This paper reports the synthesis and general properties of the new reagent CPFP. Its dissociation constants have been determined. The characterization in determinating total RE with CPAP reagent has been investigated ...This paper reports the synthesis and general properties of the new reagent CPFP. Its dissociation constants have been determined. The characterization in determinating total RE with CPAP reagent has been investigated in detail. Analytic data for synthetic sample are satisfactory.展开更多
The title compound, [Co（C7N2H7O2）2]n·nH2O 1, was synthesized via the hydrothermal reaction of Co（OAc）2 with 3,5-diaminobenzoic acid and characterized by elemental analysis and infrared spectra. The crystal cr...The title compound, [Co（C7N2H7O2）2]n·nH2O 1, was synthesized via the hydrothermal reaction of Co（OAc）2 with 3,5-diaminobenzoic acid and characterized by elemental analysis and infrared spectra. The crystal crystallizes in the monoclinic system, space group P21/c with a = 7.456（3）, b = 9.972（3）, c = 10.391（3）A, β= 106.435（2）°, V = 741.0（4） A^3, Z = 2, C14H16CoN4O5, Mr = 379.24, Dc = 1.700 g/cm^3, F（000） = 390 and μ（MoKa） = 1.194 mm^-l. The final R = 0.0324 and wR = 0.0886 for 1516 observed reflections with I 〉 2σ（I） and R = 0.0337 and wR = 0.0899 for all data. X-ray diffraction studies reveal that the title compound has an interesting 3D microporous architecture with guest water molecules inside the channel. Each Co atom, adopting a distorted octahedral geometry, is coordinated by two O atoms from two 3,5-diaminobenzoate ligands and four N atoms from four symmetry-related 3,5-diaminobenzoate ligands.展开更多
The title compound glycin.3,5-dihydroxybenzoic acid （GDB） has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513（10）, b = 4.668...The title compound glycin.3,5-dihydroxybenzoic acid （GDB） has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513（10）, b = 4.668（2）, c = 9.150（4） A°, Z= 4, V= 1089.8（8） A°^3, C9H13NO7, Mr= 247.20, Dc = 1.507 g/m^3,/z（MoKa） = 0.132 mm^-1, F（000） = 520, R1 = 0.0322 and wR2 = 0.0611 for 885 observed reflections （I 〉 2σ（I））. The title compound is a 1：1 molecular complex of glycin and 3,5-dihydroxybenzoic acid, which is linked by O-H…O and N-H…O hydrogen bonds to form a three-dimensional framework. Test of SHG （second harmonic generation） indicates that NLO generation of the crystal is higher than that of KDP.展开更多
Two novel zinc（Ⅱ） coordination polymers, [Zn2（BCB）（CH3OH）（μ3-OH）]n（1） and {[Zn2（BCB）（μ3-OH）（H2O）2]·CH3OH}n （2）, have been constructed from 3,5-bis（2-carboxylphenoxy）benzoic acid（H3BCB） an...Two novel zinc（Ⅱ） coordination polymers, [Zn2（BCB）（CH3OH）（μ3-OH）]n（1） and {[Zn2（BCB）（μ3-OH）（H2O）2]·CH3OH}n （2）, have been constructed from 3,5-bis（2-carboxylphenoxy）benzoic acid（H3BCB） and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. Structural analysis reveals that complexes 1 and 2 are both 1D polymeric chains with unprecedented tetranuclear {Zn4（COO）4（μ3-OH）2} clusters, which were further expanded into a 2D structure. Fluorescence measurements show that 1 and 2 have highly selective and sensitive detection of nitrobenzene.展开更多
Two coordination compounds, namely [Ce（3,5-Br2BC）3（3,5-HBrzBC）]n （1） and [Zn（3,5-Br2BC）2（phen）] （2, 3,5-HBr2BC = 3,5-dibromobenzoic acid, phen = 1,10-phenanthroline）, were assembled. Single-crystal X-ray d...Two coordination compounds, namely [Ce（3,5-Br2BC）3（3,5-HBrzBC）]n （1） and [Zn（3,5-Br2BC）2（phen）] （2, 3,5-HBr2BC = 3,5-dibromobenzoic acid, phen = 1,10-phenanthroline）, were assembled. Single-crystal X-ray diffraction studies show that compound 1 possesses a ID chain coordination network, which is further extended into a 3D supramolecular architecture via Br..＇Br and Br＇＂O halogen bonding. Compound 2 consists of a mononuclear molecule, which is assembled to a 3D supramolecular framework through C-H..-O hydrogen bond, π-π stacking interactions and Br..π halogen bonding. Luminescent and magnetic properties of both compounds have also been studied.展开更多
In this work, we report a new two-dimensional Sr（II） coordination polymer, namely, [Sr（L）（phen）（H20）] （1）, based on 3,5-dinitro-salicylic acid （H2L） and 1,10-phenanthroline （phen）. It crystallizes in mon...In this work, we report a new two-dimensional Sr（II） coordination polymer, namely, [Sr（L）（phen）（H20）] （1）, based on 3,5-dinitro-salicylic acid （H2L） and 1,10-phenanthroline （phen）. It crystallizes in monoclinic, space group P2/1 with a = 15.479（3）, b = 9.4020（19）, c = 13.884（3）/k, β= 103.76（3）°, V= 1962.5（7） A3, Z = 4, C19H12SrN4O8, Mr = 511.95, Dc = 1.733 g/cm^3, F（000） = 1024,μ（MoKa） = 2.805 mm^-1, R = 0.0411 and wR = 0.1069. In 1, each L anion bridges three Sr（II） atoms by using carboxylate and hydroxyl groups, yielding a two-dimensional layer structure. The phen ligands are alternately attached to both sides of the layer. The π-π stacking between L and phen in the same layer and hydrogen-bonding interactions between water molecule and carboxylate oxygen atom play an important role in stabilizing the layer structure of 1. The solid state luminescent property of 1 was also studied at room temperature.展开更多
One new organic adduct,isonicotinamide·3,5-dinitrosalicylic acid with isonico-tin-amide（ina） and 3,5-dinitrosalicylic acid（3,5-dnsa） in 1：1 molar ratio,has been synthesized.Its struc-ture（C13H10N4O8,Mr = 35...One new organic adduct,isonicotinamide·3,5-dinitrosalicylic acid with isonico-tin-amide（ina） and 3,5-dinitrosalicylic acid（3,5-dnsa） in 1：1 molar ratio,has been synthesized.Its struc-ture（C13H10N4O8,Mr = 350.25） was characterized by elemental analysis,IR and single-crystal X-ray diffraction analysis.The crystal belongs to the triclinic system,space group P1,with a = 8.812（4）,b = 9.487（5）,c = 9.604（6） ,α = 116.54（2）,β = 97.29（5）,γ = 98.35（4）°,V = 693.8（7） 3,Z = 2,Dc = 1.677 g/cm3,λ（MoKα） = 0.71073 ,μ = 0.142 mm-1,F（000） = 360,the final R = 0.0539 and wR = 0.1402 for 2417 unique reflections（Rint = 0.0288） with 1819 observed ones（Ⅰ 〉 2σ（Ⅰ））.Proton transfer reaction occurs between 3,5-dnsa and ina molecules,and the hydrogen bonds（N-H…O and C-H…O） with other interactions（π…π stacking and weak interactions of O…O and C…O） cooperatively construct a three-dimensional（3D） supramolecular structure.展开更多
The title adduct （C9H11N3O6, Mr= 257.21） was synthesized and it crystallizes in orthorhombic, space group P212121 with a = 5.8835（19）, b =9.517（3）, c = 20.399（6） A, V= 1142.2（6） ,A^3 Z = 4, Dc= 1.496 g/cm^3...The title adduct （C9H11N3O6, Mr= 257.21） was synthesized and it crystallizes in orthorhombic, space group P212121 with a = 5.8835（19）, b =9.517（3）, c = 20.399（6） A, V= 1142.2（6） ,A^3 Z = 4, Dc= 1.496 g/cm^3, F（000） = 536,μ（MoKα） = 0.128 mm^-1, the final R = 0.0396 and wR = 0.0800 for 1047 observed reflections with I 〉 2σ（I）. The compound is a 1：1 adduct of dimethylamine and 3,5-dinitrobenzoic acid which are linked by hydrogen bonds to form a two-dimensional network. The dimethylamine is protonated at the nitrogen atom with the proton from the carboxyl of 3,5- dinitrobenzoic acid.展开更多
3,5-Dimethoxyhomophthalic acid was synthesized in four steps from 3,5-dimethoxycinnamic acid via a series of reactions including cyclization of 3-（3＇,5＇-dimethoxyphenyl）propionic acid to 5,7-dimethoxy-1-indanone a...3,5-Dimethoxyhomophthalic acid was synthesized in four steps from 3,5-dimethoxycinnamic acid via a series of reactions including cyclization of 3-（3＇,5＇-dimethoxyphenyl）propionic acid to 5,7-dimethoxy-1-indanone and oxidative decomposition of methyl-2-hydroxy-2-[5,7-dimethyoxy-1-oxo-1H-inden-2（3H）-ylidene]acetate to 3,5-dimethoxyhomophthalic acid.The synthesized compounds were characterized by elemental analysis,IR,1H NMR,and MS.The biological evaluation experiments of 3,5-dimthoxyhomophthalic acid and the related synthesized compounds were also carried out.Naturally occurring biologically active isocoumarins were prepared in a single step by the condensation of the homophthalic acid with appropriate acid chlorides.展开更多
The title compound nicotinic acid3,5-dinitrobenzoic acid (NDNT) has been obtained by the reaction of nicotinic acid with 3,5-dinitrobenzoic acid in deionic water at room temperature. The crystal is of monoclinic, spac...The title compound nicotinic acid3,5-dinitrobenzoic acid (NDNT) has been obtained by the reaction of nicotinic acid with 3,5-dinitrobenzoic acid in deionic water at room temperature. The crystal is of monoclinic, space group P21/n with a = 14.053(6), b = 5.046(2), c = 20.105(8) ? ?= 103.573(8)? C13H9N3O8, Mr = 335.23, Z = 4, V = 1385.8(10) 3, Dc = 1.607 g/cm3, (MoK? = 0.137 mm-1, F(000) = 688, R = 0.0435 and wR = 0.0993 for 1239 observed reflections (I > 2(I)). In the crystals, the asymmetric unit contains one nicotinic acid (C6H5NO2) and one 3,5- dinitrobenzoic acid (C7H4N2O6) molecules which are linked by some hydrogen bonds to form a twenty-membered hydrogen-bonded ring and an extended linear structure.展开更多
Three stable coordination polymers(CPs) assembled by 3,5-(carboxybenzyloxy)-benzoic acid(H3 L) and 1,10-phenanthroline(phen), namely, [Zn(HL)(phen)]n(1), [Cd(HL)(phen)]_n(2) and [Co(HL)(phen)]_n(3), have been synthesi...Three stable coordination polymers(CPs) assembled by 3,5-(carboxybenzyloxy)-benzoic acid(H3 L) and 1,10-phenanthroline(phen), namely, [Zn(HL)(phen)]n(1), [Cd(HL)(phen)]_n(2) and [Co(HL)(phen)]_n(3), have been synthesized under hydrothermal conditions. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, infrared(IR) spectroscopy and powder X-ray diffraction(PXRD). Investigation on crystal structure indicates that complexes 1 ～ 3 exhibit similar architecture. In these complexes, metal ions coordinate with H3 L and phen ligands, forming infinite 1 D chains. Then the adjacent chains combine together through intramolecular hydrogen-bonding interactions, generating 2 D supramolecular architectures. In addition, complexes 1～3 present excellent thermal stabilities and 1 and 2 exhibit strong luminescent emission bands at room temperature.展开更多
The title compound （C2H7NO·C7H4N2O6） has been obtained by the reaction of ethanolamine with 3,5-dinitrobenzoic acid in deionized water at room temperature. The crystal crystallizes in orthorhombic, space group ...The title compound （C2H7NO·C7H4N2O6） has been obtained by the reaction of ethanolamine with 3,5-dinitrobenzoic acid in deionized water at room temperature. The crystal crystallizes in orthorhombic, space group P212121 with a = 6.048（2）, b = 9.146（3）, c = 21.955（7） A^°, C9H11N3O7, Mr = 273.21, Z = 4, V= 1214.3（7） , A^°3, Dc = 1.494 g/cm^3, F（000） = 568,μ（MoKα） = 0.131 mm^-1, R1 = 0.0338 and wR2 = 0.0497. The new organic adduct is composed of one ethanolamine and one 3,5-dinitrobenzoic acid, which are linked up by O-H…O and N-H…O types of hydrogen bonds to form a nine-membered ring and an eleven-membered ring, extending into a one-dimensional network structure.展开更多
文摘This paper reports the synthesis and general properties of the new reagent CPFP. Its dissociation constants have been determined. The characterization in determinating total RE with CPAP reagent has been investigated in detail. Analytic data for synthetic sample are satisfactory.
基金Supported by the National Natural Science Foundation of China (29733090 and 20173063), the State Key Basic Research and Development Plan of China (001CB108906), Key Project in KIP of CAS (KJCX2-H3) and the NSF of Fujian Province (E0020001)
文摘The title compound, [Co（C7N2H7O2）2]n·nH2O 1, was synthesized via the hydrothermal reaction of Co（OAc）2 with 3,5-diaminobenzoic acid and characterized by elemental analysis and infrared spectra. The crystal crystallizes in the monoclinic system, space group P21/c with a = 7.456（3）, b = 9.972（3）, c = 10.391（3）A, β= 106.435（2）°, V = 741.0（4） A^3, Z = 2, C14H16CoN4O5, Mr = 379.24, Dc = 1.700 g/cm^3, F（000） = 390 and μ（MoKa） = 1.194 mm^-l. The final R = 0.0324 and wR = 0.0886 for 1516 observed reflections with I 〉 2σ（I） and R = 0.0337 and wR = 0.0899 for all data. X-ray diffraction studies reveal that the title compound has an interesting 3D microporous architecture with guest water molecules inside the channel. Each Co atom, adopting a distorted octahedral geometry, is coordinated by two O atoms from two 3,5-diaminobenzoate ligands and four N atoms from four symmetry-related 3,5-diaminobenzoate ligands.
文摘The title compound glycin.3,5-dihydroxybenzoic acid （GDB） has been synthesized and characterized by single-crystal X-ray analysis. It crystallizes in orthorhombic, space group Pca21 with a = 25.513（10）, b = 4.668（2）, c = 9.150（4） A°, Z= 4, V= 1089.8（8） A°^3, C9H13NO7, Mr= 247.20, Dc = 1.507 g/m^3,/z（MoKa） = 0.132 mm^-1, F（000） = 520, R1 = 0.0322 and wR2 = 0.0611 for 885 observed reflections （I 〉 2σ（I））. The title compound is a 1：1 molecular complex of glycin and 3,5-dihydroxybenzoic acid, which is linked by O-H…O and N-H…O hydrogen bonds to form a three-dimensional framework. Test of SHG （second harmonic generation） indicates that NLO generation of the crystal is higher than that of KDP.
基金supported by the Foundation of State Key Laboratory of Coal Conversion(No.J17-18-611)the National Natural Science Foundation of China(No.21676258)
文摘Two novel zinc（Ⅱ） coordination polymers, [Zn2（BCB）（CH3OH）（μ3-OH）]n（1） and {[Zn2（BCB）（μ3-OH）（H2O）2]·CH3OH}n （2）, have been constructed from 3,5-bis（2-carboxylphenoxy）benzoic acid（H3BCB） and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. Structural analysis reveals that complexes 1 and 2 are both 1D polymeric chains with unprecedented tetranuclear {Zn4（COO）4（μ3-OH）2} clusters, which were further expanded into a 2D structure. Fluorescence measurements show that 1 and 2 have highly selective and sensitive detection of nitrobenzene.
基金supported by the Natural Science Foundation of Shanxi Province(No.2013011011-6)the Subject Team of Taiyuan University of Science and Technology
文摘Two coordination compounds, namely [Ce（3,5-Br2BC）3（3,5-HBrzBC）]n （1） and [Zn（3,5-Br2BC）2（phen）] （2, 3,5-HBr2BC = 3,5-dibromobenzoic acid, phen = 1,10-phenanthroline）, were assembled. Single-crystal X-ray diffraction studies show that compound 1 possesses a ID chain coordination network, which is further extended into a 3D supramolecular architecture via Br..＇Br and Br＇＂O halogen bonding. Compound 2 consists of a mononuclear molecule, which is assembled to a 3D supramolecular framework through C-H..-O hydrogen bond, π-π stacking interactions and Br..π halogen bonding. Luminescent and magnetic properties of both compounds have also been studied.
基金Supported by the Institute Foundation of Siping City(No.2013036)
文摘In this work, we report a new two-dimensional Sr（II） coordination polymer, namely, [Sr（L）（phen）（H20）] （1）, based on 3,5-dinitro-salicylic acid （H2L） and 1,10-phenanthroline （phen）. It crystallizes in monoclinic, space group P2/1 with a = 15.479（3）, b = 9.4020（19）, c = 13.884（3）/k, β= 103.76（3）°, V= 1962.5（7） A3, Z = 4, C19H12SrN4O8, Mr = 511.95, Dc = 1.733 g/cm^3, F（000） = 1024,μ（MoKa） = 2.805 mm^-1, R = 0.0411 and wR = 0.1069. In 1, each L anion bridges three Sr（II） atoms by using carboxylate and hydroxyl groups, yielding a two-dimensional layer structure. The phen ligands are alternately attached to both sides of the layer. The π-π stacking between L and phen in the same layer and hydrogen-bonding interactions between water molecule and carboxylate oxygen atom play an important role in stabilizing the layer structure of 1. The solid state luminescent property of 1 was also studied at room temperature.
基金supported by the National Natural Science Foundation of China (No. 50872057)
文摘One new organic adduct,isonicotinamide·3,5-dinitrosalicylic acid with isonico-tin-amide（ina） and 3,5-dinitrosalicylic acid（3,5-dnsa） in 1：1 molar ratio,has been synthesized.Its struc-ture（C13H10N4O8,Mr = 350.25） was characterized by elemental analysis,IR and single-crystal X-ray diffraction analysis.The crystal belongs to the triclinic system,space group P1,with a = 8.812（4）,b = 9.487（5）,c = 9.604（6） ,α = 116.54（2）,β = 97.29（5）,γ = 98.35（4）°,V = 693.8（7） 3,Z = 2,Dc = 1.677 g/cm3,λ（MoKα） = 0.71073 ,μ = 0.142 mm-1,F（000） = 360,the final R = 0.0539 and wR = 0.1402 for 2417 unique reflections（Rint = 0.0288） with 1819 observed ones（Ⅰ 〉 2σ（Ⅰ））.Proton transfer reaction occurs between 3,5-dnsa and ina molecules,and the hydrogen bonds（N-H…O and C-H…O） with other interactions（π…π stacking and weak interactions of O…O and C…O） cooperatively construct a three-dimensional（3D） supramolecular structure.
基金This work was supported by the National Natural Science Foundation of China (50572040)
文摘The title adduct （C9H11N3O6, Mr= 257.21） was synthesized and it crystallizes in orthorhombic, space group P212121 with a = 5.8835（19）, b =9.517（3）, c = 20.399（6） A, V= 1142.2（6） ,A^3 Z = 4, Dc= 1.496 g/cm^3, F（000） = 536,μ（MoKα） = 0.128 mm^-1, the final R = 0.0396 and wR = 0.0800 for 1047 observed reflections with I 〉 2σ（I）. The compound is a 1：1 adduct of dimethylamine and 3,5-dinitrobenzoic acid which are linked by hydrogen bonds to form a two-dimensional network. The dimethylamine is protonated at the nitrogen atom with the proton from the carboxyl of 3,5- dinitrobenzoic acid.
基金Supported by Higher Education Commission of Pakistan,the National Basic Research Program of China(No.2003CB114402)the National Natrual Science Foundation of China(No.20672062)the Tianjin Natural Science Foundation(No.07JCYBJC01200).
文摘3,5-Dimethoxyhomophthalic acid was synthesized in four steps from 3,5-dimethoxycinnamic acid via a series of reactions including cyclization of 3-（3＇,5＇-dimethoxyphenyl）propionic acid to 5,7-dimethoxy-1-indanone and oxidative decomposition of methyl-2-hydroxy-2-[5,7-dimethyoxy-1-oxo-1H-inden-2（3H）-ylidene]acetate to 3,5-dimethoxyhomophthalic acid.The synthesized compounds were characterized by elemental analysis,IR,1H NMR,and MS.The biological evaluation experiments of 3,5-dimthoxyhomophthalic acid and the related synthesized compounds were also carried out.Naturally occurring biologically active isocoumarins were prepared in a single step by the condensation of the homophthalic acid with appropriate acid chlorides.
文摘The title compound nicotinic acid3,5-dinitrobenzoic acid (NDNT) has been obtained by the reaction of nicotinic acid with 3,5-dinitrobenzoic acid in deionic water at room temperature. The crystal is of monoclinic, space group P21/n with a = 14.053(6), b = 5.046(2), c = 20.105(8) ? ?= 103.573(8)? C13H9N3O8, Mr = 335.23, Z = 4, V = 1385.8(10) 3, Dc = 1.607 g/cm3, (MoK? = 0.137 mm-1, F(000) = 688, R = 0.0435 and wR = 0.0993 for 1239 observed reflections (I > 2(I)). In the crystals, the asymmetric unit contains one nicotinic acid (C6H5NO2) and one 3,5- dinitrobenzoic acid (C7H4N2O6) molecules which are linked by some hydrogen bonds to form a twenty-membered hydrogen-bonded ring and an extended linear structure.
基金Supported by the NNSFC(No.21576112)NSF of Jilin Province(20180623042TC,20180101181JC,20150623024TC-19)+2 种基金the Project of Education Department of Jilin Province(JJKH20180775KJ)the Project of Human Resources and Social Security Department of Jilin Province(2017956)the Opening Project of Key Laboratory of Polyoxometalate Science of Ministry of Education
文摘Three stable coordination polymers(CPs) assembled by 3,5-(carboxybenzyloxy)-benzoic acid(H3 L) and 1,10-phenanthroline(phen), namely, [Zn(HL)(phen)]n(1), [Cd(HL)(phen)]_n(2) and [Co(HL)(phen)]_n(3), have been synthesized under hydrothermal conditions. Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, infrared(IR) spectroscopy and powder X-ray diffraction(PXRD). Investigation on crystal structure indicates that complexes 1 ～ 3 exhibit similar architecture. In these complexes, metal ions coordinate with H3 L and phen ligands, forming infinite 1 D chains. Then the adjacent chains combine together through intramolecular hydrogen-bonding interactions, generating 2 D supramolecular architectures. In addition, complexes 1～3 present excellent thermal stabilities and 1 and 2 exhibit strong luminescent emission bands at room temperature.
基金This project was supported by the Innovation Foundation for College Students of Nankai University
文摘The title compound （C2H7NO·C7H4N2O6） has been obtained by the reaction of ethanolamine with 3,5-dinitrobenzoic acid in deionized water at room temperature. The crystal crystallizes in orthorhombic, space group P212121 with a = 6.048（2）, b = 9.146（3）, c = 21.955（7） A^°, C9H11N3O7, Mr = 273.21, Z = 4, V= 1214.3（7） , A^°3, Dc = 1.494 g/cm^3, F（000） = 568,μ（MoKα） = 0.131 mm^-1, R1 = 0.0338 and wR2 = 0.0497. The new organic adduct is composed of one ethanolamine and one 3,5-dinitrobenzoic acid, which are linked up by O-H…O and N-H…O types of hydrogen bonds to form a nine-membered ring and an eleven-membered ring, extending into a one-dimensional network structure.
