The title complex Pd（H2BDA）Cl2·2DMSO （C16H14Cl2N2O6PdS2, H2BDA = 2,2＇- bipyridine-3,3＇-dicarboxylic acid） has been synthesized and characterized by IR spectra, elemental analysis and ^1H NMR spectra. Its st...The title complex Pd（H2BDA）Cl2·2DMSO （C16H14Cl2N2O6PdS2, H2BDA = 2,2＇- bipyridine-3,3＇-dicarboxylic acid） has been synthesized and characterized by IR spectra, elemental analysis and ^1H NMR spectra. Its structure was determined by single-crystal X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P2（1/c） with a = 1.3604（6）, b = 1.2606（6）, c = 1.3521 （6） nm, β = 103.677（7）°, V = 2.2530（17） nm^3, Mr = 571.75, Z = 4, Dc = 1.686 g/cm^3,μ = 1.280 mm^-1, F（000） = 1136, R= 0.0405 and wR= 0.0908. The complex presents a planar quadrangle arrangement and is assembled via hydrogen bonds.展开更多
The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ra...The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.展开更多
A new compound, [Ni（Hdctrz）（H2O）4]（1, H3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid）, has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysi...A new compound, [Ni（Hdctrz）（H2O）4]（1, H3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid）, has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 6.871（1）, b = 11.468（1）, c = 12.178（1） A, b = 101.291（1）o, V = 941.01（16） A3, Z = 4, C4H9N3O8Ni, Mr = 285.85, Dc = 2.018 g·cm–3, m = 2.10 mm–1, F（000） = 584, GOOF = 1.025, the final R = 0.0515 and wR = 0.2125 for 1404 observed reflections（I 〉 2s（I））. The crystal structure is assembled by a slightly distorted {NiNO5} octahedral geometry and hydrogen bonds viz. N–H…O, O–H…O, C–O…π and π···π weak interactions. A rare π···π interaction from triazolate and carboxylate is affirmed through the molecular orbitals（MO） of three adjacent Ni CN molecules. The 3D Hirshfeld surface analysis was employed to gain additional insight into the interactions responsible for the packing of compound 1. Quantitative examination of 2D fingerprint plots revealed, amongst others, the dominating participation of O···H, N···H and π···π interactions in the molecular packing.展开更多
The title complex 1,{[CuEu（Hbidc）2（H2O）4]·H2O}n（H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid）,has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Comple...The title complex 1,{[CuEu（Hbidc）2（H2O）4]·H2O}n（H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid）,has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1,with a = 7.791（2）,b = 12.058（3）,c = 12.109（3）,α = 82.189（5）,β = 72.407（5）,γ = 89.184（4）°,V = 1073.7（5）3,C18H18CuEuN4O13,Mr = 713.86,Dc = 2.208 g/cm3,μ（MoKα） = 3.967 mm-1,F（000） = 700,GOOF = 0.950,Z = 2,the final R = 0.0531 and wR = 0.1068 for I 2σ（I）.Complex 1 possess a tape-like chain structure consisting of Eu2C8O4 and Cu2Eu2C18N4O4 metallic rings alternatively arranged and is the first 3d-4f heterometallic complex based on the 1H-ben-zimidazole-5,6-dicarboxylato ligand（Hbidc）.Plenty of hydrogen-bonding and π...π stacking interactions connect the 1D chains to construct a 3D supramolecular architecture.展开更多
A new metal-organic coordination polymer [Zn（pzdc）（mbix）]n·nH2O（H2pzdc = pyrazine-2,3- dicarboxylic acid, mbix = 1,3-bis（imidazol-1-ylmethyl）-benzene） 1 has been hydrothermally synthesized and structurall...A new metal-organic coordination polymer [Zn（pzdc）（mbix）]n·nH2O（H2pzdc = pyrazine-2,3- dicarboxylic acid, mbix = 1,3-bis（imidazol-1-ylmethyl）-benzene） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in monoclinic system, space group P21/n with a = 8.5519（6）, b = 14.8764（10）, c = 16.4108（11） A, β = 103.4520（10）o, V = 2030.5（2）A^3, C（20）H（18）N6O5Zn, Mr = 487.77, Dc = 1.596 g/cm^3, F（000） = 1000, Z = 4, μ（MoK α） = 1.257 mm^-1, the final R = 0.0260 and w R = 0.0706 for 3445 observed reflections（I 〉 2σ（I））. The structure of 1 exhibits a one-dimensional chain-like structure. In addition, natural bond orbital（NBO） analysis was performed by the PBE0/LANL2DZ method in Gaussian 03 Program. The calculation results show obvious covalent interaction between the coordinated atoms and Zn（Ⅱ） ion.展开更多
Recently,azobenzene-4,4'-dicarboxylic acid(ADCA)has been produced gradually for use as an organic synthesis or pharmaceutical intermediate due to its eminent performance.With large quantities put into application ...Recently,azobenzene-4,4'-dicarboxylic acid(ADCA)has been produced gradually for use as an organic synthesis or pharmaceutical intermediate due to its eminent performance.With large quantities put into application in the future,the thermal stability of this substance during storage,transportation,and use will become quite important.Thus,in this work,the thermal decomposition behavior,thermal decomposition kinetics,and thermal hazard of ADCA were investigated.Experiments were conducted by using a SENSYS evo DSC device.A combination of differential iso-conversion method,compensation parameter method,and nonlinear fitting evaluation were also used to analyze thermal kinetics and mechanism of ADCA decomposition.The results show that when conversion rate α increases,the activation energies of ADCA's first and main decomposition peaks fall.The amount of heat released during decomposition varies between 182.46 and 231.16 J·g^(-1).The proposed kinetic equation is based on the Avrami-Erofeev model,which is consistent with the decomposition progress.Applying the Frank-Kamenetskii model,a calculated self-accelerating decomposition temperature of 287.0℃is obtained.展开更多
Various 4-alkoxypyridine-2, 6-dicarboxylic acids were synthesized starting from 2, 6- lutidine. Through aldol condensation and Michael addition, various 4-arylpyridine-2, 6-dicarboxylic acids were synthesized starting...Various 4-alkoxypyridine-2, 6-dicarboxylic acids were synthesized starting from 2, 6- lutidine. Through aldol condensation and Michael addition, various 4-arylpyridine-2, 6-dicarboxylic acids were synthesized starting from aromatic aldehydes and 2-acetylfuran.展开更多
The structure of a zinc（Ⅱ） coordination complex（1）, [C14 H10 N3 O5 Zn1.5]n or [Zn1.5（bzim）（pydc）（H2 O）]n（H2 pydc = pyridine-2,3-dicarboxylic acid, Hbzim = benzimidazole）, has been determined by X-ray crys...The structure of a zinc（Ⅱ） coordination complex（1）, [C14 H10 N3 O5 Zn1.5]n or [Zn1.5（bzim）（pydc）（H2 O）]n（H2 pydc = pyridine-2,3-dicarboxylic acid, Hbzim = benzimidazole）, has been determined by X-ray crystallography and characterized by elemental analysis, IR spectrum and luminescence. Chemical formula： C14 H10 N3 O5 Zn1.5. It crystallizes in the monoclinic system, space group P21/c with a = 12.303（4）, b = 12.052（4）, c = 10.212（3） ？, β = 104.147（4）, V = 1468.3（8） ？3, Z = 4, Mr = 398.30, Dc = 1.802 g/cm3, F（000） = 800, μ = 2.501 mm-1 and S = 1.000. The 2-D network architecture of 1 is constructed from benzimidazole, zinc and pyridine-2,3-dicarboxylic acid. The quantum-chemical calculations have been performed on ‘molecular fragments’ extracted from the crystal structure using the B3 LYP method in Gaussian 09. The luminescence spectrum shows that complex 1 emits blue luminescence.展开更多
A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- ...A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.展开更多
A new metal-organic coordination polymer [Zn2（trz）2（mpda）（H2O）]n（1, trz = 1,2,4-triazole, H2 mpda = 2,6-dimethylpyridine-3,5-dicarboxylic acid） was synthesized and characterized by single-crystal X-ray analyse...A new metal-organic coordination polymer [Zn2（trz）2（mpda）（H2O）]n（1, trz = 1,2,4-triazole, H2 mpda = 2,6-dimethylpyridine-3,5-dicarboxylic acid） was synthesized and characterized by single-crystal X-ray analyses. The crystal is of monoclinic system, space group P21/n, a = 9.619（3）, b = 8.920（3）, c = 22.159（6）, β = 96.897（4）°, V = 1887.3（9）3, Z = 4, Mr = 478.04, D3 c = 1.682 Mg/m, F（000） = 960, the final R = 0.0264 and wR = 0.0870（I 2σ（I））. Compound 1 consists of {[Zn4（trz）4]4＋}n layers, which are further connected by mpda2- to complete a three-dimensional structure. The title compound exhibits luminescence at λmax = 415 nm upon excitation at 364 nm.展开更多
基金This project was supported by the Science Foundation of Shenyang Institute of Chemical Technology, National Science Foundation for Post-doctoral and Corporation Post-doctoral Foundation of Liaoning Province
文摘The title complex Pd（H2BDA）Cl2·2DMSO （C16H14Cl2N2O6PdS2, H2BDA = 2,2＇- bipyridine-3,3＇-dicarboxylic acid） has been synthesized and characterized by IR spectra, elemental analysis and ^1H NMR spectra. Its structure was determined by single-crystal X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P2（1/c） with a = 1.3604（6）, b = 1.2606（6）, c = 1.3521 （6） nm, β = 103.677（7）°, V = 2.2530（17） nm^3, Mr = 571.75, Z = 4, Dc = 1.686 g/cm^3,μ = 1.280 mm^-1, F（000） = 1136, R= 0.0405 and wR= 0.0908. The complex presents a planar quadrangle arrangement and is assembled via hydrogen bonds.
基金The project was supported by the Natural Science Foundation of Jilin Province (No. 20060516)the Doctoral Foundation of Jilin Normal University (No. 2006006)+1 种基金the Science and Technology Institute Foundation of Siping City (No. 2005016)the Subject and Base Construction Foundation of Jilin Normal University (No. 2006041)
文摘The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.
基金Supported by the National Natural Science Foundation of China(No.21571118)Shanxi Scholarship Council of China(2013-026)
文摘A new compound, [Ni（Hdctrz）（H2O）4]（1, H3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid）, has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 6.871（1）, b = 11.468（1）, c = 12.178（1） A, b = 101.291（1）o, V = 941.01（16） A3, Z = 4, C4H9N3O8Ni, Mr = 285.85, Dc = 2.018 g·cm–3, m = 2.10 mm–1, F（000） = 584, GOOF = 1.025, the final R = 0.0515 and wR = 0.2125 for 1404 observed reflections（I 〉 2s（I））. The crystal structure is assembled by a slightly distorted {NiNO5} octahedral geometry and hydrogen bonds viz. N–H…O, O–H…O, C–O…π and π···π weak interactions. A rare π···π interaction from triazolate and carboxylate is affirmed through the molecular orbitals（MO） of three adjacent Ni CN molecules. The 3D Hirshfeld surface analysis was employed to gain additional insight into the interactions responsible for the packing of compound 1. Quantitative examination of 2D fingerprint plots revealed, amongst others, the dominating participation of O···H, N···H and π···π interactions in the molecular packing.
基金Supported by the Nanjing University of Posts and Telecommunications(No.NY209032)the National Natural Science Foundation of China(No.21001065)the Major State Basic Research Development Program of China (973 Program,No.2009CB930600)
文摘The title complex 1,{[CuEu（Hbidc）2（H2O）4]·H2O}n（H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid）,has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1,with a = 7.791（2）,b = 12.058（3）,c = 12.109（3）,α = 82.189（5）,β = 72.407（5）,γ = 89.184（4）°,V = 1073.7（5）3,C18H18CuEuN4O13,Mr = 713.86,Dc = 2.208 g/cm3,μ（MoKα） = 3.967 mm-1,F（000） = 700,GOOF = 0.950,Z = 2,the final R = 0.0531 and wR = 0.1068 for I 2σ（I）.Complex 1 possess a tape-like chain structure consisting of Eu2C8O4 and Cu2Eu2C18N4O4 metallic rings alternatively arranged and is the first 3d-4f heterometallic complex based on the 1H-ben-zimidazole-5,6-dicarboxylato ligand（Hbidc）.Plenty of hydrogen-bonding and π...π stacking interactions connect the 1D chains to construct a 3D supramolecular architecture.
基金supported by the Science and Technology Development Project of Jilin Provincial Science&Technology Department(201205080)the Science and Technology Research Projects of the Education Office of Jilin Province(No.2013.384)
文摘A new metal-organic coordination polymer [Zn（pzdc）（mbix）]n·nH2O（H2pzdc = pyrazine-2,3- dicarboxylic acid, mbix = 1,3-bis（imidazol-1-ylmethyl）-benzene） 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in monoclinic system, space group P21/n with a = 8.5519（6）, b = 14.8764（10）, c = 16.4108（11） A, β = 103.4520（10）o, V = 2030.5（2）A^3, C（20）H（18）N6O5Zn, Mr = 487.77, Dc = 1.596 g/cm^3, F（000） = 1000, Z = 4, μ（MoK α） = 1.257 mm^-1, the final R = 0.0260 and w R = 0.0706 for 3445 observed reflections（I 〉 2σ（I））. The structure of 1 exhibits a one-dimensional chain-like structure. In addition, natural bond orbital（NBO） analysis was performed by the PBE0/LANL2DZ method in Gaussian 03 Program. The calculation results show obvious covalent interaction between the coordinated atoms and Zn（Ⅱ） ion.
基金supported by National Natural Science Foundation of China(51974166).
文摘Recently,azobenzene-4,4'-dicarboxylic acid(ADCA)has been produced gradually for use as an organic synthesis or pharmaceutical intermediate due to its eminent performance.With large quantities put into application in the future,the thermal stability of this substance during storage,transportation,and use will become quite important.Thus,in this work,the thermal decomposition behavior,thermal decomposition kinetics,and thermal hazard of ADCA were investigated.Experiments were conducted by using a SENSYS evo DSC device.A combination of differential iso-conversion method,compensation parameter method,and nonlinear fitting evaluation were also used to analyze thermal kinetics and mechanism of ADCA decomposition.The results show that when conversion rate α increases,the activation energies of ADCA's first and main decomposition peaks fall.The amount of heat released during decomposition varies between 182.46 and 231.16 J·g^(-1).The proposed kinetic equation is based on the Avrami-Erofeev model,which is consistent with the decomposition progress.Applying the Frank-Kamenetskii model,a calculated self-accelerating decomposition temperature of 287.0℃is obtained.
文摘Various 4-alkoxypyridine-2, 6-dicarboxylic acids were synthesized starting from 2, 6- lutidine. Through aldol condensation and Michael addition, various 4-arylpyridine-2, 6-dicarboxylic acids were synthesized starting from aromatic aldehydes and 2-acetylfuran.
基金Supported by the Jilin Province Science and Technology Development Plan Item(No.20140204080GX)the Project of the Education Department of Jilin Province,China(No.JJKH20180777KJ)the Science and Technology Development Projects of Siping City(No.2017057)
文摘The structure of a zinc（Ⅱ） coordination complex（1）, [C14 H10 N3 O5 Zn1.5]n or [Zn1.5（bzim）（pydc）（H2 O）]n（H2 pydc = pyridine-2,3-dicarboxylic acid, Hbzim = benzimidazole）, has been determined by X-ray crystallography and characterized by elemental analysis, IR spectrum and luminescence. Chemical formula： C14 H10 N3 O5 Zn1.5. It crystallizes in the monoclinic system, space group P21/c with a = 12.303（4）, b = 12.052（4）, c = 10.212（3） ？, β = 104.147（4）, V = 1468.3（8） ？3, Z = 4, Mr = 398.30, Dc = 1.802 g/cm3, F（000） = 800, μ = 2.501 mm-1 and S = 1.000. The 2-D network architecture of 1 is constructed from benzimidazole, zinc and pyridine-2,3-dicarboxylic acid. The quantum-chemical calculations have been performed on ‘molecular fragments’ extracted from the crystal structure using the B3 LYP method in Gaussian 09. The luminescence spectrum shows that complex 1 emits blue luminescence.
基金This work was supported by the Science and Technology Bureau of Jinhua City (No 2003-01-179)
文摘A novel pyrazine-2,3-dicarboxylic acid bridged Co(II) phen complex 2 ∞ [Co- (phen)(μ-L)3/3]?H2O (H2L = pyrazine-2,3-dicarboxylic acid) has been hydrothermally synthesized, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group P21/n with a = 11.480(2), b = 11.885(2), c = 12.939(3) ?, β = 110.55(3)°, V = 1653.1(6) ?3, Mr = 423.25, Dc = 0.425 g/cm3, Z = 4, R = 0.0361 and wR = 0.1011. The title complex consists of 2D 2 ∞ [Co(phen)(μ-L)3/3] layers and crystal water molecules. Each Co atom is octahedrally coordinated by three N atoms and three O atoms to form 2D 2 ∞ [Co(phen)(μ-L)3/3] polymeric layers. Furthermore, such 2D layers are stacked into 3D supramolecular frameworks via Van der Waals’ intermolecular forces, strong and weak hydrogen-bond interactions. The coordination phen and crystal water molecules are resided into cavities of the frameworks.
基金Supported by the Science and Technology Projects of Chongqing Municipal Education Commission(KJ120663,KJ100602,KJ120632,KJ130638)Chongqing Normal University Scientific Research Foundation Project(2011XLS30)Program for Innovation Team Building at Institutions of Higher Education in Chongqing(KJTD201309)
文摘A new metal-organic coordination polymer [Zn2（trz）2（mpda）（H2O）]n（1, trz = 1,2,4-triazole, H2 mpda = 2,6-dimethylpyridine-3,5-dicarboxylic acid） was synthesized and characterized by single-crystal X-ray analyses. The crystal is of monoclinic system, space group P21/n, a = 9.619（3）, b = 8.920（3）, c = 22.159（6）, β = 96.897（4）°, V = 1887.3（9）3, Z = 4, Mr = 478.04, D3 c = 1.682 Mg/m, F（000） = 960, the final R = 0.0264 and wR = 0.0870（I 2σ（I））. Compound 1 consists of {[Zn4（trz）4]4＋}n layers, which are further connected by mpda2- to complete a three-dimensional structure. The title compound exhibits luminescence at λmax = 415 nm upon excitation at 364 nm.
