The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its st...The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) ? a = 79.5990(10), = 83.6300(10), ? = 71.8280(10)o, V = 1272.60(8) ?, C48H44Cu4N8O24, Mr = 1371.07, Z = 1, Dc = 1.789 g/cm3, = 1.747 mm-1, F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2s(I)). There are two kinds of Cu coordination environments, and each central copper(II) atom is five-coordinated in a distorted square-based pyramidal coordination geo- metry. Four copper(II) atoms are linked by four pdc and two 4,4?-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate O atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network struc- ture.展开更多
Crystal structure of pyridine-2,6-dicarboxylate(dipc) vanadium complex:[(dipc)VO_2]_2( 4, 4'-bipyridine)·4H_2O(M_r=724.34) is monoclinic with space group C2/c and a=25.857(8),b=6.896(1),c=16.267(5),β=106.27(...Crystal structure of pyridine-2,6-dicarboxylate(dipc) vanadium complex:[(dipc)VO_2]_2( 4, 4'-bipyridine)·4H_2O(M_r=724.34) is monoclinic with space group C2/c and a=25.857(8),b=6.896(1),c=16.267(5),β=106.27(4)°,V=2784.62 D_c=1.73 g/cm￣3,F(000)=1472,Z=4.The structural solutions and refinements based on 1661 reflections (I>2σ(I))converged at R=0. 043.The coordinated number of vanadium atom is 5,the geometrical form of the five atoms are coordinated to the vanadium atom is a distorted tetragonal bipyramid of which the four coordinated atoms O(3),O(5),N(1) and O(2) make up the equatorial plane,while the other coordinated atom O(1) is to occupy the apex.展开更多
New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebip...New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.展开更多
A series of 4,4＇-disubstituted-[2,2＇]-bipyridines, featuring electron withdrawing/donating functional groups such as amino, chloro, nitro, ethoxycarbonyl, carboxy, methyl, methoxy and hydroxymethyl, have been syn- t...A series of 4,4＇-disubstituted-[2,2＇]-bipyridines, featuring electron withdrawing/donating functional groups such as amino, chloro, nitro, ethoxycarbonyl, carboxy, methyl, methoxy and hydroxymethyl, have been syn- thesized and employed in the copolymerization of carbon monoxide （CO） and styrene. The available bipyridine and its derivatives were coordinated with palladium （ II ） acetate for catalyzing the copolymerization of CO and styrene, and the concomitant polyketone was characterized by means of t3C NMR, FTIR, differential scanning calo- rimetry （DSC） and element analysis techniques concerning its structure and thermal performance. The effect of dif- ferent electron-donating and electron-withdrawing groups on catalyst performance and molecular weight of co- polymer was studied under certain experimental condition. It has been proved that the enhancement of electron donating and conjugative effects on bipyridine ligand will not only improve the catalytic activity of the composi- tion, but also increase the molecular weight of the as-prepared polyketone. The catalytic activity is the highest in hydroxymethyl substituted 2,2＇-bipyridine ligand（l 356 gSTCO/（gPd · h））, when the molecular weight and polydispersity index of the polyketone are Mn = 8 502, Mw = 1 3440 and Mw/Mn = 1.581, respectively.展开更多
基金This work was financially supported by the NNSFC (No. 20173063) the State Key Basic Research and Development Plan of China (001CB108906) and the NSF of Fujian Province (E0020001)
文摘The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) ? a = 79.5990(10), = 83.6300(10), ? = 71.8280(10)o, V = 1272.60(8) ?, C48H44Cu4N8O24, Mr = 1371.07, Z = 1, Dc = 1.789 g/cm3, = 1.747 mm-1, F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2s(I)). There are two kinds of Cu coordination environments, and each central copper(II) atom is five-coordinated in a distorted square-based pyramidal coordination geo- metry. Four copper(II) atoms are linked by four pdc and two 4,4?-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate O atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network struc- ture.
文摘Crystal structure of pyridine-2,6-dicarboxylate(dipc) vanadium complex:[(dipc)VO_2]_2( 4, 4'-bipyridine)·4H_2O(M_r=724.34) is monoclinic with space group C2/c and a=25.857(8),b=6.896(1),c=16.267(5),β=106.27(4)°,V=2784.62 D_c=1.73 g/cm￣3,F(000)=1472,Z=4.The structural solutions and refinements based on 1661 reflections (I>2σ(I))converged at R=0. 043.The coordinated number of vanadium atom is 5,the geometrical form of the five atoms are coordinated to the vanadium atom is a distorted tetragonal bipyramid of which the four coordinated atoms O(3),O(5),N(1) and O(2) make up the equatorial plane,while the other coordinated atom O(1) is to occupy the apex.
文摘New heteroleptic and homoleptic complexes of the type[Pd（4,5-dmbipy）C12], [Pd（4,5-dmbipy）L2], and [Pd（4,5-dimebipy）2]2＋ （L = Pyridine or 4-methylpyridine（4-picoline）, bipy = 2,2＇-bipyridine, and 4,5-dimebipy = 4,5-dimethyl-2,2＇-bipyridine） were synthesized and characterized by IH NMR and elemental analysis. The crystal structure of bis（4-methylpyridine）-4,5- dimethyl-2,2＇-bipyridinepalladium（II）perchlorate [Pd（4,5-dmbipy）（4-pic）2]（CIO4）2 was also determined by single crystal X-ray diffraction. This complex crystallized in the triclinic crystal system and space group PI with a = 9.562 （2）, b = 11.326 （4）, c = 15.0120 （10） A°; α = 70.940°, β= 77.60 （2）, γ= 67.86 （2） and z = 4. The Pd （II） in square planar environment showed a small distortion towards tetrahedral through one coordinated bipyridine ring twisting with respect to the other.
基金Supported by Tianjin Natural Science Foundation(No.07JCYBJC00600)
文摘A series of 4,4＇-disubstituted-[2,2＇]-bipyridines, featuring electron withdrawing/donating functional groups such as amino, chloro, nitro, ethoxycarbonyl, carboxy, methyl, methoxy and hydroxymethyl, have been syn- thesized and employed in the copolymerization of carbon monoxide （CO） and styrene. The available bipyridine and its derivatives were coordinated with palladium （ II ） acetate for catalyzing the copolymerization of CO and styrene, and the concomitant polyketone was characterized by means of t3C NMR, FTIR, differential scanning calo- rimetry （DSC） and element analysis techniques concerning its structure and thermal performance. The effect of dif- ferent electron-donating and electron-withdrawing groups on catalyst performance and molecular weight of co- polymer was studied under certain experimental condition. It has been proved that the enhancement of electron donating and conjugative effects on bipyridine ligand will not only improve the catalytic activity of the composi- tion, but also increase the molecular weight of the as-prepared polyketone. The catalytic activity is the highest in hydroxymethyl substituted 2,2＇-bipyridine ligand（l 356 gSTCO/（gPd · h））, when the molecular weight and polydispersity index of the polyketone are Mn = 8 502, Mw = 1 3440 and Mw/Mn = 1.581, respectively.
