A novel and simple fluorescent molecular sensor,1-pyrenecarboxaldehyde thiosemicarbazone（Hpytsc）,was synthesized.Its higher sensitivity and selectivity to mercury（Ⅱ） ion were studied through absorption and emissi...A novel and simple fluorescent molecular sensor,1-pyrenecarboxaldehyde thiosemicarbazone（Hpytsc）,was synthesized.Its higher sensitivity and selectivity to mercury（Ⅱ） ion were studied through absorption and emission channels.The UV-vis spectra show that the increasing mercury（Ⅱ） ion concentrations result in the decreasing absorption intensity.The fluorescence monomer emission of Hpytsc is enhanced upon binding mercury（Ⅱ） ion,which should be due to the 1：1 complex formation between Hpytsc and metal ion.展开更多
The reaction of 1,3-dipropyn-2-yloxycalix[4]arene with mercury（U） acetate could give mercury-containing alkynyl calixarene polymer. The extraction behavior of 1,3-dipropyn-2-yl-oxycalix[4]arene towards mercury（Ⅱ）...The reaction of 1,3-dipropyn-2-yloxycalix[4]arene with mercury（U） acetate could give mercury-containing alkynyl calixarene polymer. The extraction behavior of 1,3-dipropyn-2-yl-oxycalix[4]arene towards mercury（Ⅱ） ion was examined. When the mole ratio of Hg^2＋/calixarene was 1：1, the extractive percent can reach to 99.1%, and the extraction capacity was up to 431 mg/g. It could also decrease the Hg^2＋ concentration from 5 to 0.85 mg/L, which was only 17% of the national standard of effluent and satisfied the national standard of drinking water. The extraction process included chemical reaction.展开更多
Reaction of HgCl2 and double betaine ligands in water at about 80 ℃ yielded two new Hg（Ⅱ） complexes,[Hg（L1）Cl2]·H2O 1 and [Hg2（L2）Cl4]·3HgCl2 2（L1 = 1,3-bis（pyridinio-4-carboxylato）-propane,L2 = 1...Reaction of HgCl2 and double betaine ligands in water at about 80 ℃ yielded two new Hg（Ⅱ） complexes,[Hg（L1）Cl2]·H2O 1 and [Hg2（L2）Cl4]·3HgCl2 2（L1 = 1,3-bis（pyridinio-4-carboxylato）-propane,L2 = 1,4-bis（pyridinio-4-carboxylato）-1,4-dimenthylbenzene）.Their struc-tures have been characterized by single-crystal X-ray diffraction techniques.The structure of 1 contains 1-D chains,in which the adjacent Hg（Ⅱ） atoms are bridged by L1 ligands in a syn-syn bis-monodentate mode.The chains are further connected through face-to-face π-π stacking interactions between pyridine rings to generate an infinite double-chain network.In 2,two Hg（Ⅱ） atoms are joined by L2 ligands in the same coordination mode as 1 to form an isolated dinuclear structure.The thermal stabilities of both complexes have also been investigated.展开更多
A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally ch...A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data： C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218（4）, b = 9.551（3）, c = 15.877（4） A^°, β = 129.697（15）°, V = 1308.9（7） A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F（000） = 995, μ（MoKa） = 14.415 mm^-1, 2（MoKa） = 0.71073 A^°, T= 293（2） K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ（I） （refinement on F^2）. Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439（4） and 3.603（4） A^°, so complex 1 expands the chains into a two-dimensional network.展开更多
A novel mercury（H） complex HgL2Br2 was prepared from HgBr2 and the organic ligand 2-（N-methyl-N-（4-（（E）-2-（pyridine-4-yl）vinyl）phenyl）amino）ethanol （L）. The ligand was synthesized and then characterized ...A novel mercury（H） complex HgL2Br2 was prepared from HgBr2 and the organic ligand 2-（N-methyl-N-（4-（（E）-2-（pyridine-4-yl）vinyl）phenyl）amino）ethanol （L）. The ligand was synthesized and then characterized by FT-IR spectroscopy, tH NMR, mass spectrum and elemental analysis, while the single-crystal diffraction data of the complex were collected on a Siemens Smart CCD diffractometer. The complex crystallizes in triclinic space group PI with a = 5.367（5）, b = 12.466（5）, c = 23.945（5） A, α = 90.812（5）, β = 96.318（4）, γ = 96.093（5）°, Z = 2, Dc = 1.817 g.cm3,μ = 7.395 mm^-1, S = 0.825, and the final R= 0.0396. The Hg（Ⅱ） ion in the distorted tetrahedral mercury（Ⅱ） complex C32H36HgBr2N4O2 is coordinated by two N atoms from the two ligands together with two bromide ions. Solid-state emission of the ligand and its complex has been investigated at room temperature.展开更多
A novel iodine-bridged mercury（Ⅱ） complex [Hg（L）（μ-I）（I）]2 was isolated by a reaction between HgI2 and the organic ligand tris[4-（1-pyrazolyl）phenyl]amine L, and the complex and ligand were both characteri...A novel iodine-bridged mercury（Ⅱ） complex [Hg（L）（μ-I）（I）]2 was isolated by a reaction between HgI2 and the organic ligand tris[4-（1-pyrazolyl）phenyl]amine L, and the complex and ligand were both characterized by FT-IR spectroscopy, ^1H NMR and elemental analysis. The complex crystallizes in monoclinic space group P21/c with a = 9.579（5）, b = 27.331 （5）, c = 11.268（5） А, β= 105.624（5）°, Z = 2, Dc = 2.099 g·cm^-3 and μ= 7.620 mm^-1. The title complex C54H42Hg2I4N14 is a diplex bridged dinuclear complex consisting of two Hg（Ⅱ） ions, two ligands, two bridging I-anions, and two terminal I-anions. Universal hydrogen bonds in the complex with the partners of neighboring molecule have generated a supramolecular arrangement. Solid-state emission of the ligand and its complex have been investigated at room temperature.展开更多
The adsorption isotherms of the polysulfone hollow fiber chelating membrane modified with thionrea as chelating groups for Hg^2＋ were determined. The effects of mobile phase conditions and the operating parameters on...The adsorption isotherms of the polysulfone hollow fiber chelating membrane modified with thionrea as chelating groups for Hg^2＋ were determined. The effects of mobile phase conditions and the operating parameters on removal performance of the chelating membrane for Hg^2＋ were also investigated. The recovery of Hg^2＋ decreased at low pH and the optimum range of pH was from 6 to 7. The feed concentration effected on recovery of Hg^2＋ at the specified loading amount of Hg^2＋. The Hg^2＋ could be removed from different concentration feed solution by chelating membrane. The increase of feed flow rate led to slight decrease of recovery of Hg^2＋ at the specified loading amount of Hg^2＋. The chelating membrane could be operated at height feed flow rate and a large-scale removal of H^2＋ could be realized. With the increase of load amount, Hg^2＋ recovery decreased, but the saturation degree of chelating membrane increased. According to required recovery of H^2＋ and the saturation degree of chelating membrane, the optimum loading amount of Hg^2＋ should be selected in the actual removal of H^2＋.展开更多
Two novel mononuclear complexes with 5-chloro-8-（methoxycarbonylmethoxy）quinoline ligand（L）, namely, HgLBr2 1 and CuL2Cl2 2, have been prepared by solvothermal reaction of（5-chloro-quinolin-8-yloxy）acetic acid w...Two novel mononuclear complexes with 5-chloro-8-（methoxycarbonylmethoxy）quinoline ligand（L）, namely, HgLBr2 1 and CuL2Cl2 2, have been prepared by solvothermal reaction of（5-chloro-quinolin-8-yloxy）acetic acid with HgBr2 and CuCl2, respectively. Their structures were characterized by IR, elemental analysis, UV-Vis-NIR spectra, TG and single-crystal X-ray diffraction analysis. Interestingly,（5-chloro-quinolin-8-yloxy）acetic acid is changed as 5-chloro-8-（methoxycarbonylmethoxy）quinoline ligand（L） in complexes 1 and 2. Crystal data for 1： C12H10Br2 Cl Hg NO3, Mr = 612.07, triclinic, space group P1 with a = 8.5983（7）, b = 9.7726（6）, c = 10.1549（6） A, α = 66.355（6）, β = 77.067（8）, γ = 78.803（8）°, V = 756.6（9）A^3, Z = 2, Dc = 2.687 g/cm^3, F（000） = 560, μ = 15.633 mm^-1, R = 0.0351 and w R = 0.0504. Crystal data for 2： C24H20Cl4 Cu N2O6, Mr = 637.76, triclinic, space group P1 with a = 10.5324（9）, b = 11.2377（16）, c = 12.0143（12） ？, α = 83.413（11）, β = 64.475（9）, γ = 83.144（11）°, V = 1270.9（2） ？3, Z = 2, Dc = 1.667 g/cm3, F（000） = 646, μ = 1.324 mm-1, R = 0.0408 and wR = 0.0922. In 1, the HgII centre is a distorted trigonal planar geometry comprised of two Br atoms and one quinoline N atom of L. Intermolecular π-π, C–H…π stacking interactions and intermolecular C–H…Br hydrogen bonds are observed in the molecular packing of 1. In complex 2, each CuII center has a distorted octahedral geometry comprised of two chloride ions, two quinoline N atoms and two O atoms of two L ligands. Intermolecular C–H…Cl hydrogen bonds exist in the molecular packing of 2. The fluorescence emission peak of complexes 1 and 2 appears near 406 and 410 nm, respectively. Optical diffuse-reflection spectral results suggest complex 1 has the property of semiconductor.展开更多
The title complex, mercury bridged biferrocene trinuclear complex Hg(FcL)2. Bis (S-methyl-N- (1-ferrocenyl-1-methyl) methylenedithiocarbazate) mercury,Crystallizes in space group Pbca with a =19. 510 (4), b=19. 921 (5...The title complex, mercury bridged biferrocene trinuclear complex Hg(FcL)2. Bis (S-methyl-N- (1-ferrocenyl-1-methyl) methylenedithiocarbazate) mercury,Crystallizes in space group Pbca with a =19. 510 (4), b=19. 921 (5), c=15. 581 (3)A. V=6095(3) A, Z=8,M.=863. 12, Dc=1.881 g/cm3; u=19. 24 cm-1 and F(000) = 3376. The final refinement of 2455 observed reflections is converged with R= 0. 043 and Rw=0.047. X-ray crystal structure analysis revealed that the coordinationgeometry of Hg atom is a distorted tetrahedron with two Hg-N bonds and two Hg- S bonds. The Schiff-base ligand loses a proton from its tautomeric thiol form and is cryordianted to the Hg aotm uia the mercapto sulphur and the β-nitrogen atoms.展开更多
基金financed by the Graduate Innovation Foundation of Logistic Engineering University(Chongqing, China)
文摘A novel and simple fluorescent molecular sensor,1-pyrenecarboxaldehyde thiosemicarbazone（Hpytsc）,was synthesized.Its higher sensitivity and selectivity to mercury（Ⅱ） ion were studied through absorption and emission channels.The UV-vis spectra show that the increasing mercury（Ⅱ） ion concentrations result in the decreasing absorption intensity.The fluorescence monomer emission of Hpytsc is enhanced upon binding mercury（Ⅱ） ion,which should be due to the 1：1 complex formation between Hpytsc and metal ion.
文摘The reaction of 1,3-dipropyn-2-yloxycalix[4]arene with mercury（U） acetate could give mercury-containing alkynyl calixarene polymer. The extraction behavior of 1,3-dipropyn-2-yl-oxycalix[4]arene towards mercury（Ⅱ） ion was examined. When the mole ratio of Hg^2＋/calixarene was 1：1, the extractive percent can reach to 99.1%, and the extraction capacity was up to 431 mg/g. It could also decrease the Hg^2＋ concentration from 5 to 0.85 mg/L, which was only 17% of the national standard of effluent and satisfied the national standard of drinking water. The extraction process included chemical reaction.
基金financially supported by the National Natural Science Foundation of China (20871115)Fujian Provincial Key Laboratory of Nanomaterials (NM10-06)
文摘Reaction of HgCl2 and double betaine ligands in water at about 80 ℃ yielded two new Hg（Ⅱ） complexes,[Hg（L1）Cl2]·H2O 1 and [Hg2（L2）Cl4]·3HgCl2 2（L1 = 1,3-bis（pyridinio-4-carboxylato）-propane,L2 = 1,4-bis（pyridinio-4-carboxylato）-1,4-dimenthylbenzene）.Their struc-tures have been characterized by single-crystal X-ray diffraction techniques.The structure of 1 contains 1-D chains,in which the adjacent Hg（Ⅱ） atoms are bridged by L1 ligands in a syn-syn bis-monodentate mode.The chains are further connected through face-to-face π-π stacking interactions between pyridine rings to generate an infinite double-chain network.In 2,two Hg（Ⅱ） atoms are joined by L2 ligands in the same coordination mode as 1 to form an isolated dinuclear structure.The thermal stabilities of both complexes have also been investigated.
基金supported by 973 Program (2006CB932900)the National Natural Science Foundation of China (20571074)
文摘A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data： C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218（4）, b = 9.551（3）, c = 15.877（4） A^°, β = 129.697（15）°, V = 1308.9（7） A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F（000） = 995, μ（MoKa） = 14.415 mm^-1, 2（MoKa） = 0.71073 A^°, T= 293（2） K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ（I） （refinement on F^2）. Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439（4） and 3.603（4） A^°, so complex 1 expands the chains into a two-dimensional network.
基金supported by the National Natural Science Foundation of China(No.20771001,50703001)Team for Scientific Innovation Foundation of Hefei University(No.2006KJ007TD)
文摘A novel mercury（H） complex HgL2Br2 was prepared from HgBr2 and the organic ligand 2-（N-methyl-N-（4-（（E）-2-（pyridine-4-yl）vinyl）phenyl）amino）ethanol （L）. The ligand was synthesized and then characterized by FT-IR spectroscopy, tH NMR, mass spectrum and elemental analysis, while the single-crystal diffraction data of the complex were collected on a Siemens Smart CCD diffractometer. The complex crystallizes in triclinic space group PI with a = 5.367（5）, b = 12.466（5）, c = 23.945（5） A, α = 90.812（5）, β = 96.318（4）, γ = 96.093（5）°, Z = 2, Dc = 1.817 g.cm3,μ = 7.395 mm^-1, S = 0.825, and the final R= 0.0396. The Hg（Ⅱ） ion in the distorted tetrahedral mercury（Ⅱ） complex C32H36HgBr2N4O2 is coordinated by two N atoms from the two ligands together with two bromide ions. Solid-state emission of the ligand and its complex has been investigated at room temperature.
基金supported by the National Natural Science Foundation of China (No. 50532030, 50703001, 20771001)Team for Scientific Innovation Foundation of Hefei University (No. 2006KJ007TD)
文摘A novel iodine-bridged mercury（Ⅱ） complex [Hg（L）（μ-I）（I）]2 was isolated by a reaction between HgI2 and the organic ligand tris[4-（1-pyrazolyl）phenyl]amine L, and the complex and ligand were both characterized by FT-IR spectroscopy, ^1H NMR and elemental analysis. The complex crystallizes in monoclinic space group P21/c with a = 9.579（5）, b = 27.331 （5）, c = 11.268（5） А, β= 105.624（5）°, Z = 2, Dc = 2.099 g·cm^-3 and μ= 7.620 mm^-1. The title complex C54H42Hg2I4N14 is a diplex bridged dinuclear complex consisting of two Hg（Ⅱ） ions, two ligands, two bridging I-anions, and two terminal I-anions. Universal hydrogen bonds in the complex with the partners of neighboring molecule have generated a supramolecular arrangement. Solid-state emission of the ligand and its complex have been investigated at room temperature.
基金the Natural Science Foundation of Tianjin (No05YFJ MJC04200)
文摘The adsorption isotherms of the polysulfone hollow fiber chelating membrane modified with thionrea as chelating groups for Hg^2＋ were determined. The effects of mobile phase conditions and the operating parameters on removal performance of the chelating membrane for Hg^2＋ were also investigated. The recovery of Hg^2＋ decreased at low pH and the optimum range of pH was from 6 to 7. The feed concentration effected on recovery of Hg^2＋ at the specified loading amount of Hg^2＋. The Hg^2＋ could be removed from different concentration feed solution by chelating membrane. The increase of feed flow rate led to slight decrease of recovery of Hg^2＋ at the specified loading amount of Hg^2＋. The chelating membrane could be operated at height feed flow rate and a large-scale removal of H^2＋ could be realized. With the increase of load amount, Hg^2＋ recovery decreased, but the saturation degree of chelating membrane increased. According to required recovery of H^2＋ and the saturation degree of chelating membrane, the optimum loading amount of Hg^2＋ should be selected in the actual removal of H^2＋.
基金Supported by Key Laboratory of Organic Synthesis of Jiangsu Province(KJS1308)
文摘Two novel mononuclear complexes with 5-chloro-8-（methoxycarbonylmethoxy）quinoline ligand（L）, namely, HgLBr2 1 and CuL2Cl2 2, have been prepared by solvothermal reaction of（5-chloro-quinolin-8-yloxy）acetic acid with HgBr2 and CuCl2, respectively. Their structures were characterized by IR, elemental analysis, UV-Vis-NIR spectra, TG and single-crystal X-ray diffraction analysis. Interestingly,（5-chloro-quinolin-8-yloxy）acetic acid is changed as 5-chloro-8-（methoxycarbonylmethoxy）quinoline ligand（L） in complexes 1 and 2. Crystal data for 1： C12H10Br2 Cl Hg NO3, Mr = 612.07, triclinic, space group P1 with a = 8.5983（7）, b = 9.7726（6）, c = 10.1549（6） A, α = 66.355（6）, β = 77.067（8）, γ = 78.803（8）°, V = 756.6（9）A^3, Z = 2, Dc = 2.687 g/cm^3, F（000） = 560, μ = 15.633 mm^-1, R = 0.0351 and w R = 0.0504. Crystal data for 2： C24H20Cl4 Cu N2O6, Mr = 637.76, triclinic, space group P1 with a = 10.5324（9）, b = 11.2377（16）, c = 12.0143（12） ？, α = 83.413（11）, β = 64.475（9）, γ = 83.144（11）°, V = 1270.9（2） ？3, Z = 2, Dc = 1.667 g/cm3, F（000） = 646, μ = 1.324 mm-1, R = 0.0408 and wR = 0.0922. In 1, the HgII centre is a distorted trigonal planar geometry comprised of two Br atoms and one quinoline N atom of L. Intermolecular π-π, C–H…π stacking interactions and intermolecular C–H…Br hydrogen bonds are observed in the molecular packing of 1. In complex 2, each CuII center has a distorted octahedral geometry comprised of two chloride ions, two quinoline N atoms and two O atoms of two L ligands. Intermolecular C–H…Cl hydrogen bonds exist in the molecular packing of 2. The fluorescence emission peak of complexes 1 and 2 appears near 406 and 410 nm, respectively. Optical diffuse-reflection spectral results suggest complex 1 has the property of semiconductor.
文摘The title complex, mercury bridged biferrocene trinuclear complex Hg(FcL)2. Bis (S-methyl-N- (1-ferrocenyl-1-methyl) methylenedithiocarbazate) mercury,Crystallizes in space group Pbca with a =19. 510 (4), b=19. 921 (5), c=15. 581 (3)A. V=6095(3) A, Z=8,M.=863. 12, Dc=1.881 g/cm3; u=19. 24 cm-1 and F(000) = 3376. The final refinement of 2455 observed reflections is converged with R= 0. 043 and Rw=0.047. X-ray crystal structure analysis revealed that the coordinationgeometry of Hg atom is a distorted tetrahedron with two Hg-N bonds and two Hg- S bonds. The Schiff-base ligand loses a proton from its tautomeric thiol form and is cryordianted to the Hg aotm uia the mercapto sulphur and the β-nitrogen atoms.
