The novel coordination structures of europium and terbium chloride-picolinamide complexes （EuCl3-（C6H6N2O）2.5H2O, Eu-pa and TbCl3.（C6H6N2O）2.5H2O, Tb-pa） are reported. The crystal structures in the solid state a...The novel coordination structures of europium and terbium chloride-picolinamide complexes （EuCl3-（C6H6N2O）2.5H2O, Eu-pa and TbCl3.（C6H6N2O）2.5H2O, Tb-pa） are reported. The crystal structures in the solid state are characterized by X-ray single crystal diffraction, FTIR, Raman, FIR, THz and luminescence spectroscopy. In the crystal structures, the pyridyl nitrogen and carbonyl oxygen atoms in picolinamide are coordinated to the metal ions to form a five-membered ring structure. The experimental results indicate the similar coordination structures of Eu and Tb-pa complexes and the changes of hydrogen bonds and conformation provide models for the coordination structures of the ligands induced by complexation. The results of lanthanide ions with ligands having amide groups.展开更多
Three full-substituted calix[6]arenes containing the picolinamide groups were synmesized and characterized by IR, ^1HNMR and MS, after series reactions, including lower rim etherification, upper rim ipso-nitration, re...Three full-substituted calix[6]arenes containing the picolinamide groups were synmesized and characterized by IR, ^1HNMR and MS, after series reactions, including lower rim etherification, upper rim ipso-nitration, reduction, amidation.展开更多
A hydrogen-bonded supermolecular compound [（C6H5N2O）3·Cu1.5]·6H2O was synthesized from picolinamide and Cu（NO3）2·6H2O at the presence of sodium pyrophosphate decahydrate. It crystallizes in triclini...A hydrogen-bonded supermolecular compound [（C6H5N2O）3·Cu1.5]·6H2O was synthesized from picolinamide and Cu（NO3）2·6H2O at the presence of sodium pyrophosphate decahydrate. It crystallizes in triclinic, space group P1^- with a = 1.05947（8）, b = 1.09130（8）, c = 1.11456（8） nm, a = 67.8460（10）, β= 84.497（1）, γ = 74.6210（10）°, C18H27Cu1.5N6O9, Mr = 566.77, V = 1.15077（15） nm^3, Z = 2, Dc = 1.636 g/cm^3, F（000） = 585,μ= 1.461 mm^-1, R1 = 0.0278 and wR2 = 0.0749. In the complex, the Cu（Ⅱ） ion reveals a distorted tetradentate plane-tetragonal geometry. The structure consists of neutral two-dimensional layers via hydrogen bonds O-H...O and N-H...O between the molecules, and the layers are connected by weak interactions of the Cu-Cu, Cu-N, π-π and hydrogen bonds to form a three-dimensional network structure.展开更多
The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. T...The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. The crystal structure of the title compound, was reported previously from Weissenberg photographic data with R = 0.127. It has now been redetermined, providing a significant increase in the precision of the derived geometric parameters. The crystal packing is governed by N--HO hydrogen bond-type intermolecular interactions, forming infinite one-dimensional chains with graph-set notation C(4), R22(8) and R24(8).展开更多
Directing group-assisted, transition metal-catalyzed three-component difunctionalization of alkenes has emerged as a powerful tool to drive molecular complexity. However, this strategy generally works with the substra...Directing group-assisted, transition metal-catalyzed three-component difunctionalization of alkenes has emerged as a powerful tool to drive molecular complexity. However, this strategy generally works with the substrates bearing directing groups in close proximity to the alkene moieties, due to the preference for formation of kinetically stable five-membered metallacycles. Herein, we have disclosed a complementary strategy to accomplish a nickel-catalyzed remote arylalkylation of alkenyl amines with excellent regioselectivity and diastereofidelity, involving rare six- or seven-membered metallacycles. This general protocol is compatible with a series of δ- and ε-alkenyl amines, providing corresponding valuable δ,ε- and ε,ζ-difunctionalized aliphatic amines that would be difficult to synthesize. The coordination of the bidentate picolinamide auxiliary and the facile oxidative addition of alkyl halides to Ni(I) species are the key to the success of the developed remote olefin dicarbofunctionalization.展开更多
基金National Natural Science Foundation of China for the grants(Nos.21001009 and 50973003)the State Key Project for Fundamental Research of MOST(No.2011CB808304)+2 种基金National High-tech R&D Program of China(863 Program) of MOST (No.2010AA03A406)the Scientific Research Project of Beijing Municipal Commission of EducationBeijing Natural Science Foundation(No.KZ201310028032)
文摘The novel coordination structures of europium and terbium chloride-picolinamide complexes （EuCl3-（C6H6N2O）2.5H2O, Eu-pa and TbCl3.（C6H6N2O）2.5H2O, Tb-pa） are reported. The crystal structures in the solid state are characterized by X-ray single crystal diffraction, FTIR, Raman, FIR, THz and luminescence spectroscopy. In the crystal structures, the pyridyl nitrogen and carbonyl oxygen atoms in picolinamide are coordinated to the metal ions to form a five-membered ring structure. The experimental results indicate the similar coordination structures of Eu and Tb-pa complexes and the changes of hydrogen bonds and conformation provide models for the coordination structures of the ligands induced by complexation. The results of lanthanide ions with ligands having amide groups.
基金Thanks for the support of the National Natural Science Foundation of China （No.20376059）.
文摘Three full-substituted calix[6]arenes containing the picolinamide groups were synmesized and characterized by IR, ^1HNMR and MS, after series reactions, including lower rim etherification, upper rim ipso-nitration, reduction, amidation.
文摘A hydrogen-bonded supermolecular compound [（C6H5N2O）3·Cu1.5]·6H2O was synthesized from picolinamide and Cu（NO3）2·6H2O at the presence of sodium pyrophosphate decahydrate. It crystallizes in triclinic, space group P1^- with a = 1.05947（8）, b = 1.09130（8）, c = 1.11456（8） nm, a = 67.8460（10）, β= 84.497（1）, γ = 74.6210（10）°, C18H27Cu1.5N6O9, Mr = 566.77, V = 1.15077（15） nm^3, Z = 2, Dc = 1.636 g/cm^3, F（000） = 585,μ= 1.461 mm^-1, R1 = 0.0278 and wR2 = 0.0749. In the complex, the Cu（Ⅱ） ion reveals a distorted tetradentate plane-tetragonal geometry. The structure consists of neutral two-dimensional layers via hydrogen bonds O-H...O and N-H...O between the molecules, and the layers are connected by weak interactions of the Cu-Cu, Cu-N, π-π and hydrogen bonds to form a three-dimensional network structure.
文摘The title compound, 2-pyridinecarboxamide, C6H6N2O, crystallize in the monoclinic system with space group P21/n (No14), Z = 4, and unit cell parameters a = 5.2074(1) , b = 7.1004(1) , c = 16.2531(3) , = 100.260(1)o. The crystal structure of the title compound, was reported previously from Weissenberg photographic data with R = 0.127. It has now been redetermined, providing a significant increase in the precision of the derived geometric parameters. The crystal packing is governed by N--HO hydrogen bond-type intermolecular interactions, forming infinite one-dimensional chains with graph-set notation C(4), R22(8) and R24(8).
基金This work was supported by the National Natural Science Foundation of China(21901185,22002037)the Innovation and Entrepreneurship Training Programme for University Students(202110546007)+1 种基金the Scientific Research Hunan Provincial Education Department(19A068)funds provided by Tianjin Normal University.
文摘Directing group-assisted, transition metal-catalyzed three-component difunctionalization of alkenes has emerged as a powerful tool to drive molecular complexity. However, this strategy generally works with the substrates bearing directing groups in close proximity to the alkene moieties, due to the preference for formation of kinetically stable five-membered metallacycles. Herein, we have disclosed a complementary strategy to accomplish a nickel-catalyzed remote arylalkylation of alkenyl amines with excellent regioselectivity and diastereofidelity, involving rare six- or seven-membered metallacycles. This general protocol is compatible with a series of δ- and ε-alkenyl amines, providing corresponding valuable δ,ε- and ε,ζ-difunctionalized aliphatic amines that would be difficult to synthesize. The coordination of the bidentate picolinamide auxiliary and the facile oxidative addition of alkyl halides to Ni(I) species are the key to the success of the developed remote olefin dicarbofunctionalization.
