The title complex bis{1-[[(3-ethyl-6-methyl-2-pyridinyl)imino]methylenyl]- 2-na- phthalenola-to-N,O}nickel has been synthesized by the reaction of 1-[[(3-ethyl-6-methyl-2- pyridinyl) imino] methylenyl]-2-naphthale...The title complex bis{1-[[(3-ethyl-6-methyl-2-pyridinyl)imino]methylenyl]- 2-na- phthalenola-to-N,O}nickel has been synthesized by the reaction of 1-[[(3-ethyl-6-methyl-2- pyridinyl) imino] methylenyl]-2-naphthalenol with Ni(CH3 COO)2 ·4H2 O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group Pbca with a = 11.100(2), b = 15.900(3), c = 18.000(4), V = 3176.8(11)3, C38 H34 N4 NiO2, Mr = 637.40, Z = 4, Dc = 1.333 g/cm3, μ = 0.651 mm-1, F(000) = 1336, the final R = 0.0783 and wR = 0.2119. This title compound was investigated for the catalytic behavior towards norbornene(NB) vinyl addition polymerization. And the complex exhibited good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.展开更多
The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methy...The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. Single-crystal X-ray diffraction analysis results further confirmed the molecular structures. The crystal belongs to the monoclinic system, space group P2_1/c with a = 4.1324(2), b = 23.5432(16), c = 11.8943(8) A, β = 91.238(5)o, V = 1156.93(12) ?~3, C_(26)H_(20)Cl_2N_4O_2Pd, M_r = 597.76, Z = 2, D_c = 1.716 g/cm^3, μ = 1.067 mm^(-1), F(000) = 600, the final R = 0.0247 and w R = 0.0677(I 〉 2σ(I)). In the presence of methylaluminoxane(MAO), the complex exhibits excellent catalytic activities(1.737×10~7 g of PNB(mol of Pd)^(-1)·h^(-1)) in the vinyl polymerization of norbornene.展开更多
The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphtha...The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphthalenol with Ni(CH3COO)2·4H2O, and characterized by IR spectrum, elemental analysis and TG. The complicated space structure has been confirmed by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.410(4), b = 14.382(4), c = 18.121(6) ,A, β = 97.147(6)% V= 2950.5(16)A3, C36H32N4O2Ni, Mr = 611.37, Z = 4, Dc = 1.376 g/cm3, μ = 0.698 mm-1 F(000) = 1280, the final R = 0.0519 and wR = 0.1493 (1 〉2σ(I)). This title compound was used as precatalysts for the polymerisation of norbornene. When activated with MAO, the complex exhibited excellent catalytic activity up to 1.98 × 107 g ofPNB (mol of Ni)-1 h-1 with high monomer conversion.展开更多
A novel polyoxometalate {[Ag^I(4,4'-bipy)]3[PW12O40]}·(4,4'-bipy)·4H2O 1 has been synthesized hydrothermally and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crysta...A novel polyoxometalate {[Ag^I(4,4'-bipy)]3[PW12O40]}·(4,4'-bipy)·4H2O 1 has been synthesized hydrothermally and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of 1 belongs to the triclinic system, space group P1 with a = 11.3710(17), b = 12.0701(16), c = 13.1061(12) A, α = 112.838(3), β = 94.545(6), γ = 99.526(4)°, V = 1614.4(4) A^3, Mr = 3825.40, Z = 1, Dc = 3.935, μ = 22.289mm^-1, F(000) = 1692, the final R = 0.0507 and wR = 0.1054. X-ray diffraction analysis reveals that the molecular structure of 1 consists of three coordinated cations [AgI(4,4'-bipy)]+, a polyanion unit [PW12O40]3-, and a discrete 4,4′-bipy molecule. Significantly, there exist two crystallographically independent silver(I) centers in 1 and all [AgI(4,4'-bipy)]^+ cations are linked with each other to form a one-dimensional Ag-4,4'-bipy polymer chain. The neighboring polymer chains are further interconnected to form a 3D framework by the covalent effect of silver atoms and terminal oxygen atoms of the polyanion. The electrochemical behaviors of 1 have also been studied in detail by cyclic voltammograms.展开更多
A Keggin-type tungstohosphate compound [Cu^l(2,2'-bipy)2]3[PW^Ⅵ12O40] 1 (bipy = bipyddine) was prepared by the hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C60H48Cu3...A Keggin-type tungstohosphate compound [Cu^l(2,2'-bipy)2]3[PW^Ⅵ12O40] 1 (bipy = bipyddine) was prepared by the hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C60H48Cu3N12O40PW12) crystallizes in the monoclinic system, space group P21/c with a = 16.9837(10), b = 17.9732(13) c = 27.8701(13)A°, β = 96.1039(10)°, V = 8459.2(9) A°^3, Mr = 4004.89, Z = 4, Dc = 3.145 g/cm^3, μ = 17.089 mm^-1, F(000) = 7208, S = 1.005, the final R = 0.0469 and wR = 0.0827 for 10807 observed reflections (I 〉 2σ(I)). Compound 1 consists of one discrete normal Keggin polyanion [PW^Ⅵ 12O40]^3- and three isolated coordinated cations [Cu^1(2,2'-bipy)2]^+. Significantly, there exist three crystallographically independent asymmetric reduced copper (I) centers in 1. Furthermore, the compound shows strong photoluminescence property in solid state at room temperature.展开更多
The title complex bis{(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine-N,O}nickel has been synthesized by the reaction of(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-...The title complex bis{(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine-N,O}nickel has been synthesized by the reaction of(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine with Ni(CH3COO)2·4H2O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 12.373(4), b = 18.434(7), c = 27.814(10) A, β = 92.291(6)o, V = 6339(4) A^3, C7 2H8 0N2 Ni O2, Mr = 1064.09, Z = 4, Dc = 1.115 g/cm^3, μ = 0.350 mm^-1, F(000) = 2280, the final R = 0.0846 and wR = 0.2926(I 〉 2s(I)). This title compound was used as homogeneous catalysis of polymerization of norbornene, and the complex exhibited good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.展开更多
The title compound,bromo-(2-diphenylphosphino-N-(2-oxybenzylidene)-aniline)- nickel,was synthesized by simple condensation of 2-diphenylphosphino-N-(2-oxybenzylidene)- aniline with NiBr2·6H2O and characteri...The title compound,bromo-(2-diphenylphosphino-N-(2-oxybenzylidene)-aniline)- nickel,was synthesized by simple condensation of 2-diphenylphosphino-N-(2-oxybenzylidene)- aniline with NiBr2·6H2O and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a = 9.756(2),b = 10.232(2),c = 13.313(3)A,α = 95.09(3),β = 102.48(3),γ = 95.45(3)o,V = 1283.5(4) A^3,C29H23BrNNiO2P,Mr = 587.07,Z = 2,Dc = 1.519 g/cm^3,λ(MoKα) = 0.71073 A,F(000) = 596 and μ = 2.402 mm^-1. The structure was refined to the final R = 0.0408 and wR = 0.0965 for 4507 observed reflections (I 〉 2σ(I)). Intermolecular π-π interactions (with distances of about 3.705 A) are pronounced in the crystal structure. Under methylaluminoxane (MAO) activation,the title compound was able to catalyze norbornene polymerization,exhibiting good polymerization activities.展开更多
The title complex N,O-bis{2-[[(2-benzhydryl-4,6-dimethylphenyl)imino]-methyl]-phenol}-nickel(II)(C56H48N2NiO2) has been synthesized by the reaction of 2-[[(2-benzhydryl-4,6-dimethylphenyl)mino]-methyl]-phenol ...The title complex N,O-bis{2-[[(2-benzhydryl-4,6-dimethylphenyl)imino]-methyl]-phenol}-nickel(II)(C56H48N2NiO2) has been synthesized by the reaction of 2-[[(2-benzhydryl-4,6-dimethylphenyl)mino]-methyl]-phenol with Ni(CH3COO)2·4 H2O, and characterized by elemental analysis and IR spectrum. The spatial structure of the complex has been confirmed by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group C2/c with a = 39.035(8), b = 13.276(3), c = 17.679(4) A°, β = 98.06(3)°, V = 9071(3) A°^3, C56H48N2NiO2, Mr = 839.67, Z = 8, Dc = 1.230 Mg/m^3, μ = 0.472 mm^-1, F(000) = 3536, T = 293(2) K, the final R = 0.0675 and w R = 0.1345(I 〉 2s(I)). The compound showed excellent catalytic activity up to 1.268 × 10^7 g of PNB(mol of Ni)^-1h^-1 for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.展开更多
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{1-[[(3-ethyl-6-methyl-2-pyridinyl)imino]methylenyl]- 2-na- phthalenola-to-N,O}nickel has been synthesized by the reaction of 1-[[(3-ethyl-6-methyl-2- pyridinyl) imino] methylenyl]-2-naphthalenol with Ni(CH3 COO)2 ·4H2 O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group Pbca with a = 11.100(2), b = 15.900(3), c = 18.000(4), V = 3176.8(11)3, C38 H34 N4 NiO2, Mr = 637.40, Z = 4, Dc = 1.333 g/cm3, μ = 0.651 mm-1, F(000) = 1336, the final R = 0.0783 and wR = 0.2119. This title compound was investigated for the catalytic behavior towards norbornene(NB) vinyl addition polymerization. And the complex exhibited good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.
基金Supported by the Ministry of Education of China(No.208066)the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. Single-crystal X-ray diffraction analysis results further confirmed the molecular structures. The crystal belongs to the monoclinic system, space group P2_1/c with a = 4.1324(2), b = 23.5432(16), c = 11.8943(8) A, β = 91.238(5)o, V = 1156.93(12) ?~3, C_(26)H_(20)Cl_2N_4O_2Pd, M_r = 597.76, Z = 2, D_c = 1.716 g/cm^3, μ = 1.067 mm^(-1), F(000) = 600, the final R = 0.0247 and w R = 0.0677(I 〉 2σ(I)). In the presence of methylaluminoxane(MAO), the complex exhibits excellent catalytic activities(1.737×10~7 g of PNB(mol of Pd)^(-1)·h^(-1)) in the vinyl polymerization of norbornene.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphthalenol with Ni(CH3COO)2·4H2O, and characterized by IR spectrum, elemental analysis and TG. The complicated space structure has been confirmed by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.410(4), b = 14.382(4), c = 18.121(6) ,A, β = 97.147(6)% V= 2950.5(16)A3, C36H32N4O2Ni, Mr = 611.37, Z = 4, Dc = 1.376 g/cm3, μ = 0.698 mm-1 F(000) = 1280, the final R = 0.0519 and wR = 0.1493 (1 〉2σ(I)). This title compound was used as precatalysts for the polymerisation of norbornene. When activated with MAO, the complex exhibited excellent catalytic activity up to 1.98 × 107 g ofPNB (mol of Ni)-1 h-1 with high monomer conversion.
基金Supported by the Ministry of Education of China (No. 208066)the Education Department of Fujian Province (JA07029)+1 种基金the Natural Science Foundation of Fujian Province (2010J01026)the State Key Laboratory of Structural Chemistry (No. 20080053)
文摘A novel polyoxometalate {[Ag^I(4,4'-bipy)]3[PW12O40]}·(4,4'-bipy)·4H2O 1 has been synthesized hydrothermally and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of 1 belongs to the triclinic system, space group P1 with a = 11.3710(17), b = 12.0701(16), c = 13.1061(12) A, α = 112.838(3), β = 94.545(6), γ = 99.526(4)°, V = 1614.4(4) A^3, Mr = 3825.40, Z = 1, Dc = 3.935, μ = 22.289mm^-1, F(000) = 1692, the final R = 0.0507 and wR = 0.1054. X-ray diffraction analysis reveals that the molecular structure of 1 consists of three coordinated cations [AgI(4,4'-bipy)]+, a polyanion unit [PW12O40]3-, and a discrete 4,4′-bipy molecule. Significantly, there exist two crystallographically independent silver(I) centers in 1 and all [AgI(4,4'-bipy)]^+ cations are linked with each other to form a one-dimensional Ag-4,4'-bipy polymer chain. The neighboring polymer chains are further interconnected to form a 3D framework by the covalent effect of silver atoms and terminal oxygen atoms of the polyanion. The electrochemical behaviors of 1 have also been studied in detail by cyclic voltammograms.
基金Project supported by the Natural Science Foundation of Fujian Province (E0310016) and the Education Committee Foundation of Fujian Province (JB05309)
文摘A Keggin-type tungstohosphate compound [Cu^l(2,2'-bipy)2]3[PW^Ⅵ12O40] 1 (bipy = bipyddine) was prepared by the hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C60H48Cu3N12O40PW12) crystallizes in the monoclinic system, space group P21/c with a = 16.9837(10), b = 17.9732(13) c = 27.8701(13)A°, β = 96.1039(10)°, V = 8459.2(9) A°^3, Mr = 4004.89, Z = 4, Dc = 3.145 g/cm^3, μ = 17.089 mm^-1, F(000) = 7208, S = 1.005, the final R = 0.0469 and wR = 0.0827 for 10807 observed reflections (I 〉 2σ(I)). Compound 1 consists of one discrete normal Keggin polyanion [PW^Ⅵ 12O40]^3- and three isolated coordinated cations [Cu^1(2,2'-bipy)2]^+. Significantly, there exist three crystallographically independent asymmetric reduced copper (I) centers in 1. Furthermore, the compound shows strong photoluminescence property in solid state at room temperature.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine-N,O}nickel has been synthesized by the reaction of(2-benzhydryl-4,6-dimethyl-phenyl)-(3,5-di-tert-butyl-2-methyl-benzylidene)-amine with Ni(CH3COO)2·4H2O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 12.373(4), b = 18.434(7), c = 27.814(10) A, β = 92.291(6)o, V = 6339(4) A^3, C7 2H8 0N2 Ni O2, Mr = 1064.09, Z = 4, Dc = 1.115 g/cm^3, μ = 0.350 mm^-1, F(000) = 2280, the final R = 0.0846 and wR = 0.2926(I 〉 2s(I)). This title compound was used as homogeneous catalysis of polymerization of norbornene, and the complex exhibited good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.
基金supported by the Key Project of Chinese Ministry of Education (No. 208066)Natural Science Foundation of Fujian Province (2007J0216, U0750004)+1 种基金Education Department of Fujian Province (JA07029)State Key Laboratory of Structural Chemistry (No. 20080053)
文摘The title compound,bromo-(2-diphenylphosphino-N-(2-oxybenzylidene)-aniline)- nickel,was synthesized by simple condensation of 2-diphenylphosphino-N-(2-oxybenzylidene)- aniline with NiBr2·6H2O and characterized by elemental analysis,IR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system,space group P1 with a = 9.756(2),b = 10.232(2),c = 13.313(3)A,α = 95.09(3),β = 102.48(3),γ = 95.45(3)o,V = 1283.5(4) A^3,C29H23BrNNiO2P,Mr = 587.07,Z = 2,Dc = 1.519 g/cm^3,λ(MoKα) = 0.71073 A,F(000) = 596 and μ = 2.402 mm^-1. The structure was refined to the final R = 0.0408 and wR = 0.0965 for 4507 observed reflections (I 〉 2σ(I)). Intermolecular π-π interactions (with distances of about 3.705 A) are pronounced in the crystal structure. Under methylaluminoxane (MAO) activation,the title compound was able to catalyze norbornene polymerization,exhibiting good polymerization activities.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex N,O-bis{2-[[(2-benzhydryl-4,6-dimethylphenyl)imino]-methyl]-phenol}-nickel(II)(C56H48N2NiO2) has been synthesized by the reaction of 2-[[(2-benzhydryl-4,6-dimethylphenyl)mino]-methyl]-phenol with Ni(CH3COO)2·4 H2O, and characterized by elemental analysis and IR spectrum. The spatial structure of the complex has been confirmed by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group C2/c with a = 39.035(8), b = 13.276(3), c = 17.679(4) A°, β = 98.06(3)°, V = 9071(3) A°^3, C56H48N2NiO2, Mr = 839.67, Z = 8, Dc = 1.230 Mg/m^3, μ = 0.472 mm^-1, F(000) = 3536, T = 293(2) K, the final R = 0.0675 and w R = 0.1345(I 〉 2s(I)). The compound showed excellent catalytic activity up to 1.268 × 10^7 g of PNB(mol of Ni)^-1h^-1 for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.