=107.454（2）°, V=395.51（14）3 , Z=2, Dc=1.689g/cm3 , F（000）=208, μ（MoKα）=0.149 mm-1 , the final R=0.0473 and wR=0.1306 for 2853 observed reflections （I〉2σ （I））. A three-dimensional framework was assembled through intermolecular hydrogen bonding between water and 3-carboxy-2-pyrazine-carbohydroxamic acid molecules.
