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1.
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) ?, 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.  相似文献   

2.
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.  相似文献   

3.
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.  相似文献   

4.
A new 1D copper(Ⅱ) polymer [Cu(Hpt)(3,5-DMBA)]n has been hydrothermally synthesized with copper acetate,3-(pyridin-2-yl)-1,2,4-triazole(Hpt) and 3,5-dimethylbenzoic acid(3,5-DMBA). It crystallizes in triclinic space group P1,with a = 8.1974(6),b = 8.3280(6),c = 12.5021(9) ?,α = 84.3320(10),β = 71.8870(10),γ= 65.4560(10)o,V = 737.44(9) ?~3,Dc = 1.612 g/cm3,Z = 2,F(000) = 366,GOOF = 1.035,R = 0.0298 and w R = 0.0855. The crystal structure is a one-dimensional(1-D) chain in which the Cu(Ⅱ) is five-coordinated with square pyramidal geometry. The crystal structure shows that the whole molecule consists of two copper ions bridged by two μ12-η:η0-3,5-dimethylbenzoic acid anions and two 3-(pyridin-2-yl)-1,2,4-triazole molecules. The coordination environment of Cu(Ⅱ) ion is CuO+2N_3. The luminescence and thermal properties of the complex were investigated.  相似文献   

5.
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(CH_3COO)_2·4H_2O, and characterized by IR spectrum and single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P2_1/c with a = 12.373(4), b = 18.434(7), c = 27.814(10) ?, β = 92.291(6)o, V = 6339(4) ?~3, C7 2H8 0N2 Ni O_2, M_r = 1064.09, Z = 4, D_c = 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.  相似文献   

6.
Novel chiral tetraaza ligands(R)-N,N′-bis[2-(piperidin-1-yl)benzylidene]propane-l,2-diamine 6 and(S)-N-[2-(piperidin-l- yl)benzylidene]-3-{[2-(piperidin-1-yl)benzylidene]amino}-alanine sodium salt 7 have been synthesized and fully characterized by NMR,IR,MS and CD spectra.The catalytic property of the ligands was investigated in Ir-catalyzed enantioselective transfer hydrogenation of ketones.The corresponding optical active alcohols were obtained with high yields and moderate ees under mild reaction conditions.  相似文献   

7.
A new binuclear nickel(Ⅱ) complex [Ni_2(C_7 N_4 H_5)_3(C_9 H_9 O_2)]n has been hydrothermally synthesized with nickel sulfate, 3-(pyridin-2-yl)-~1 H-1,2,4-triazole and 3,5-dimethylbenzoic acid(3,5-DMBA). It crystallizes in the triclinic space group P1 with a = 11.5769(7), b = 12.3115(7), c = 12.6431(7) ?, α = 81.4860(10)o, β = 64.2830(10)o, γ = 63.7130(10)o, V = 1453.45(15) ?~3, D_c = 1.604 g/cm~3, Z = 2, F(000) = 720, the final GOOF = 1.048, R = 0.0285 and wR = 0.0628. The crystal structure shows that the whole molecule consists of two nickel ions bridged by three μ_2-η~1:η~0-3-(pyridin-2-yl)-1,2,4-triazole anions. The coordination environment of Ni(Ⅱ) ion is NiO_2 N_4 and NiN_5, giving a distorted octahedral geometry and square pyramidal geometry respectively. The luminescence and thermal properties of the complex were investigated.  相似文献   

8.
The title complex 1,3-diphenyl-2-((quinolin-8-ylamino)methylene)propane-1,3-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), V = 2107.9(7)3 , C25H17ClN2O2Pd, Mr = 519.26, Z = 4, Dc = 1.636 g/cm3 , μ = 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 2.18×108 g of PNB (mol of Pd)-1 h-1 with high monomer conversion using methylaluminoxane (MAO) as the cocatalyst.  相似文献   

9.
2,4-Bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine(bpt) has been synthesized by using a new, simple and general method with high yields. Reactions of bpt with Ni(CIO4)2 · 6H2O and Zn(CIO4)2 · 6H2O in methanol gave mononuclear complex [Ni(bpt)2] · (CIO4)2 · H2O and ternary complex [Zn(mpt)2(dmp)](CIO4)2 respectively, where mpt (2,4-dimethoxy-6-(3,5-dimethyl-pyrazol-1-yl)-1,3,5-triazine) and dmp(3,5-dimethylpyrazole) are the alcoholysis products of bpt in the presence of Zn2+ ion. A possible mechanism for this catalytic reaction was proposed. X-ray crystal structure for ligand bpt, Ni and Zn complexes are reported. The protonated form of the ligand bpt crystallizes as its perchlorate salt including one molecule of water, [Hbpt · H2O · CIO4]. The proton is located on one pyrazole N-atom. [Hbpt ?H2O ?CIO4], in which [Hbpt]+ is in cis-cis conformation, are packed in slipped stacks of approximately parallel layers. The π-π overlap interactions between the non-protonized pyrazoles of the adjace  相似文献   

10.
A novel crystal with the molecular formula [Pd(DCA)(bipy)]2 [Pd(bipy)Cl2 ]·6.75H2O was formed by PdCl2 with disodium demethylcantharate (Na2 (DCA),DCA2= 7-oxa-bicyclo[2.2.1]heptane-2,3-bicarboxylate) and 2,2-bipyidine (bipy) through the hydrothermal method.The complex was characterized by elemental analysis and infrared spectroscopy.The structure of the complex was determined by single-crystal X-ray diffraction,which is of triclinic system,space group P1 with a=13.6818(7),b=14.8426(8),c=15.0043(8),α=97.319(3),β=92.521(3),γ=105.776(2)°,V=2898.4(3) 3,Dc=1.545 g·cm-3,Z=1,F(000)=1420,S=0.852,the final R=0.0525 and wR=0.1777 for 13634 observer reflections (I>2σ(I)).The binding reaction of the complex with ct-DNA and bovine serum albumin (BSA) was studied by fluorescence spectroscopy.The results indicated that the complex binds to ct-DNA via the partial intercalation.The binding constant K A of the complex interaction with BSA was 3.98×10 5 L·mol-1 and one binding site would be formed.The antiproliferative activity of the complex against human hepatoma cells (SMMC7721) in vitro is much higher than that of Na 2 (DCA).  相似文献   

11.
The title compound has been synthesized and characterized crystallographically. It is a co-crystal consisting of two different neutral zinc(Ⅱ) complexes with Hbpbm (Hbpbm = 4-bromo-2-(benzimidazol-2-yl)phenol) and Hnpbm (Hnpbm = 2-(1-butylbenzimidazol-2-yl)phenol).One is a monomeric mixed-ligand complex of [Zn(bpbm)(npbm)] 1 and the other a dimer of[Zn2(npbm)4] 2 with their ratio of 2:1. Thus the overall formula for the title compound is 21·2.Adjacent 1 and 2 are connected to each other by intermolecular hydrogen bonding interactions in the lattice. The crystal data: monoclinic, space group P21/c, a= 15.0141(12), b = 20.9941(17), c =18.4686(15) (A), β = 97.445(2)°, V= 5772.4(8) (A)3, Mr= 2429.68, Z = 2, Dc = 1.398 g/cm3,μ = 1.579mm-1, F(000) = 2504, R = 0.0637 and wR = 0.1771 for 6464 observed reflections (I> 2σ(Ⅰ)). The geometrical structure for 1 has also been theoretically optimized and compared with the experimental one.  相似文献   

12.
<正>A novel mercury(n)complex HgL_2Br_2 was prepared from HgBr_2 and the organic ligand 2-(N-methyl-N-(4-((E)-2-(pyridine-4-yl)vinyl)phenyl)amino)ethanol(L).The ligand was synthesized and then characterized by FT-IR spectroscopy,~1H NMR,mass spectrum and elemental analysis,while the single-crystal diffraction data of the complex were collected on a Siemens Smart CCD diffractometer.The complex crystallizes in triclinic space group P_1~-with a=5.367(5),b= 12.466(5),c=23.945(5)(?),α=90.812(5),β=96.318(4),γ=96.093(5)°,Z=2,D_c=1.817g·cm~(-3),μ=7.395 mm~(-1),S=0.825,and the final R=0.0396.The Hg(Ⅱ)ion in the distorted tetrahedral mercury(Ⅱ)complex C_(32)H_(36)HgBr_2N_4O_2 is coordinated by two N atoms from the two ligands together with two bromide ions.Solid-state emission of the ligand and its complex has been investigated at room temperature.  相似文献   

13.
The title complex N,N-bis(2-benzoyl-3-oxobutane)-trans-1,2-diaminocyclohexane-palladium(C28H28N2PdO4) has been synthesized by the reaction of N,N-bis(2-benzoyl-3-oxobutane)-trans-1,2-diamino-cyclohexane with PdCl2,and characterized by elemental 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) ,β = 102.75(3)°,V = 5668(2) 3,C28H28N2PdO4·CH3OH,Mr = 594.97,Z = 8,Dc = 1.394 g/cm3,μ(MoKα) = 0.694 mm-1,F(000) = 2448,T = 293(2) K,R = 0.0572 and wR = 0.1347(I 2(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 9.97×106 g of PNB(mol of Pd)-1 h-1 with high monomer conversion using methylaluminoxane(MAO) as a cocatalyst.  相似文献   

14.
苏清  赵天琦  张杰  李佩  赵晴  叶玲 《结构化学》2014,(2):237-243
6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxa- zine(1) was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3(C28 H35 Cl3 N2 O, Mr = 521.93) belongs to the triclinic system, space group P1 with a = 10.852(2), b = 11.352(2), c = 13.050(3), α = 101.95(3), β = 92.94(3), γ = 114.64(3)o, V = 1412.4(5)3, Z = 2, Dc = 1.227 g/cm3, F(000) = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725(I 2?(I)). The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H···O interactions, intermolecular C–H···N interactions, C–H···π interactions, and π···π interactions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.  相似文献   

15.
The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthalenolato-N,O}-nickel(Ⅱ)(C36H32N4O2Ni) has been synthesized by the reaction of 1-{[(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) , β = 97.147(6)°, V = 2950.5(16) 3, 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(Ⅰ 2δ(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 of PNB(mol of Ni)-1 h-1 with high monomer conversion.  相似文献   

16.
A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C_(58)H_(52)N_2NiO_2](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 P2_1/c with a = 14.510(6), b = 18.573(7), c = 20.961(6) ?, β = 123.453(19)°, V = 4713(3) ?~3, M_r = 867.73, Z = 4, D_c = 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)~(-1)h~(-1),and the yields of these reactions depend on the nature of the substituent in the aromatic ring.  相似文献   

17.
Reaction of a new type of bidentate ligand PhPQu [ PhPQu = 2-diphenylphosphino-4-methylquinoline] with Fe(CO)5 in bu-tanol gave trans-Fe(PhPQu-P)(CO)3 (1).Compound 1,which can act as a neutral tridentate organometallic ligand,was reacted with I B,II B metal compounds and a rhodium complex to give six binuclear complexes with Fe-M bonds,Fe(CO)3(u-Ph2PQu)MXn(2-7) [M=Zn(Ⅰ),Cd(Ⅱ),Hg(Ⅱ),Cu(Ⅰ),Ag(Ⅰ),Rh(Ⅰ)],and an ion-pair complex [Fe(CO)3(n-Ph2PQu)2HgI][HgI3]- (8).The structure of 8 was determined by X-ray crystallography.Complex 8 crystallizes in the space group P-1 with a=1.0758(3),b= 1.6210(4),c = 1.7155(4) nm; a = 75.60(2)β=71.81(2),Y = 81.78(2) and Z = 2 and its structure was refined to give agreement factors of R =0.050 and Rw = 0.057.The Fe-Hg bond distance is 0.2536 nm.  相似文献   

18.
The complex [Cd(bbb)Cl2]·DMF·H2O, where bbb is 2-(2-(1H-benzo[d]imidazol-2-yl)benzyl)-1H-benzo[d]imidazole, was synthesized and characterized by X-ray single-crystal structure analyses. For the complex: C24H25Cl2CdN5O2, Mr = 598.77, crystal system, triclinic, space group P1, a = 9.9878(12), b = 10.0008(12), c = 13.2217(15) , α = 80.674(2), β = 72.158(2), γ = 86.776(2)°, V = 1240.5(3) 3, Z = 2, Dc = 1.598 g/cm3, λ = 0.71073, μ(MoKα) = 1.127 mm–1, F(000) = 600, S = 1.04, R = 0.0905 and wR = 0.3088 for 4805 observed reflections with I 2σ(I). It is a neutral complex. The distorted tetrahedral geometry of cadmium ion is coordinated by two nitrogen atoms of ligand and two chloride ions. The complex emits blue green luminescence with emission peaks at 480 nm in DMF solution.  相似文献   

19.
Two monomeric cobalt(Ⅱ)complexes,[CoL(N3)] ClO4(1)and CoL(N3)2(2),where L is tris((3,5-dimethylpyrazol-1-yl)methyl)amine,were synthesized and their crystal structures were determined by X-ray diffraction technique.Complex 1 is five coordinated with one azide nitrogen atom and four nitrogen atoms of the tris((3,5-dimethylpyrazol-l-yl)-methyl)amine ligand,and the metal center is in distorted trigonal bipyramidal environment.Complex 2 is six coordinated distorted octahedron with the two azide nitrogen atoms and four nitrogen donors of the tris((3,5-dimethylpyrazol-1-yl)-methyl)amine ligand.The solution behaviors of the title complexes have been further investigated by UV-Vis,and 1H NMR analysis.It is found that the formation of 1 and 2 depends on the molar ratio of the azide ion to metal salt and ligand Complex 1 attached with one azide group is more stable and easy to generate than complex 2 incorporated with two azide groups,and the reasons were well discussed.  相似文献   

20.
手性铜(Ⅱ)-席夫碱配合物催化苯乙烯不对称环丙烷化反应   总被引:22,自引:0,他引:22  
Twelve chiral copper(Ⅱ) Schiff base complexes, derived from (R) (+) 2 amino 1,1 diaryl 1 propanol with substituted salicylaldehydes, were examined as a catalyst for asymmetric cyclopropanation of styrene with ethyl diazoacetate. It was found that the substituents at 3 and 5 positions of salicylaldehyde in the ligands had great effects on catalytic activity and enantioselectivity of the catalyst. The complex with strong electron withdrawing group (NO 2) at 5 position and the smallest stereo hinder (H) at 3 position of salicylaldehyde showed highly catalytic activity and enantioselectivity, up to ee =87 4% for trans and ee =82 8% for cis isomers respectively, and the ratio 39/61 of cis to trans isomers was obtained at 40 ℃ with 1,2 dichloroethane as solvent.  相似文献   

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