2,9-Diformyl-l, 10-phenanthrolinebis（2,6-dimethylanil）cobalt（Ⅱ） perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space grou...2,9-Diformyl-l, 10-phenanthrolinebis（2,6-dimethylanil）cobalt（Ⅱ） perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294（4）, b = 15.122（3）, c = 20.640（4） A, β = 119.618（4）°, V = 6048.9（19） A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F（000） = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections （I 〉 2σ（I））. In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.展开更多
An efficient synthetic method was developed to synthesize 2-substituted benzimidazoles and benzo- xazoles with β-keto esters as starting materials under mild reaction conditions, during which other functional groups ...An efficient synthetic method was developed to synthesize 2-substituted benzimidazoles and benzo- xazoles with β-keto esters as starting materials under mild reaction conditions, during which other functional groups are bearable from reactants to products.展开更多
The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1...The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1H/13C--NMR. Theproposal concerning mechanism was discussed herewith and the structure was reportedas well. Crystallographic data: Mr= 563. 85, monoclinicl P21/n(# 14); a= 8. 009(2), b= 17. 600(5), c=12. 003(4) A; β=95. 91(2)°; V= 1683. 0 (9) A3; Z=4;Dc=2. 22 g. cm-3; F(000) = 1048, μ=89. 27 cm-1 ; final R=0. 039 and Rw=0. 049for 2121 observable reflections with (I≥3. cσ(I) ). The crystal structure determinationshows that S atom coordinates to all three metal (W,Fe,Co) atoms in a μ3,-fashion,thetitle cluster core has the tetrahedral skeleton.展开更多
The title nickel complex （C34H3oCl2N2NiO4, Mr = 660.21） has been synthesized and its crystal structure was determined by single-crystal X-ray structure analysis. It crystallizes in the monoclinic system, space group...The title nickel complex （C34H3oCl2N2NiO4, Mr = 660.21） has been synthesized and its crystal structure was determined by single-crystal X-ray structure analysis. It crystallizes in the monoclinic system, space group P21/n with a = 11.026（8）, b = 11.491（8）, c = 12.119（9） A°, β=91.328（13）°, Z= 2, V= 1535.0（19） ,A°^3, Dc = 1.428 g/cm^3, F（000） = 684 andμ（MoKa） = 0.848 mm^-1 The structure was refined to R = 0.0544 for 1813 observed reflections with I 〉 2σ（I） and wR =0.0867 for 3132 unique reflections. The molecule of the complex is high symmetrical. Ni（Ⅱ） atom is located in the symmetric center and coordinated to two phenolic oxygen and two imino nitrogen atoms, forming two six-membered rings. Upon activation with methylaluminoxane （MAO）, it is active for ethylene oligomerization.展开更多
文摘2,9-Diformyl-l, 10-phenanthrolinebis（2,6-dimethylanil）cobalt（Ⅱ） perchlorate was synthesized and demonstrated to be [COL2][ClO4]2 by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group C2/c with a = 22.294（4）, b = 15.122（3）, c = 20.640（4） A, β = 119.618（4）°, V = 6048.9（19） A^3, C63H52Cl2CoN9O9, Mr= 1208.97, F（000） = 2504, De= 1.328g/cm^3, Z = 4, μ= 0.436, the final R = 0.0712 and wR = 0.1718 for 1734 observed reflections （I 〉 2σ（I））. In its solid state the helical polymeric chains are supramolecularly associated through intermolecular and interionic hydrogen bonding interactions.
基金Supported by the National Natural Science Foundation of China(No.20874105)the Foundation of Hebei Education Department China(No.2010268)
文摘An efficient synthetic method was developed to synthesize 2-substituted benzimidazoles and benzo- xazoles with β-keto esters as starting materials under mild reaction conditions, during which other functional groups are bearable from reactants to products.
文摘The chiral sulfido cluster (η5-C5H5)WFeCo(CO)8(μ3--S) was synthesized by refluxing a solution of HFe2Co(CO)9 (μ3,--S) and (η5-C5H5)Fe(CO)3Cl in tetrahydrofuran. It was characterized by elemental analysis, IR and 1H/13C--NMR. Theproposal concerning mechanism was discussed herewith and the structure was reportedas well. Crystallographic data: Mr= 563. 85, monoclinicl P21/n(# 14); a= 8. 009(2), b= 17. 600(5), c=12. 003(4) A; β=95. 91(2)°; V= 1683. 0 (9) A3; Z=4;Dc=2. 22 g. cm-3; F(000) = 1048, μ=89. 27 cm-1 ; final R=0. 039 and Rw=0. 049for 2121 observable reflections with (I≥3. cσ(I) ). The crystal structure determinationshows that S atom coordinates to all three metal (W,Fe,Co) atoms in a μ3,-fashion,thetitle cluster core has the tetrahedral skeleton.
基金This work was supported by the National Natural Science Foundation of China (No. 20272062 and 20473099) and National 863 Project (2002AA333060)
文摘The title nickel complex （C34H3oCl2N2NiO4, Mr = 660.21） has been synthesized and its crystal structure was determined by single-crystal X-ray structure analysis. It crystallizes in the monoclinic system, space group P21/n with a = 11.026（8）, b = 11.491（8）, c = 12.119（9） A°, β=91.328（13）°, Z= 2, V= 1535.0（19） ,A°^3, Dc = 1.428 g/cm^3, F（000） = 684 andμ（MoKa） = 0.848 mm^-1 The structure was refined to R = 0.0544 for 1813 observed reflections with I 〉 2σ（I） and wR =0.0867 for 3132 unique reflections. The molecule of the complex is high symmetrical. Ni（Ⅱ） atom is located in the symmetric center and coordinated to two phenolic oxygen and two imino nitrogen atoms, forming two six-membered rings. Upon activation with methylaluminoxane （MAO）, it is active for ethylene oligomerization.
