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
By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid（H2FDA） ligand and 4,4＇-bipyridine（bipy）, [Cu（FDA）（4,4＇-bipy）（DMF）]n·solvent（1） and {[Zn（4,4＇-b...By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid（H2FDA） ligand and 4,4＇-bipyridine（bipy）, [Cu（FDA）（4,4＇-bipy）（DMF）]n·solvent（1） and {[Zn（4,4＇-bipy）（FDA）（DMF）]·DMF}n（2）, were produced and characterized by single-crystal X-ray diffraction analyses, elemental analyses, IR and powder X-ray diffraction. Compound 1 crystallizes in monoclinic space group P21/c with a = 11.104（2）, b = 10.396（2）, c = 18.772（4） , β = 96.20（3）o, V = 2154.2（7） 3, Dc = 1.378 g/cm^3, C19H17 Cu N3O6, Mr = 446.90, F（000） = 916, μ（Mo Kα） = 1.05 mm^-1, Z = 4, R = 0.0691 and wR = 0.1341 for 3537 observed reflections（I 2σ（I））, and R = 0.1062 and w R = 0.1482 for all data. Compound 2 crystallizes in monoclinic space group C2/c with a = 29.779（6）, b = 9.6417（19）, c = 17.292（3）, β = 105.69（3）°, V = 4779.9（16） 3, Dc = 1.445 g/cm^3, C22H22N4O7 Zn, Mr = 519.81, F（000） = 2144, μ（Mo Kα）= 1.08 mm^-1, Z = 8, R = 0.0641 and w R = 0.1007 for 2985 observed reflections（I 2σ（I））, and R = 0.1028 and w R = 0.1112 for all data. Different coordination geometry of metal ions, square pyramid of Cu2＋ and trigonal bipyramid of Zn2＋, bring about different orientations of FDA2- ligands as well as 4,4＇-bipyridine ligands, and furthermore distinct assembly structures for 1 and 2. The thermal stabilities of 1 and 2 are also investigated.展开更多
Fourier-transform infrared（FTIR）,Raman and ultraviolet-visible spectra of 4,4＇-bipyridine and its me-tal-organic coordination compounds synthesized from 4,4＇-bipyridine and nitrate of Co（Ⅱ）,Ni（Ⅱ） and Zn（Ⅱ...Fourier-transform infrared（FTIR）,Raman and ultraviolet-visible spectra of 4,4＇-bipyridine and its me-tal-organic coordination compounds synthesized from 4,4＇-bipyridine and nitrate of Co（Ⅱ）,Ni（Ⅱ） and Zn（Ⅱ） were measured and analyzed,respectively.The main FTIR and Raman bands were assigned in detail.The relationship between these characteristic bands and the structure of ligands and coordination compounds were discussed.展开更多
A new 3D metal-organic framework of {[Co3（IDC）2（bipy）2（py）2]·7H2O}n （1） was obtained by the hydrothermal reaction of Co（NO3）2·6H2O, imidazole-4,5-dicarboxylic acid （H3IDC）, 4,4＇-bipyridine （bip...A new 3D metal-organic framework of {[Co3（IDC）2（bipy）2（py）2]·7H2O}n （1） was obtained by the hydrothermal reaction of Co（NO3）2·6H2O, imidazole-4,5-dicarboxylic acid （H3IDC）, 4,4＇-bipyridine （bipy）, and pyridine （py）, and structurally characterized by elemental analysis, infrared spectroscopy, thermal gravimetric analysis, and single-crystal X-ray diffraction. X-ray diffraction crystal structural analysis reveals that it crystallizes in orthorhombic system, space group Pccn with a = 11.1040（3）, b = 19.8834（5）, c = 21.3025（5）, V = 4703.3（2）3, Mr = 1079.63, Z = 4, Dc = 1.525 Mg·m-3, F（000） = 2212, μ（CuKα） = 8.855 mm-1, the final R = 0.0331 and wR = 0.0713 for 2525 observed reflections with I ≥ 2σ（I）. In compound 1, each cobalt（II） ion is six-coordinated with a slightly distorted octahedral coordination geometry, and each μ3-IDC3- acts as a bridge to bond three neighboring Co（II） ions, leading to an infinite 2D network layer structure of [Co3（IDC）2]n with Kagomé lattice. The adjacent layers are further linked by μ2-bipy to form an infinite 3D layered-pillared framework architecture of [Co3（IDC）2（bipy）2（py）2]n.展开更多
A new complex [Cu2（sala）2（H20）2（4,4＇-bipy）]＇H20 （sala = N-（2-hydroxybenzyl）- D,L-alaninate, 4,4＇-bipy = 4,4＇-bipyridine） has been synthesized and characterized by elemental analysis, IR spectroscopy, the...A new complex [Cu2（sala）2（H20）2（4,4＇-bipy）]＇H20 （sala = N-（2-hydroxybenzyl）- D,L-alaninate, 4,4＇-bipy = 4,4＇-bipyridine） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in monoclinic system, space group C2/c with a = 42.44（3）, b = 10.416（8）, c = 15.487（13） ./k, fl = 97.455（14）°, C30H36Cu2N4O9, Mr = 723.71, V = 6789（9） A3, Dc = 1.416 g/cm3, Z = 8, F（000） = 2992, μ（MoKa） = 1.308 mm-1, R = 0.0493 and wR = 0.1004 for 4878 observed reflections （I 〉 2σ（I））. Structural analysis shows that each copper（II） atom displays a distorted square-based pyramidal coordination geometry with two oxygen atoms and one nitrogen atom from one N-（2-hydroxybenzyl）-D,L-alaninate, one nitrogen atom from 4,4＇-bipyridine ligand and one water molecule. 4,4＇-Bipyridine ligand bridges two Cu（II） ions to form a dinuclear compound. The molecular structure is extended into a one-dimensional wavy chain through hydrogen bonds. These 1D chains are further expanded into 2D networks through hydrogen bonds.展开更多
A new Zn（II） coordination polymer [Zn3（BTC）2（4,4＇-bpy）（CO）2]n （1, H3BTC = 1,3,5-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine） has been prepared through urothermal reaction of zinc nitrate hexahyd...A new Zn（II） coordination polymer [Zn3（BTC）2（4,4＇-bpy）（CO）2]n （1, H3BTC = 1,3,5-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine） has been prepared through urothermal reaction of zinc nitrate hexahydrate with 1,3,5-benzenetricarboxylic acid and 4,4＇-bipyridine, and characterized by elemental analysis, IR spectroscopy, TGA and powder XRD, and its crystal structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 10.262（3）, b = 18.838（5）, c = 15.083（4）/k, fl = 99.203（4）°, V = 2878.3（14） A3, C30H14Zn3N2O14, Mr= 822.54, Z = 4, Dc = 1.898 g/cm3,μ = 2.561 mm-1,F（000） = 1640, R = 0.0363 and wR = 0.0932 for 2828 observed reflections （I 〉 2σ（I））. X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn（lI） atoms which are connected by BTC3- ligands and 4,4＇-bpy coligands to form a 3D framework with 1D channels. The solid luminescence of ligand and the title complex was also studied at room temperature.展开更多
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supported by URT program of Beijing Institute of Petrochemical Technology(Beijing municipal level 2015J00058)URT program of Beijing Institute of Petrochemical Technology(State level 2015J00056)
文摘By using solvothermal method, two new metal coordination polymers based on 2,5-furandicarboxylic acid（H2FDA） ligand and 4,4＇-bipyridine（bipy）, [Cu（FDA）（4,4＇-bipy）（DMF）]n·solvent（1） and {[Zn（4,4＇-bipy）（FDA）（DMF）]·DMF}n（2）, were produced and characterized by single-crystal X-ray diffraction analyses, elemental analyses, IR and powder X-ray diffraction. Compound 1 crystallizes in monoclinic space group P21/c with a = 11.104（2）, b = 10.396（2）, c = 18.772（4） , β = 96.20（3）o, V = 2154.2（7） 3, Dc = 1.378 g/cm^3, C19H17 Cu N3O6, Mr = 446.90, F（000） = 916, μ（Mo Kα） = 1.05 mm^-1, Z = 4, R = 0.0691 and wR = 0.1341 for 3537 observed reflections（I 2σ（I））, and R = 0.1062 and w R = 0.1482 for all data. Compound 2 crystallizes in monoclinic space group C2/c with a = 29.779（6）, b = 9.6417（19）, c = 17.292（3）, β = 105.69（3）°, V = 4779.9（16） 3, Dc = 1.445 g/cm^3, C22H22N4O7 Zn, Mr = 519.81, F（000） = 2144, μ（Mo Kα）= 1.08 mm^-1, Z = 8, R = 0.0641 and w R = 0.1007 for 2985 observed reflections（I 2σ（I））, and R = 0.1028 and w R = 0.1112 for all data. Different coordination geometry of metal ions, square pyramid of Cu2＋ and trigonal bipyramid of Zn2＋, bring about different orientations of FDA2- ligands as well as 4,4＇-bipyridine ligands, and furthermore distinct assembly structures for 1 and 2. The thermal stabilities of 1 and 2 are also investigated.
基金Supported by the National Natural Science Foundation of China(Nos.20773044,20873050,20921003 and 20973074)the "111" Project of Minstry of Education of China(No.B06009)
文摘Fourier-transform infrared（FTIR）,Raman and ultraviolet-visible spectra of 4,4＇-bipyridine and its me-tal-organic coordination compounds synthesized from 4,4＇-bipyridine and nitrate of Co（Ⅱ）,Ni（Ⅱ） and Zn（Ⅱ） were measured and analyzed,respectively.The main FTIR and Raman bands were assigned in detail.The relationship between these characteristic bands and the structure of ligands and coordination compounds were discussed.
基金supported by the National Natural Science Foundation of China (No. 21071099)
文摘A new 3D metal-organic framework of {[Co3（IDC）2（bipy）2（py）2]·7H2O}n （1） was obtained by the hydrothermal reaction of Co（NO3）2·6H2O, imidazole-4,5-dicarboxylic acid （H3IDC）, 4,4＇-bipyridine （bipy）, and pyridine （py）, and structurally characterized by elemental analysis, infrared spectroscopy, thermal gravimetric analysis, and single-crystal X-ray diffraction. X-ray diffraction crystal structural analysis reveals that it crystallizes in orthorhombic system, space group Pccn with a = 11.1040（3）, b = 19.8834（5）, c = 21.3025（5）, V = 4703.3（2）3, Mr = 1079.63, Z = 4, Dc = 1.525 Mg·m-3, F（000） = 2212, μ（CuKα） = 8.855 mm-1, the final R = 0.0331 and wR = 0.0713 for 2525 observed reflections with I ≥ 2σ（I）. In compound 1, each cobalt（II） ion is six-coordinated with a slightly distorted octahedral coordination geometry, and each μ3-IDC3- acts as a bridge to bond three neighboring Co（II） ions, leading to an infinite 2D network layer structure of [Co3（IDC）2]n with Kagomé lattice. The adjacent layers are further linked by μ2-bipy to form an infinite 3D layered-pillared framework architecture of [Co3（IDC）2（bipy）2（py）2]n.
基金supported by the Science and Technology Research Project of Key Laboratory of Higher Institutions of Jiangxi Province(No.GJJ10732)the Science and Technology Research Projects of the Education Department of Jiangxi Province(No.GJJ10608)+1 种基金the Research Fund of Shangrao Normal University(No.0807)Fourth point of Specialty Construction College of Education Ministry(No.TS11524)
文摘A new complex [Cu2（sala）2（H20）2（4,4＇-bipy）]＇H20 （sala = N-（2-hydroxybenzyl）- D,L-alaninate, 4,4＇-bipy = 4,4＇-bipyridine） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in monoclinic system, space group C2/c with a = 42.44（3）, b = 10.416（8）, c = 15.487（13） ./k, fl = 97.455（14）°, C30H36Cu2N4O9, Mr = 723.71, V = 6789（9） A3, Dc = 1.416 g/cm3, Z = 8, F（000） = 2992, μ（MoKa） = 1.308 mm-1, R = 0.0493 and wR = 0.1004 for 4878 observed reflections （I 〉 2σ（I））. Structural analysis shows that each copper（II） atom displays a distorted square-based pyramidal coordination geometry with two oxygen atoms and one nitrogen atom from one N-（2-hydroxybenzyl）-D,L-alaninate, one nitrogen atom from 4,4＇-bipyridine ligand and one water molecule. 4,4＇-Bipyridine ligand bridges two Cu（II） ions to form a dinuclear compound. The molecular structure is extended into a one-dimensional wavy chain through hydrogen bonds. These 1D chains are further expanded into 2D networks through hydrogen bonds.
基金supported by the National Natural Science Foundation of China(60976019)the Foundation of Education Committee of Fujian Province(No.JB13007)
文摘A new Zn（II） coordination polymer [Zn3（BTC）2（4,4＇-bpy）（CO）2]n （1, H3BTC = 1,3,5-benzenetricarboxylic acid, 4,4＇-bpy = 4,4＇-bipyridine） has been prepared through urothermal reaction of zinc nitrate hexahydrate with 1,3,5-benzenetricarboxylic acid and 4,4＇-bipyridine, and characterized by elemental analysis, IR spectroscopy, TGA and powder XRD, and its crystal structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 10.262（3）, b = 18.838（5）, c = 15.083（4）/k, fl = 99.203（4）°, V = 2878.3（14） A3, C30H14Zn3N2O14, Mr= 822.54, Z = 4, Dc = 1.898 g/cm3,μ = 2.561 mm-1,F（000） = 1640, R = 0.0363 and wR = 0.0932 for 2828 observed reflections （I 〉 2σ（I））. X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn（lI） atoms which are connected by BTC3- ligands and 4,4＇-bpy coligands to form a 3D framework with 1D channels. The solid luminescence of ligand and the title complex was also studied at room temperature.
