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 1,3-diphenyl-2-((quinolin-8-ylamino)methylene)propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-((quinolin-8-ylamino)-methylene)propane-1,3-dione with PdCl2, and ...The title complex 1,3-diphenyl-2-((quinolin-8-ylamino)methylene)propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-((quinolin-8-ylamino)-methylene)propane-1,3-dione with PdCl2, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group P21212 with a = 21.838(4), b = 8.3952(17), c = 11.497(2) A, V= 2107.9(7) A3, C25H17C1N2O2Pd, Mr = 519.26, Z= 4, Dc= 1.636 g/cm3, H = 1.032 mm-1, F (000) = 1040, the final R = 0.0307 and wR = 0.0778. This compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the complex exhibits excellent catalytic activities up to 2.18×10^8g of PNB (tool of Pd)-1 h-1 with high monomer conversion using methylaluminoxane (MAO) as the cocatalyst.展开更多
The title complex, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927(6), b = 11.079(6), c = 11.233(6) ?, a = 73.970(12), β = 85.738(16), γ = 83.300(12)o...The title complex, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927(6), b = 11.079(6), c = 11.233(6) ?, a = 73.970(12), β = 85.738(16), γ = 83.300(12)o, V = 1178.1(11) ?3, Mr = 648.55, Z = 2, Dc = 1.520 g/cm3, μ = 1.884 mm-1, F(000) = 634, the final R = 0.0460 and wR = 0.1280. This title compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the complex exhibits good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.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 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 phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elem...A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elemental analysis, TG, WAXD spectra, ^1H NMR and ^(13)C NMR. In addition, the molecular structure has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 14.510(6), b = 18.573(7), c = 20.961(6) A, β = 123.453(19)°, V = 4713(3)A^3, Mr = 867.73, Z = 4, Dc = 1.223 g/cm^3, μ = 0.456 mm^-1, F(000) = 1832, the final R = 0.0685 and wR = 0.1758(I 〉 2σ(I)). The complex was used as homogeneous catalysis of polymerization of norbornene, and the MAO as cocatalyst. The nickel complex exhibited good catalytic activity up to 1.913 × 10^7 g of PNB(mol of Ni)^-1h^-1,and the yields of these reactions depend on the nature of the substituent in the aromatic ring.展开更多
A novel salicylaldimine ligand and its mononuclear nickel complex [NiL](L = 2-[[[2,6-bis(diphenylmethyl)-4-methylphenyl]imino]methyl]phenol) have been synthesized and characterized by IR spectrum, elemental analys...A novel salicylaldimine ligand and its mononuclear nickel complex [NiL](L = 2-[[[2,6-bis(diphenylmethyl)-4-methylphenyl]imino]methyl]phenol) have been synthesized and characterized by IR spectrum, elemental analysis and thermogravimetry(TG). The molecular structure of the complex has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/n with a = 13.281(3), b = 16.938(3), c = 13.981(3) ?, β = 97.03(3)o, V = 3121.2(11) A^3, C80H64N2O2Ni, Mr = 1144.04, Z = 2, Dc = 1.217 Mg/m^3, μ = 0.361 mm^-1, F(000) = 1204, the final R = 0.0582 and wR = 0.1108(I 〉 2s(I)). The compound showed excellent catalytic activity up to 12.78 × 10^6 g of PNB(polynorbornene)(mol of Ni)^-1 h^-1 for the addition polymerization of norbornene(NB) by using methylaluminoxane(MAO) as a cocatalyst.展开更多
The title complex N,N'-bis(2-benzoyl-3-oxobutane)-trans-l,2-diaminocyclo- hexane-palladium (C28H28N2PdO4) has been synthesized by the reaction of N,N'-bis(2- benzoyl-3-oxobutane)-trans-l,2-diamino-cyclohexane ...The title complex N,N'-bis(2-benzoyl-3-oxobutane)-trans-l,2-diaminocyclo- hexane-palladium (C28H28N2PdO4) has been synthesized by the reaction of N,N'-bis(2- benzoyl-3-oxobutane)-trans-l,2-diamino-cyclohexane with PdCI2, and characterized by ele- mental analysis, IR spectrum, WAXD and TG. The spatial structures of the complex have been confirmed by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic system, space group C2/c with a = 29.763(6), b = 10.320(2), c = 18.921(4) A, fl = 102.75(3)°, V = 5668(2) A3, C28H28N2PdO4·CH3OH, Mr = 594.97, Z = 8, Dc = 1.394 g/cm3, μ(MoKa) = 0.694 mm-1, F(000) = 2448, T= 293(2) K, R = 0.0572 and wR = 0.1347 (I〉 2σ(I)). The compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the palladium complex showed excellent catalytic activity up to 9.97x 106g of PNB (mol of Pd)-1 h-1 with high monomer conversion using methylaluminoxane (MAO) as a cocatalyst.展开更多
The title complex bis{1-[[(3-methyl-pyridin-2-yl) amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium(C_(42)H_(56)O_2N_4Pd) has been synthesized by the reaction of 1-[[(3-methyl-pyridin-2-yl)a...The title complex bis{1-[[(3-methyl-pyridin-2-yl) amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium(C_(42)H_(56)O_2N_4Pd) has been synthesized by the reaction of 1-[[(3-methyl-pyridin-2-yl)amino]methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol with Pd(OAc)_2, and was characterized by IR and elemental analyses(C, H, N). Single-crystal X-ray diffraction analysis of the complex revealed an almost parallelogram geometry of the metal center, space group P1 with a = 12.3870(13), b = 12.9673(12), c = 14.3998(4) ?, α = 67.53(2), β = 75.34(2), γ = 86.89(3)°, V = 2065.5(3) A3, M_r = 773.32, Z = 2, D_c = 1.243 g/cm^3, μ = 0.489 mm^(-1), F(000) = 816, the final R = 0.0649 and wR = 0.1567. The compound was investigated for the catalytic behavior towards norbornene(NB) vinyl addition polymerization. And the complex exhibits high catalytic activities up to 1.668 × 10~7 g of PNB(mol of Pd)^(-1) h^(-1) with high monomer conversion using methylaluminoxane(MAO) as the cocatalyst.展开更多
Polynorbornenes were synthesized in the presence of an iron based catalyst, 2,6-bis[1-(2,6-diisopropyl-phenylimino)ethyl]pyridine iron(Ⅱ) dichloride. The FTIR, 1H NMR and 13C NMR analysis results revealed t...Polynorbornenes were synthesized in the presence of an iron based catalyst, 2,6-bis[1-(2,6-diisopropyl-phenylimino)ethyl]pyridine iron(Ⅱ) dichloride. The FTIR, 1H NMR and 13C NMR analysis results revealed that the structure of the obtained polynorbornenes consisted of vinyl addition polymer substructures without any ring-opening structures. The polymers were amorphous with a short-range order, displayed in the WAXD(wide angle X-ray diffraction) diagrams. The glass transition temperatures ranged from 200 to 400 ℃. The effects of the polymerization reaction conditions, such as Al/Fe molar ratio and toluene/CH_2Cl_2 volume ratio, on the activity, intrinsic viscosity and T_g were also studied.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
The title complex N,O-bis{[2-[(2,4-dimethylphenyl)imino]-5-methoxyl]-phenol}-palladium(Ⅱ)(CC_(32)H_(32)N_2O_4Pd) has been synthesized by the reaction of 2-[(2,4-dimethylphenyl)imino]-5-methoxyl-phenol wit...The title complex N,O-bis{[2-[(2,4-dimethylphenyl)imino]-5-methoxyl]-phenol}-palladium(Ⅱ)(CC_(32)H_(32)N_2O_4Pd) has been synthesized by the reaction of 2-[(2,4-dimethylphenyl)imino]-5-methoxyl-phenol with Pd(CH_3COO)_2,and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P2_1/c with a = 12.058(2),b = 8.3624(17),c = 14.735(3) ?,β = 107.66(3)°,V = 1415.7(5)?~3,C_(32)H_(32)N_2O_4Pd,Mr = 615,Z = 2,D_c = 1.443 Mg/m^3,μ = 0.695 mm^(-1),F(000) = 632,T = 293(2) K,the final R = 0.0514 and w R = 0.1356(I 〉 2s(I)).Under the co-catalysis of methylaluminoxane(MAO),the palladium compound exhibited favorable catalytic activity for the polymerization of norbornene(NB).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
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 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 1,3-diphenyl-2-((quinolin-8-ylamino)methylene)propane-l,3- dione-palladium was synthesized by the reaction of 1,3-diphenyl-2-((quinolin-8-ylamino)-methylene)propane-1,3-dione with PdCl2, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group P21212 with a = 21.838(4), b = 8.3952(17), c = 11.497(2) A, V= 2107.9(7) A3, C25H17C1N2O2Pd, Mr = 519.26, Z= 4, Dc= 1.636 g/cm3, H = 1.032 mm-1, F (000) = 1040, the final R = 0.0307 and wR = 0.0778. This compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the complex exhibits excellent catalytic activities up to 2.18×10^8g of PNB (tool of Pd)-1 h-1 with high monomer conversion using methylaluminoxane (MAO) as the cocatalyst.
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, C20H17N4Pd2Cl3·0.5CH3OH, crystallizes in the triclinic system, space group Pī with α = 9.927(6), b = 11.079(6), c = 11.233(6) ?, a = 73.970(12), β = 85.738(16), γ = 83.300(12)o, V = 1178.1(11) ?3, Mr = 648.55, Z = 2, Dc = 1.520 g/cm3, μ = 1.884 mm-1, F(000) = 634, the final R = 0.0460 and wR = 0.1280. This title compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the complex exhibits good catalytic activity to catalyze norbornene polymerization using MAO as a cocatalyst.
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 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)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elemental analysis, TG, WAXD spectra, ^1H NMR and ^(13)C NMR. In addition, the molecular structure has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 14.510(6), b = 18.573(7), c = 20.961(6) A, β = 123.453(19)°, V = 4713(3)A^3, Mr = 867.73, Z = 4, Dc = 1.223 g/cm^3, μ = 0.456 mm^-1, F(000) = 1832, the final R = 0.0685 and wR = 0.1758(I 〉 2σ(I)). The complex was used as homogeneous catalysis of polymerization of norbornene, and the MAO as cocatalyst. The nickel complex exhibited good catalytic activity up to 1.913 × 10^7 g of PNB(mol of Ni)^-1h^-1,and the yields of these reactions depend on the nature of the substituent in the aromatic ring.
基金Supported by the Natural Science Foundation of Fujian Province(2007J0216)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structure Chemistry(No.20130013)
文摘A novel salicylaldimine ligand and its mononuclear nickel complex [NiL](L = 2-[[[2,6-bis(diphenylmethyl)-4-methylphenyl]imino]methyl]phenol) have been synthesized and characterized by IR spectrum, elemental analysis and thermogravimetry(TG). The molecular structure of the complex has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/n with a = 13.281(3), b = 16.938(3), c = 13.981(3) ?, β = 97.03(3)o, V = 3121.2(11) A^3, C80H64N2O2Ni, Mr = 1144.04, Z = 2, Dc = 1.217 Mg/m^3, μ = 0.361 mm^-1, F(000) = 1204, the final R = 0.0582 and wR = 0.1108(I 〉 2s(I)). The compound showed excellent catalytic activity up to 12.78 × 10^6 g of PNB(polynorbornene)(mol of Ni)^-1 h^-1 for the addition polymerization of norbornene(NB) by using methylaluminoxane(MAO) as a cocatalyst.
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,N'-bis(2-benzoyl-3-oxobutane)-trans-l,2-diaminocyclo- hexane-palladium (C28H28N2PdO4) has been synthesized by the reaction of N,N'-bis(2- benzoyl-3-oxobutane)-trans-l,2-diamino-cyclohexane with PdCI2, and characterized by ele- mental analysis, IR spectrum, WAXD and TG. The spatial structures of the complex have been confirmed by single-crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic system, space group C2/c with a = 29.763(6), b = 10.320(2), c = 18.921(4) A, fl = 102.75(3)°, V = 5668(2) A3, C28H28N2PdO4·CH3OH, Mr = 594.97, Z = 8, Dc = 1.394 g/cm3, μ(MoKa) = 0.694 mm-1, F(000) = 2448, T= 293(2) K, R = 0.0572 and wR = 0.1347 (I〉 2σ(I)). The compound was investigated for the catalytic behavior towards norbornene (NB) vinyl addition polymerization. And the palladium complex showed excellent catalytic activity up to 9.97x 106g of PNB (mol of Pd)-1 h-1 with high monomer conversion using methylaluminoxane (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{1-[[(3-methyl-pyridin-2-yl) amino] methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol} palladium(C_(42)H_(56)O_2N_4Pd) has been synthesized by the reaction of 1-[[(3-methyl-pyridin-2-yl)amino]methyl-phenyl]-2-hydroxy-3,5-di-tert-butylphenol with Pd(OAc)_2, and was characterized by IR and elemental analyses(C, H, N). Single-crystal X-ray diffraction analysis of the complex revealed an almost parallelogram geometry of the metal center, space group P1 with a = 12.3870(13), b = 12.9673(12), c = 14.3998(4) ?, α = 67.53(2), β = 75.34(2), γ = 86.89(3)°, V = 2065.5(3) A3, M_r = 773.32, Z = 2, D_c = 1.243 g/cm^3, μ = 0.489 mm^(-1), F(000) = 816, the final R = 0.0649 and wR = 0.1567. The compound was investigated for the catalytic behavior towards norbornene(NB) vinyl addition polymerization. And the complex exhibits high catalytic activities up to 1.668 × 10~7 g of PNB(mol of Pd)^(-1) h^(-1) with high monomer conversion using methylaluminoxane(MAO) as the cocatalyst.
基金Supported by the Special Funds for Major State Basic Research Projects( No.G19990 64 80 0 ),the National NaturalScience Foundation of China( No.2 973 4141) ,and SKL EP ( 0 0 62 ) ,SINOPEC and CNPC.
文摘Polynorbornenes were synthesized in the presence of an iron based catalyst, 2,6-bis[1-(2,6-diisopropyl-phenylimino)ethyl]pyridine iron(Ⅱ) dichloride. The FTIR, 1H NMR and 13C NMR analysis results revealed that the structure of the obtained polynorbornenes consisted of vinyl addition polymer substructures without any ring-opening structures. The polymers were amorphous with a short-range order, displayed in the WAXD(wide angle X-ray diffraction) diagrams. The glass transition temperatures ranged from 200 to 400 ℃. The effects of the polymerization reaction conditions, such as Al/Fe molar ratio and toluene/CH_2Cl_2 volume ratio, on the activity, intrinsic viscosity and T_g were also studied.
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.
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-[(2,4-dimethylphenyl)imino]-5-methoxyl]-phenol}-palladium(Ⅱ)(CC_(32)H_(32)N_2O_4Pd) has been synthesized by the reaction of 2-[(2,4-dimethylphenyl)imino]-5-methoxyl-phenol with Pd(CH_3COO)_2,and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P2_1/c with a = 12.058(2),b = 8.3624(17),c = 14.735(3) ?,β = 107.66(3)°,V = 1415.7(5)?~3,C_(32)H_(32)N_2O_4Pd,Mr = 615,Z = 2,D_c = 1.443 Mg/m^3,μ = 0.695 mm^(-1),F(000) = 632,T = 293(2) K,the final R = 0.0514 and w R = 0.1356(I 〉 2s(I)).Under the co-catalysis of methylaluminoxane(MAO),the palladium compound exhibited favorable catalytic activity for the polymerization of norbornene(NB).
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.