A series of 2-aryl-1-arylmethyl-1H-1,3-benzimidazoles was synthesized expeditiously in good yields from o-phenylenediamines and aldehydes in the presence of Fe（ClO4）3 without solvent at room temperature.
Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst u...Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst under solvent-free conditions at room temperature.For unsymmetrical o-phenylenediamines bearing electron-withdrawing groups,regio-selective quinoxalines were obtained.展开更多
The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.73...The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.734(3), b = 13.112(4), c = 15.327(4) , = 93.023(6), V = 2154.2(11) ?, Mr = 532.80, Z = 4, Dc = 1.643 g/cm3, m(MoKa) = 0.71073 ? F(000) = 1088, R = 0.0502 and wR = 0.0928. The CoⅢ atom is coordinated by one chelating TPA ligand and two terminal azide groups to form a distorted octahedral geometry. The crystal of 2 belongs to monoclinic, space group P21/c with a = 15.405(6), b = 9.269(4), c = 14.998(6) 3, = 93.489(7), V = 2137.6(14) ? Mr = 495.38, Z = 4, Dc = 1.539 g/cm3, m(MoKa ) = 0.71073 ? F(000) = 1012, R = 0.0521 and wR = 0.0992. The CuⅡ atom is coordinated by one chelating TPA ligand and one terminal azide group, forming a distorted trigonal bipyramidal geometry.展开更多
Mononuclear complex {[Cu(N-men)2(cda)2]·[Cu(N-men)2]-(ClO4)2} was synthesized by sodium carbamyldicyanomethanide Na(cda), N-methylethylenediamine and hydrate copper perchlorate. The crystal belongs to the triclin...Mononuclear complex {[Cu(N-men)2(cda)2]·[Cu(N-men)2]-(ClO4)2} was synthesized by sodium carbamyldicyanomethanide Na(cda), N-methylethylenediamine and hydrate copper perchlorate. The crystal belongs to the triclinic system, space group P 1 with a = 7.229(2), b = 8.114(2), c = 15.936(4) A, α = 80.511(4), β = 78.993(4), r= 72.118(4)°, V = 867.6(3) A3, Z = 1, C20H44Cl2Cu2N14O10, Mr = 838.68, Dc = 1.605 g/cm3, F(000) = 434 and μ = 1.449 mm-1. The structure was refined to R = 0.0480 and wR = 0.1289 for 2503 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination models for Cu (II) ions. One is that the Cu (II) ion is coordinated by four nitrogen atoms which are from two N-men molecules, and a slightly distorted square planar coordinate environment is formed around the Cu (II) ion; the other is that the Cu (II) ion is coordinated by six nitrogen atoms, of which four are from two N-men molecules and the left from nitrile groups, resulting in a distorted octahedron around the Cu (II) ion. The deposition number of the crystal at CCDC is 161868.展开更多
A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crysta...A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crystallizes in triclinic system, space group P?with a = 11.6297(5), b = 12.5165(5), c = 13.8986(6) ? a = 63.345(1), b = 87.747(1), g = 71.862(1), V = 1706.20(1) ?, Z = 1, Dc = 1.673 g/cm3, F(000) = 868 and m(MoKa) = 1.185 mm-1 (l = 0.71073 ). R = 0.0800 and wR = 0.1793 for 7653 observed reflections (I > 2s(I)). The structure consists of a dinuclear cation [Cd2(phen)4(fca)2]2+, two discrete perchlorate anions and two water molecules. The cationic part of the complex shows a tetrametallic core in which two fca groups act as the (O, O) bridging ligands between two cadmium(Ⅱ) ions with a distorted octahedral environment. The Cd…Cd intradimer distance is 4.128 ?展开更多
The electron paramagnetic resonance（EPR） spectra of trigonal Mn^（2＋） centers in Zn（ClO4）2·6（H2O） and Mg（ClO4）2·6（H2O） crystals were studied on the basis of the complete energy matrices for a d^5...The electron paramagnetic resonance（EPR） spectra of trigonal Mn^（2＋） centers in Zn（ClO4）2·6（H2O） and Mg（ClO4）2·6（H2O） crystals were studied on the basis of the complete energy matrices for a d^5 configuration ion in a trigonal ligand field. It was demonstrated that the local lattice structure around a trigonal Mn^（2＋） center has an compressed distortion along the crystalline c3 axis, and when Mn^（2＋） is doped in the Zn（ClO4）2·6（H2O） and Mg（ClO4）2·6（H2O） crystals, there is a similar local distortion. From the EPR calculation, the local lattice structure parameters R=2.183 2 ？, for Zn（ClO4）2·6（H2O）, R=2.130 2 ？, for Mg（ClO4）2·6（H2O） have been determined.展开更多
文摘A series of 2-aryl-1-arylmethyl-1H-1,3-benzimidazoles was synthesized expeditiously in good yields from o-phenylenediamines and aldehydes in the presence of Fe（ClO4）3 without solvent at room temperature.
基金Supported by the National Natural Science Foundation of China(Nos.20772088,21172163)the Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions,China(No.JSSYSXK2010007)
文摘Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst under solvent-free conditions at room temperature.For unsymmetrical o-phenylenediamines bearing electron-withdrawing groups,regio-selective quinoxalines were obtained.
基金Supported by the National Natural Science Foundation of China (No. 20171026) and Natural Science Foundation of Tianjin (No. 013605811)
文摘The title complexes [CoⅢ(TPA)(N3)2](ClO4) 1 and [CuⅡ(TPA)(N3)](ClO4) 2 have been synthesized and characterized by single-crystal X-ray diffraction. The crystal of 1 is of monoclinic, space group P21/n with a = 10.734(3), b = 13.112(4), c = 15.327(4) , = 93.023(6), V = 2154.2(11) ?, Mr = 532.80, Z = 4, Dc = 1.643 g/cm3, m(MoKa) = 0.71073 ? F(000) = 1088, R = 0.0502 and wR = 0.0928. The CoⅢ atom is coordinated by one chelating TPA ligand and two terminal azide groups to form a distorted octahedral geometry. The crystal of 2 belongs to monoclinic, space group P21/c with a = 15.405(6), b = 9.269(4), c = 14.998(6) 3, = 93.489(7), V = 2137.6(14) ? Mr = 495.38, Z = 4, Dc = 1.539 g/cm3, m(MoKa ) = 0.71073 ? F(000) = 1012, R = 0.0521 and wR = 0.0992. The CuⅡ atom is coordinated by one chelating TPA ligand and one terminal azide group, forming a distorted trigonal bipyramidal geometry.
基金This work was supported by the Natural Science Foundation of Shandong province as the key project(No.Z99B02)general project(No.Q98B02118)
文摘Mononuclear complex {[Cu(N-men)2(cda)2]·[Cu(N-men)2]-(ClO4)2} was synthesized by sodium carbamyldicyanomethanide Na(cda), N-methylethylenediamine and hydrate copper perchlorate. The crystal belongs to the triclinic system, space group P 1 with a = 7.229(2), b = 8.114(2), c = 15.936(4) A, α = 80.511(4), β = 78.993(4), r= 72.118(4)°, V = 867.6(3) A3, Z = 1, C20H44Cl2Cu2N14O10, Mr = 838.68, Dc = 1.605 g/cm3, F(000) = 434 and μ = 1.449 mm-1. The structure was refined to R = 0.0480 and wR = 0.1289 for 2503 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination models for Cu (II) ions. One is that the Cu (II) ion is coordinated by four nitrogen atoms which are from two N-men molecules, and a slightly distorted square planar coordinate environment is formed around the Cu (II) ion; the other is that the Cu (II) ion is coordinated by six nitrogen atoms, of which four are from two N-men molecules and the left from nitrile groups, resulting in a distorted octahedron around the Cu (II) ion. The deposition number of the crystal at CCDC is 161868.
基金the grants from the State Key Program of China the National Natural Science Foundation of China (29871001 20071001) and the Committee of Education of Anhui province
文摘A novel complex [Cd2(phen)4(fca)2](ClO4)2(H2O)2 (fca = dianion of 3-ferrocenyl- 2-crotonic acid, phen = 1,10-phenanthroline) has been synthesized and characterized by X-ray single-crystal structure analysis. It crystallizes in triclinic system, space group P?with a = 11.6297(5), b = 12.5165(5), c = 13.8986(6) ? a = 63.345(1), b = 87.747(1), g = 71.862(1), V = 1706.20(1) ?, Z = 1, Dc = 1.673 g/cm3, F(000) = 868 and m(MoKa) = 1.185 mm-1 (l = 0.71073 ). R = 0.0800 and wR = 0.1793 for 7653 observed reflections (I > 2s(I)). The structure consists of a dinuclear cation [Cd2(phen)4(fca)2]2+, two discrete perchlorate anions and two water molecules. The cationic part of the complex shows a tetrametallic core in which two fca groups act as the (O, O) bridging ligands between two cadmium(Ⅱ) ions with a distorted octahedral environment. The Cd…Cd intradimer distance is 4.128 ?
基金Funded in Part by the National Natural Science Foundation of China(No.61601384)
文摘The electron paramagnetic resonance（EPR） spectra of trigonal Mn^（2＋） centers in Zn（ClO4）2·6（H2O） and Mg（ClO4）2·6（H2O） crystals were studied on the basis of the complete energy matrices for a d^5 configuration ion in a trigonal ligand field. It was demonstrated that the local lattice structure around a trigonal Mn^（2＋） center has an compressed distortion along the crystalline c3 axis, and when Mn^（2＋） is doped in the Zn（ClO4）2·6（H2O） and Mg（ClO4）2·6（H2O） crystals, there is a similar local distortion. From the EPR calculation, the local lattice structure parameters R=2.183 2 ？, for Zn（ClO4）2·6（H2O）, R=2.130 2 ？, for Mg（ClO4）2·6（H2O） have been determined.
