Terbium perchlorate reacted with isonicotinic acid （Hpya） and biphenyl-2,2＇-dicarboxylic acid （H2dpa） under hydrothermal condition, a new ternary terbium complex [ Tb （pya） （dpa） （H2O） n （ 1 ） was synthes...Terbium perchlorate reacted with isonicotinic acid （Hpya） and biphenyl-2,2＇-dicarboxylic acid （H2dpa） under hydrothermal condition, a new ternary terbium complex [ Tb （pya） （dpa） （H2O） n （ 1 ） was synthesized. The structure of the ternary complex was determined by X-ray single crystal diffraction and characterized by elemental analysis, fluorescence measurement. The fluorescence spectrum shows the title complex emits strong green light. The crystal data for the com- plex： monoclinic, P21/n space group, a =0.8908（5）nm, b = 1.0569（6）nm, c =2.0969（11）nm, β = 98.446（8）°, V = 1.9528（18） nm^3, Z = 4, R = 0.0241, wR2 = 0.0534. The center Tb3＋ ion is eight coordinated. The coordination polyhedron around Tb3 ＋ ion can be described as a distorted square antiprism. The complex forms an infinite one-dimenand sional alternating chain polymer by bridging carboxyl groups of pyadpa.展开更多
The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1：1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ f...The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1：1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356（2）, b = 7.0761（11）, c = 20.539（3） A, β = 105.723（4）°, V= 1868.5（5） A3 and Z = 4.展开更多
Six N-alkyl-4＇-methyl-1,1＇-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki r...Six N-alkyl-4＇-methyl-1,1＇-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki reaction.The structures of the new compounds synthesized were confirmed by elemental analysis,IR,1H NMR and MS.This new method makes a feature of low cost and readily available starting material,fewer steps,mild condition,easiness to operate and higher yield.展开更多
Use of free air as oxidant and copper（II）chloride as catalyst,3,3＇-di-tert-butylbi-phenyl-2,5,2＇,5＇-diquinone（BBDQ）was prepared via catalytic oxidation of 2,2＇-dihydroxy-3,3＇-di-tert-butyl-5,5＇-dimethoxy-bip...Use of free air as oxidant and copper（II）chloride as catalyst,3,3＇-di-tert-butylbi-phenyl-2,5,2＇,5＇-diquinone（BBDQ）was prepared via catalytic oxidation of 2,2＇-dihydroxy-3,3＇-di-tert-butyl-5,5＇-dimethoxy-biphenyl（di-BHA）.The yield of reaction attained 95% and the selectivity for BBDQ was 100%.The single-crystal X-ray diffraction analysis reveals that the dihedral angle between two rings（benzene rings for di-BHA and quinone rings for BBDQ）changes from 89.8 to 45.3o,indicating the steric hindrance effects of methyl disappear in the oxidation process.The crystal structures of di-BHA and BBDQ are further confirmed by their spectral characterizations.The probable mechanism for this oxidation process is also discussed.展开更多
A new coordination polymer,[Cu2（bptc）（2,2＇-bpy） 2（H2O）]·H2O（2,2＇-bpy = 2,2＇-bipyridine,H4bptc = biphenyl-2,5,2＇,5＇-tetracarboxylic acid） ,has been synthesized under hydrother-mal conditions. The stru...A new coordination polymer,[Cu2（bptc）（2,2＇-bpy） 2（H2O）]·H2O（2,2＇-bpy = 2,2＇-bipyridine,H4bptc = biphenyl-2,5,2＇,5＇-tetracarboxylic acid） ,has been synthesized under hydrother-mal conditions. The structure was characterized by single-crystal X-ray diffraction,elemental analysis,IR spectra and thermogravimetric analysis. It crystallizes in triclinic,space group P1 with a = 10.6447（12） ,b = 11.0191（12）,c = 16.1253（18）A,α = 79.538（2）,β = 88.0720（10） ,γ = 61.6650（10） °,V = 1634.1（3） A^3,C36H26Cu2N4O10,Mr = 801.69,Z = 2,Dc = 1.629 g/cm^3,μ（MoKα） = 1.370 mm^-1,F（000） = 816.0,R = 0.0418 and wR = 0.1135 for 4416 observed reflections with I 〉 2σ（I） . X-ray analysis shows that the title complex exhibits 1D wavelike [Cu2（bptc） ]n chains with two types of diamond-shaped pores. These 1D chains are linked into a 3D supramolecular structure via O-H···O,C-H···O interactions and weak π···π stacking interactions. There exist H-bonded helices in a right-and left-handed sequence by turns in a 2D layer. Moreover,thermal stability has been studied and magnetic measurements show antiferromagnetic interactions for this complex.展开更多
A new 3D Ag（I） coordination polymer, [Ag8（btc）2（bpp）2]n（1, H4btc = biphenyl- 2,2ˊ,4,4ˊ-tetracarboxylic acid, bpp = 1,2-bis（4-pyridyl）propane）, has been hydrothermally synthesi- zed and characterized by sin...A new 3D Ag（I） coordination polymer, [Ag8（btc）2（bpp）2]n（1, H4btc = biphenyl- 2,2ˊ,4,4ˊ-tetracarboxylic acid, bpp = 1,2-bis（4-pyridyl）propane）, has been hydrothermally synthesi- zed and characterized by single-crystal X-ray diffraction analysis, elemental analysis and IR spectroscopy. Complex 1 crystallizes in the triclinic system, space group P1 with a = 13.4899（8）, b = 13.4928（8）, c = 16.4575（10） , α = 102.7640（10）, β = 108.8100（10）, γ = 101.4940（10）°, V = 2644.1（3） 3, Z = 2, Dc = 2.401 Mg·m-3, μ = 2.978 mm-1, F（000） = 1840, the final R = 0.0481 and wR = 0.0955 for 6794 observed reflections with I 〉 2σ（I）. Complex 1 features a 3D framework formed by Ag（I）-carboxylate chains containing [Ag16（COO）16] secondary building block. Furthermore, thermal stability and electrochemical property of 1 are also investigated in detail.展开更多
Hydrothermal reactions of biphenyl-2,3,3A,5A-tetracarboxylic acid（H4bptc） with cobalt salt in the presence of 1,4-bis（2-pyridylmethyl）piperazin（bpmp） afforded one novel coordination polymer, namely, [Co（H2bptc...Hydrothermal reactions of biphenyl-2,3,3A,5A-tetracarboxylic acid（H4bptc） with cobalt salt in the presence of 1,4-bis（2-pyridylmethyl）piperazin（bpmp） afforded one novel coordination polymer, namely, [Co（H2bptc）（bpmp）0.5（H2O）]n（1）. Its structure was established by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra and TG analysis. Complex 1 crystallizes in monoclinic, space group P21/c with a = 11.4839（11）, b = 16.6690（16）, c = 11.5559（11） A, V = 2201.8（4） A3, Mr = 539.35, Dc = 1.627 g/cm^3, μ（MoK α） = 0.841 mm-1, F（000） = 1108, Z = 4, the final R = 0.0309 and w R = 0.0705 for 4090 observed reflections（I 2σ（I））. Complex 1 displays a one-dimensional（1D） chain bridged by bpmp. Two carboxylic groups of H4 bptc ligand adopt μ01-η1：η1 and μ1-η1：η coordination modes to bridge adjacent Co（Ⅱ） ions together with bpmp ligand to give alternately arranged left- and right-handed helical chains. In addition, variable-temperature magnetic susceptibility measurements indicate that complex 1 shows weak antiferromagnetic interactions between the adjacent Co（Ⅱ） ions.展开更多
化工、纺织印染与农药化肥等产业的蓬勃发展推动着人类社会的进步,但同时也给环境治理带来了巨大难题。目前,光催化降解局限于在特定波长下针对单一有机污染物进行降解,然而现实中的情况往往更复杂。因此,开发一种多功能光催化材料用于...化工、纺织印染与农药化肥等产业的蓬勃发展推动着人类社会的进步,但同时也给环境治理带来了巨大难题。目前,光催化降解局限于在特定波长下针对单一有机污染物进行降解,然而现实中的情况往往更复杂。因此,开发一种多功能光催化材料用于光催化降解不同有机污染物显得尤为重要。采用一步无模板溶剂热法合成了核壳结构的C-TiO_(2)复合材料前驱体,并在氩气气氛下煅烧得到高结晶度的C-TiO_(2)复合光催化材料。运用SEM、TEM、XRD和TG等表征手段对材料进行表征,结论如下:550℃煅烧时的样品为包含少量碳的高结晶度的锐钛矿相TiO 2,且550℃煅烧时的样品依然保持了完整的核壳结构。此外,C-TiO_(2)复合材料的比表面积高达85.69 m 2·g^(-1),平均孔径为16.4 nm以及孔体积为0.423 m 3·g^(-1)。在UV-Vis光照射下,C-TiO_(2)复合材料分别对罗丹明B(RhB)、亚甲基蓝(MB)和刚果红(CR)3种染料显示出增强的光催化降解活性。展开更多
文摘Terbium perchlorate reacted with isonicotinic acid （Hpya） and biphenyl-2,2＇-dicarboxylic acid （H2dpa） under hydrothermal condition, a new ternary terbium complex [ Tb （pya） （dpa） （H2O） n （ 1 ） was synthesized. The structure of the ternary complex was determined by X-ray single crystal diffraction and characterized by elemental analysis, fluorescence measurement. The fluorescence spectrum shows the title complex emits strong green light. The crystal data for the com- plex： monoclinic, P21/n space group, a =0.8908（5）nm, b = 1.0569（6）nm, c =2.0969（11）nm, β = 98.446（8）°, V = 1.9528（18） nm^3, Z = 4, R = 0.0241, wR2 = 0.0534. The center Tb3＋ ion is eight coordinated. The coordination polyhedron around Tb3 ＋ ion can be described as a distorted square antiprism. The complex forms an infinite one-dimenand sional alternating chain polymer by bridging carboxyl groups of pyadpa.
文摘The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1：1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356（2）, b = 7.0761（11）, c = 20.539（3） A, β = 105.723（4）°, V= 1868.5（5） A3 and Z = 4.
文摘Six N-alkyl-4＇-methyl-1,1＇-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki reaction.The structures of the new compounds synthesized were confirmed by elemental analysis,IR,1H NMR and MS.This new method makes a feature of low cost and readily available starting material,fewer steps,mild condition,easiness to operate and higher yield.
基金supported by the 973 Program (2005CB623607)the National Natural Science Foundation of China (No.20771061)the scientific program 2008BAE64B09
文摘Use of free air as oxidant and copper（II）chloride as catalyst,3,3＇-di-tert-butylbi-phenyl-2,5,2＇,5＇-diquinone（BBDQ）was prepared via catalytic oxidation of 2,2＇-dihydroxy-3,3＇-di-tert-butyl-5,5＇-dimethoxy-biphenyl（di-BHA）.The yield of reaction attained 95% and the selectivity for BBDQ was 100%.The single-crystal X-ray diffraction analysis reveals that the dihedral angle between two rings（benzene rings for di-BHA and quinone rings for BBDQ）changes from 89.8 to 45.3o,indicating the steric hindrance effects of methyl disappear in the oxidation process.The crystal structures of di-BHA and BBDQ are further confirmed by their spectral characterizations.The probable mechanism for this oxidation process is also discussed.
基金supported by the NNSFC (No.20771023)the State 863 Program Project (No.2007AA03z218)Analysis and Testing Foundation of Northeast Normal University
文摘A new coordination polymer,[Cu2（bptc）（2,2＇-bpy） 2（H2O）]·H2O（2,2＇-bpy = 2,2＇-bipyridine,H4bptc = biphenyl-2,5,2＇,5＇-tetracarboxylic acid） ,has been synthesized under hydrother-mal conditions. The structure was characterized by single-crystal X-ray diffraction,elemental analysis,IR spectra and thermogravimetric analysis. It crystallizes in triclinic,space group P1 with a = 10.6447（12） ,b = 11.0191（12）,c = 16.1253（18）A,α = 79.538（2）,β = 88.0720（10） ,γ = 61.6650（10） °,V = 1634.1（3） A^3,C36H26Cu2N4O10,Mr = 801.69,Z = 2,Dc = 1.629 g/cm^3,μ（MoKα） = 1.370 mm^-1,F（000） = 816.0,R = 0.0418 and wR = 0.1135 for 4416 observed reflections with I 〉 2σ（I） . X-ray analysis shows that the title complex exhibits 1D wavelike [Cu2（bptc） ]n chains with two types of diamond-shaped pores. These 1D chains are linked into a 3D supramolecular structure via O-H···O,C-H···O interactions and weak π···π stacking interactions. There exist H-bonded helices in a right-and left-handed sequence by turns in a 2D layer. Moreover,thermal stability has been studied and magnetic measurements show antiferromagnetic interactions for this complex.
基金supported by the National Natural Science Foundation of China(No.21373178)the Natural Scientific Research Foundation of Shaanxi Provincial Education Office of China(No.13JS124)
文摘A new 3D Ag（I） coordination polymer, [Ag8（btc）2（bpp）2]n（1, H4btc = biphenyl- 2,2ˊ,4,4ˊ-tetracarboxylic acid, bpp = 1,2-bis（4-pyridyl）propane）, has been hydrothermally synthesi- zed and characterized by single-crystal X-ray diffraction analysis, elemental analysis and IR spectroscopy. Complex 1 crystallizes in the triclinic system, space group P1 with a = 13.4899（8）, b = 13.4928（8）, c = 16.4575（10） , α = 102.7640（10）, β = 108.8100（10）, γ = 101.4940（10）°, V = 2644.1（3） 3, Z = 2, Dc = 2.401 Mg·m-3, μ = 2.978 mm-1, F（000） = 1840, the final R = 0.0481 and wR = 0.0955 for 6794 observed reflections with I 〉 2σ（I）. Complex 1 features a 3D framework formed by Ag（I）-carboxylate chains containing [Ag16（COO）16] secondary building block. Furthermore, thermal stability and electrochemical property of 1 are also investigated in detail.
基金supported by the National Natural Science Foundation of China(No.21273101 and 21302082)the Foundation of the Program for Backbone Teachers in Universities of Henan Province(No.2012GGJS158)
文摘Hydrothermal reactions of biphenyl-2,3,3A,5A-tetracarboxylic acid（H4bptc） with cobalt salt in the presence of 1,4-bis（2-pyridylmethyl）piperazin（bpmp） afforded one novel coordination polymer, namely, [Co（H2bptc）（bpmp）0.5（H2O）]n（1）. Its structure was established by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, IR spectra and TG analysis. Complex 1 crystallizes in monoclinic, space group P21/c with a = 11.4839（11）, b = 16.6690（16）, c = 11.5559（11） A, V = 2201.8（4） A3, Mr = 539.35, Dc = 1.627 g/cm^3, μ（MoK α） = 0.841 mm-1, F（000） = 1108, Z = 4, the final R = 0.0309 and w R = 0.0705 for 4090 observed reflections（I 2σ（I））. Complex 1 displays a one-dimensional（1D） chain bridged by bpmp. Two carboxylic groups of H4 bptc ligand adopt μ01-η1：η1 and μ1-η1：η coordination modes to bridge adjacent Co（Ⅱ） ions together with bpmp ligand to give alternately arranged left- and right-handed helical chains. In addition, variable-temperature magnetic susceptibility measurements indicate that complex 1 shows weak antiferromagnetic interactions between the adjacent Co（Ⅱ） ions.
文摘化工、纺织印染与农药化肥等产业的蓬勃发展推动着人类社会的进步,但同时也给环境治理带来了巨大难题。目前,光催化降解局限于在特定波长下针对单一有机污染物进行降解,然而现实中的情况往往更复杂。因此,开发一种多功能光催化材料用于光催化降解不同有机污染物显得尤为重要。采用一步无模板溶剂热法合成了核壳结构的C-TiO_(2)复合材料前驱体,并在氩气气氛下煅烧得到高结晶度的C-TiO_(2)复合光催化材料。运用SEM、TEM、XRD和TG等表征手段对材料进行表征,结论如下:550℃煅烧时的样品为包含少量碳的高结晶度的锐钛矿相TiO 2,且550℃煅烧时的样品依然保持了完整的核壳结构。此外,C-TiO_(2)复合材料的比表面积高达85.69 m 2·g^(-1),平均孔径为16.4 nm以及孔体积为0.423 m 3·g^(-1)。在UV-Vis光照射下,C-TiO_(2)复合材料分别对罗丹明B(RhB)、亚甲基蓝(MB)和刚果红(CR)3种染料显示出增强的光催化降解活性。
