A new 1D coordination polymer [Co（bpp）3Cl2（H2O）2]n 1 （bpp = 1,3-bis（4-pyridyl）-propane） was synthesized and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction. The crystal bel...A new 1D coordination polymer [Co（bpp）3Cl2（H2O）2]n 1 （bpp = 1,3-bis（4-pyridyl）-propane） was synthesized and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system,space group Ibca with a = 16.569（9）,b = 17.240（10）,c = 27.087（16） ,V = 7738（8） 3,Z = 8,Dc = 1.306 g/cm3,Mr = 760.65,λ（MoKa） = 0.71073 ,μ = 0.623 mm1,F（000） = 3192,the final R = 0.0678 and wR = 0.2011. The Co（II） atom is coordinated in a slightly distorted octahedral CoN4Cl2 geometry by two Cl atoms in the axial positions,four N atoms from the two bridging bpp ligands and two pendant bpp ligands. The CoN4Cl2 octahedra are connected by the bridging bpp ligands to form a 1D neutral coordination polymer chain. The chains are linked by face-to-face π-π interactions between adjacent pendant bpp ligands to give rise to a 3D supramolecular architecture. The photoluminescent investigation indicates that the emission of 1 is attributed to ligand-centered emission. The variable-temperature magnetic susceptibility measurement shows weak antiferromagnetic behavior in the coπmplex.展开更多
A new 1D zigzag chain coordination polymer, { [Mn（bpp）（bac）2]·（CHaCN）}n 1 （bpp = 1,3-bis（4-pyridyl）propane, Hbac = benzoylacetone）, has been synthesized and characterized by FT-IR spectroscopy, thermal ...A new 1D zigzag chain coordination polymer, { [Mn（bpp）（bac）2]·（CHaCN）}n 1 （bpp = 1,3-bis（4-pyridyl）propane, Hbac = benzoylacetone）, has been synthesized and characterized by FT-IR spectroscopy, thermal analysis and X-ray single-crystal diffraction. In the molecular structure, all Mn atoms locate in an octahedral geometry. The guest CH3CN molecules are included in the 1D channels of the 3D packing structure of 1. Crystal data： C35H35MnNaO4, Mr = 616.60, monoclinic, space group P211c, a = 17.691（4）, b = 18,955（4）, c = 9.712（6） A, β = 93.91（3）°, V = 3249.31（1） A^3, Z = 4, Dc = 1.260 g/cm^3, F（000） = 1292, 20max = 54.9°, μ = 0.447 mm^-1, the final S = 1.020, R = 0.0693 and wR = 0.1497.展开更多
A new zinc coordination polymer, [Zn2（bpp）（tpa）2H2O] 1 （bpp=1,3-bis（4-pyridyl）-propane and tpa=terephthalate） has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal ...A new zinc coordination polymer, [Zn2（bpp）（tpa）2H2O] 1 （bpp=1,3-bis（4-pyridyl）-propane and tpa=terephthalate） has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. X-ray crystal structure analysis reveals that complex 1 crystallizes in monoclinic, space group P2/c with a=18.348（2）, b=10.9080（14）, c=13.7924（18）, β=98.156（2）°, V=2732.5（6）3 , Z=4, C29H24N2O9Zn2 , Mr=675.24, Z=4, F（000）=1376, Dc=1.641 mg/m3 , μ=1.815 mm-1 , the final R=0.0443 and wR=0.0769 for 2715 observed reflections （I〉2σ（I））. The title complex exhibits a two-dimensional （4, 4） sheet structure which is further stacked through face-to-face π-π interactions between the monodentately coordinated pyridine ring of bpp ligand and the phenyl ring of terephthalate ligand to form a 3-dimensional supramolecular structure. Thermogravimetric analyses show that the host framework of the complex is thermally stable up to ca. 400 ℃.展开更多
A new double betaine 1,1′-（propane-1,3-diyl）dipyridinium-4-carboxylate L has been synthesized. Reaction of 1, 1′-（propane-1,3-diyl）dipyridinium-4-carboxylate tetrahydrate 1 with Co（ClO4）2-6H2O leads to the for...A new double betaine 1,1′-（propane-1,3-diyl）dipyridinium-4-carboxylate L has been synthesized. Reaction of 1, 1′-（propane-1,3-diyl）dipyridinium-4-carboxylate tetrahydrate 1 with Co（ClO4）2-6H2O leads to the formation of a new Co（Ⅱ） coordination compound, namely [Co（H2O）6]-2H2O-2L-2ClO4 2. The crystal structures of 1 and 2 have been determined by single-crystal X-ray diffraction method. Crystal data for 1. monoclinic, space group C2/c, a = 18.945（4）, b = 7.700（2）, c = l 1.888（2）A,β = 101.67（3）°, V = 1698.3（6） A^3, Z = 4, F（000） = 760.0, Dc = 1.402 g/cm^3, the final R = 0.0607 and wR = 0.1607 for 950 observed reflections （1 〉 2σ（I））; and those for 2： monoclinic, space group P21/c, a = 17.982（1）, b = 15.879 （1）, c = 7.0716（5）/A,β= 100.675（1）°, V= 1984.3（3） ,A^3 Z= 4, F（000） = 1010.0, Dc = 1.631 g/cm^3, the final R = 0.0316 and wR = 0.0896 for 3784 observed reflections （1 〉20（I））. Crystal structure analysis indicates that in 1, molecules of L in a ＂V-shaped＂ conformation are linked to chains sustained by O-H…O hydrogen bonds between carboxylate groups and solvent water molecules. The chains are joined by O-H…O and C-H…O hydrogen bonds to further expand into a three-dimensional structure. For 2, molecules of L in a ＂Z-shaped＂ conformation are linked by hydrogen bonds between carboxylate groups and aqua ligands to form a chain of loops running down the b axis. The （2D→2D） polythreading in compound 2 represents the mode of parallel interpenetration of 2D sheets, having polyrotaxane character.展开更多
Reactions of 1,3-bis（pyridyl-4-ylthio）propan-2-one L and COCl2·6H2O under different conditions gave two new cobalt（Ⅱ）-chloride-L complexes with distinct structures. Complex [Co（L）2Cl2]·0.5CH3OH}n 1 pr...Reactions of 1,3-bis（pyridyl-4-ylthio）propan-2-one L and COCl2·6H2O under different conditions gave two new cobalt（Ⅱ）-chloride-L complexes with distinct structures. Complex [Co（L）2Cl2]·0.5CH3OH}n 1 prepared by solvothermal treatment is a 3D network, whereas complex {[Co3（L）2Cl6（DMF）4]·2CH3OH·H2O} 2 obtained in DMF-diethyl ether system is a discrete acyclic trimer. Crystal data for 1： space group lbca, a = 15.993（4）, b = 18.454（5）, c = 21.506（6）A, V= 6347（3） ,A^3, Z = 8, Dc = 1.462 g/cm^3,μ = 1.005 mm^-1, F（000） = 2864, C26.5H26Cl2CoN4O2.5S4, Mr = 698.58, the final R = 0.0499 and wR = 0.1024. Crystal data for 2： space group P1^-, a = 9.9177（6）, b = 11.0871 （4）, c = 15.5490（12） ,A, α = 83.1834（14）,β = 88.910（13）, γ = 71.096（ 11 ）°, V = 1605.8（2） A^3, Z = 1, Dc = 1.362 g/cm^3,μ= 1.194 mm^-1, F（000） = 677, C40H62Cl6Co3N8O9S4, Mr = 1316.71, the final R = 0.0666 and wR =0.1575.展开更多
The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]undecane 4（C17H18N2O4） has been synthesized by the reaction of 2,2-bis（hydroxymethyl）propane-1,3-diol with pyridine-2-carbaldehyde in the prese...The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]undecane 4（C17H18N2O4） has been synthesized by the reaction of 2,2-bis（hydroxymethyl）propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133（2）,b = 5.7219（5）,c = 21.942（2）（A°） ,β = 99.145（2）°,V = 3115.3（5）（A°）^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F（000） = 1328,μ = 0.097 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ（I）.X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.展开更多
2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound ar...2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound are analysized by 1HNMR,13CNMR,IR and MS.展开更多
基金supported by the National High Technology Research and Development Program of China (863 Program) (No. SQ2008AA03Z2470974)the National Natural Science Foundation of China (Nos. 50572030 and 50372022)the Young Talent Program of Fujian Province (No. 2007F3060)
文摘A new 1D coordination polymer [Co（bpp）3Cl2（H2O）2]n 1 （bpp = 1,3-bis（4-pyridyl）-propane） was synthesized and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system,space group Ibca with a = 16.569（9）,b = 17.240（10）,c = 27.087（16） ,V = 7738（8） 3,Z = 8,Dc = 1.306 g/cm3,Mr = 760.65,λ（MoKa） = 0.71073 ,μ = 0.623 mm1,F（000） = 3192,the final R = 0.0678 and wR = 0.2011. The Co（II） atom is coordinated in a slightly distorted octahedral CoN4Cl2 geometry by two Cl atoms in the axial positions,four N atoms from the two bridging bpp ligands and two pendant bpp ligands. The CoN4Cl2 octahedra are connected by the bridging bpp ligands to form a 1D neutral coordination polymer chain. The chains are linked by face-to-face π-π interactions between adjacent pendant bpp ligands to give rise to a 3D supramolecular architecture. The photoluminescent investigation indicates that the emission of 1 is attributed to ligand-centered emission. The variable-temperature magnetic susceptibility measurement shows weak antiferromagnetic behavior in the coπmplex.
基金Supported by the National Natural Science Foundation of China (20701022)the Ningbo Municipal Natural Science Foundation (2007A610024)the K. C. Wong Magna Fund in Ningbo University
文摘A new 1D zigzag chain coordination polymer, { [Mn（bpp）（bac）2]·（CHaCN）}n 1 （bpp = 1,3-bis（4-pyridyl）propane, Hbac = benzoylacetone）, has been synthesized and characterized by FT-IR spectroscopy, thermal analysis and X-ray single-crystal diffraction. In the molecular structure, all Mn atoms locate in an octahedral geometry. The guest CH3CN molecules are included in the 1D channels of the 3D packing structure of 1. Crystal data： C35H35MnNaO4, Mr = 616.60, monoclinic, space group P211c, a = 17.691（4）, b = 18,955（4）, c = 9.712（6） A, β = 93.91（3）°, V = 3249.31（1） A^3, Z = 4, Dc = 1.260 g/cm^3, F（000） = 1292, 20max = 54.9°, μ = 0.447 mm^-1, the final S = 1.020, R = 0.0693 and wR = 0.1497.
基金supported by the Education Office of Anhui Province (No. 2011SQRL080)
文摘A new zinc coordination polymer, [Zn2（bpp）（tpa）2H2O] 1 （bpp=1,3-bis（4-pyridyl）-propane and tpa=terephthalate） has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. X-ray crystal structure analysis reveals that complex 1 crystallizes in monoclinic, space group P2/c with a=18.348（2）, b=10.9080（14）, c=13.7924（18）, β=98.156（2）°, V=2732.5（6）3 , Z=4, C29H24N2O9Zn2 , Mr=675.24, Z=4, F（000）=1376, Dc=1.641 mg/m3 , μ=1.815 mm-1 , the final R=0.0443 and wR=0.0769 for 2715 observed reflections （I〉2σ（I））. The title complex exhibits a two-dimensional （4, 4） sheet structure which is further stacked through face-to-face π-π interactions between the monodentately coordinated pyridine ring of bpp ligand and the phenyl ring of terephthalate ligand to form a 3-dimensional supramolecular structure. Thermogravimetric analyses show that the host framework of the complex is thermally stable up to ca. 400 ℃.
基金This work was financially supported by Liuhui Center for Applied Mathematics, Nankai University and Tianjin University (No. H10114)
文摘A new double betaine 1,1′-（propane-1,3-diyl）dipyridinium-4-carboxylate L has been synthesized. Reaction of 1, 1′-（propane-1,3-diyl）dipyridinium-4-carboxylate tetrahydrate 1 with Co（ClO4）2-6H2O leads to the formation of a new Co（Ⅱ） coordination compound, namely [Co（H2O）6]-2H2O-2L-2ClO4 2. The crystal structures of 1 and 2 have been determined by single-crystal X-ray diffraction method. Crystal data for 1. monoclinic, space group C2/c, a = 18.945（4）, b = 7.700（2）, c = l 1.888（2）A,β = 101.67（3）°, V = 1698.3（6） A^3, Z = 4, F（000） = 760.0, Dc = 1.402 g/cm^3, the final R = 0.0607 and wR = 0.1607 for 950 observed reflections （1 〉 2σ（I））; and those for 2： monoclinic, space group P21/c, a = 17.982（1）, b = 15.879 （1）, c = 7.0716（5）/A,β= 100.675（1）°, V= 1984.3（3） ,A^3 Z= 4, F（000） = 1010.0, Dc = 1.631 g/cm^3, the final R = 0.0316 and wR = 0.0896 for 3784 observed reflections （1 〉20（I））. Crystal structure analysis indicates that in 1, molecules of L in a ＂V-shaped＂ conformation are linked to chains sustained by O-H…O hydrogen bonds between carboxylate groups and solvent water molecules. The chains are joined by O-H…O and C-H…O hydrogen bonds to further expand into a three-dimensional structure. For 2, molecules of L in a ＂Z-shaped＂ conformation are linked by hydrogen bonds between carboxylate groups and aqua ligands to form a chain of loops running down the b axis. The （2D→2D） polythreading in compound 2 represents the mode of parallel interpenetration of 2D sheets, having polyrotaxane character.
基金This work was financially support by NNSFC (No. 20231020), NSF of Fujian Province and the Key Project from CAS
文摘Reactions of 1,3-bis（pyridyl-4-ylthio）propan-2-one L and COCl2·6H2O under different conditions gave two new cobalt（Ⅱ）-chloride-L complexes with distinct structures. Complex [Co（L）2Cl2]·0.5CH3OH}n 1 prepared by solvothermal treatment is a 3D network, whereas complex {[Co3（L）2Cl6（DMF）4]·2CH3OH·H2O} 2 obtained in DMF-diethyl ether system is a discrete acyclic trimer. Crystal data for 1： space group lbca, a = 15.993（4）, b = 18.454（5）, c = 21.506（6）A, V= 6347（3） ,A^3, Z = 8, Dc = 1.462 g/cm^3,μ = 1.005 mm^-1, F（000） = 2864, C26.5H26Cl2CoN4O2.5S4, Mr = 698.58, the final R = 0.0499 and wR = 0.1024. Crystal data for 2： space group P1^-, a = 9.9177（6）, b = 11.0871 （4）, c = 15.5490（12） ,A, α = 83.1834（14）,β = 88.910（13）, γ = 71.096（ 11 ）°, V = 1605.8（2） A^3, Z = 1, Dc = 1.362 g/cm^3,μ= 1.194 mm^-1, F（000） = 677, C40H62Cl6Co3N8O9S4, Mr = 1316.71, the final R = 0.0666 and wR =0.1575.
基金supported by the National Natural Science Foundation of China (No. 20872051 and 21002009)the Scientific and Technological Project of Changzhou (CJ20115019)the Priority Academic Program Development of Jiangsu Higher Education Institutions
文摘The title compound 3,9-bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]undecane 4（C17H18N2O4） has been synthesized by the reaction of 2,2-bis（hydroxymethyl）propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133（2）,b = 5.7219（5）,c = 21.942（2）（A°） ,β = 99.145（2）°,V = 3115.3（5）（A°）^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F（000） = 1328,μ = 0.097 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ（I）.X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.
文摘2-(3-(4-methoxyphenoxy)propyl)propane-1,3-diethanethioate is synthesized from 4-methoxyphenol and 1,3-dibromopropane after five-step reaction.The overall yield is 21.2%.The key intermediates and the target compound are analysized by 1HNMR,13CNMR,IR and MS.
