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.
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.
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.
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.
The title complex N,O-bis{2-[[(2,6-benzhydryl-4-methylphenyl)imino]-methyl]-phenol}-palladium(II)(C_(80)H_(64)N_2O_2 Pd) has been synthesized by the reaction of 2-[[(2,6-benzhydryl-4-methylphenyl)imino]-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. The spatial structure of the complex has been verified by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group P21/n with a = 13.492(3), b = 16.924(3), c = 14.135(3) ?, β = 97.84(3)°, V = 3197.4(11) ?~3, C_(80)H_(64)N_2O_2 Pd, Mr = 1191.73, Z = 2, Dc = 1.238 Mg/m^3, μ = 0.339 mm^(-1), F(000) = 1240, T = 293(2) K, the final R = 0.0593 and wR = 0.1192(I > 2s(I)). The compound showed excellent catalytic activity up to 1.130 × 10~7 g of PNB(mol of Pd)^(-1)h^(-1) for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.
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.
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.