具有新颖嵌合作用的金属配合物的微波合成、晶体结构及性质研究

在微波辐射条件下合成了两种新的离子液体金属配合物[Ni(m-HNDA)2(H2O)4](1),[Zn(m-HNDA)2(H2O)4]·H2O(2),用元素分析、红外光谱、紫外光谱对它们进行了表征,通过X射线单晶衍射测定了它们的晶体结构.在晶体结构中,标题物通过基团间的嵌合作用,π-π相互作用和分子间氢键自组装成了三维网状的多孔结构.由氢键和π-π相互作用的强弱推测标题物的稳定性次序2>1,与实测热稳定性次序完全吻合;电化学性质表明,金属的配位改变了配体的循环伏安性质.另外,两种配合物可在水溶液中高选择性的识别氟离子.     

相对论磁控管透明阴极的仿真与实验

 基于一个6腔异腔结构相对论磁控管,运用粒子模拟仿真软件,对同轴阴极和透明阴极的特性进行仿真和实验研究。经仿真优化,设计并制作了一支3个带的透明阴极。粒子模拟结果表明,在相同条件下透明阴极比同轴阴极电子群聚时间大大缩短,起振时间大幅减小,整管效率提高约1倍,输出微波频谱更纯,模式竞争更小。实验结果表明,相同条件下,应用透明阴极所得到的微波脉宽较宽,在S波段获得721 MW的微波功率输出。说明应用透明阴极能缩短相对论磁控管起振时间,与粒子模拟结果相符。     

A Combined 6π-Azaelectrocyclization/Staudinger Approach to Protein and Cell Engineering: Noninvasive Tumor Targeting by N-Glycan-Engineered Lymphocytes

A Combined 6π-Azaelectrocyclization/Staudinger Approach to Protein and Cell Engineering: Noninvasive Tumor Targeting by N-Glycan-Engineered Lymphocytes

All authors

Katsunori Tanaka, Kaori Minami, Tsuyoshi Tahara, Eric R. O. Siwu, Koichi Koyama, Satoshi Nozaki, Hirotaka Onoe, Yasuyoshi Watanabe & Koichi Fukase

https://doi.org/10.1080/07328303.2010.483042

Published online:

02 June 2010

Graphical Abstract     

654.

Synthesis,Structure and Properties of a Novel Copper（II）-2,2- biimidazole Complex-supported Compound： [Cu（H2biim）2] { [Cu（H2biim）2]2 [H10W12O44] }.8H2O     

CHEN Wei-Peng  YI Xiao-Feng  SANG Rui-Li  XU Li 《结构化学》2013,(11):1696-1702

A new copper（II）-2,2＇-biimidazole metal-organic POMs-supported compound [Cu（H2biim）2]{[Cu（H2biim）212[H10W12O44]}＇8H2O （H2biim = 2,2＇-biimidazole） has been success- fully synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and TG. The crystal adopts space group Pi with a = 11.800（2）, b = 13.437（3）, c = 13.685（3） A, V = 1922.5（7） A3, D,. = 3.507 g/cm3, C36H62Cu3N24W12O52, M,. = 4059.92, F（000） = 1837,μ = 18.796 mm-1, Z = 1, R = 0.0579 and wR = 0.1465 for 8734 observed reflections （I 〉 2σ（I））. X-ray crystallography analysis exhibits that the title compound consists of one [H10W12044]6- polyanion and three [Cu（H2biim）2] units. And significant π-π stacking interactions and intermolecular O-H-,.O or N-H.＇-O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework. Thermal stability and magnetic property of the complex have also been investigated.     

655.

Inclusion Properties and Crystal Structure of Clathrates Constructed Based on “π-sandwich”     

Naoto Hayashi  Kumiko Yamaguchi  Kiyoshi Matsumoto 《Supramolecular chemistry》2013,25(1):45-52

Abstract

Inclusion behavior of structurally similar host compounds, 1,4-bis[1-(9-anthryl)-3-propen-1-on-3-yl]benzene (1) and 1,4-bis[3-(9-anthryl)-3-propen-1-on-1-yl]benzene (2), has been studied. Both hosts preferred cyclic, non-branched small molecules as a guest component, to yield 1:2 clathrates specifically. X-ray powder diffraction studies revealed that those 1:2 clathrates of 1 and 2 were respectively isostructural. X-ray analyses of (1)(THF)₂ (P 1, a = 10.910(2), b = 19.656(5), c = 9.172(4) Å, α = 95.58(3), β = 93.67(2), γ = 103.30(2)°, D _calc = 1.195 g cm^?3, Z = 2, and R = 0.067 for 8644 observed reflections) and (2)(1,4-dioxane)₂, (P2₁/n, a = 5.661(1), b = 17.971(3), c = 18.619(3) Å, β = 91.37(2)°, D _calc = 1.254 g cm^?3, Z = 2, and R = 0.097 for 4353 observed reflections) illuminated that their guest preference should be ascribed to the commonly observed π-sandwich” structure, in which guest molecules are enclathrated between two anthracene planes of the host molecules.     

656.

Catalytic reactions of bis-π-allylpalladium generated from allyltrifluoroborate     

Hiroyuki Nakamura  Kazuki Shimizu 《Tetrahedron letters》2011,52(3):426-429

Bis-π-allylpalladium-catalyzed nucleophilic allylations to aldehydes 2 and imines 3 have been achieved by replacing allylstannanes with allyltrifluoroborate. Amphiphilic bisallylation of activated olefins 6 with allyltrifluoroborate and allyl acetate also proceeded smoothly in the presence of Pd₂(dba)₃·CHCl₃ and tricyclohexylphosphine catalysts.     

657.

Synthesis, Crystal Structure and Luminescent Properties of [Zn（bipy）_2（H_2O）_4]·L·3H_2O     

陈友存  沈菲  王彦  许军军  汪快兵 《结构化学》2011,30(9):1251-1256

A novel coordination complex [Zn(bipy)2(H2O)4]·L·3H2O (1, bipy = 4,4'-bipyridine, LHNa = aniline-2,5-disulfonic acid monosodium salt) has been synthesized from LHNa by using hydrothermal method and structurally characterized. The result indicates that complex 1 belongs to the monoclinic system, space group P21/c with a = 20.392(3), b = 7.4052(12), c = 23.843(3) , β = 116.253(10)°, V = 3.2291(8) 3, Z = 4, Dc = 1.553 g·cm-3, μ = 0.962 mm-1, F(000) = 1568, and the final R = 0.0497 and wR = 0.1290. The complex 1 has a 0-D discrete structure, and generates an infinite 3-D network with the aid of O–H…O hydrogen bonds and π-π interactions.     

658.

The nonclassical noncovalent interactions control: A case study of the crystal structure of 3,5-dibromo-2-amino-4,6-dimethylpyridinium tetrahalocuprate [3,5-DBr-2-A-4,6-DMPH]₂CuX₄ (X = Cl, and Br)     

Murad A. AlDamen  Salim F. Haddad 《Journal of Molecular Structure》2011,985(1):27-33

The compound [3,5-dibromo-2-amino-4,6-dimethylpyridinium]₂CuCl₄, (1), was prepared from acidic hydrochloric acetonitrilic medium containing CuCl₂ and 3,5-dibromo-2-amino-4,6-dimethylpyridinium bromide while [3,5-dibromo-2-amino-4,6-dimethylpyridinium]₂CuBr₄, (2), from acidic HBr/Br₂ ethanolic medium containing 4,6-dimethylpyridine and CuBr₂. The ring got dibrominated at 3 and 5 positions in situ. Single-crystal X-ray diffraction proved the compounds to be isomorphous in P − 1. A systematic study of the crystallographic parameters in dibrominated and nonbrominated 2-amino-4,6-dimethylpyridine salts will explain the role of nonclassical noncovalent interaction between aryl bromine and ionic metal bromide in the control of structure.     

659.

Gemini表面活性剂与DNA在气/液界面上的相互作用     

康雪丽  陈启斌  尚亚卓  刘洪来 《物理化学学报》2011,27(6):1467-1473

在气/液界面上, 阳离子表面活性剂可以通过静电作用与阴离子型的脱氧核糖核酸(DNA)分子形成复合膜, 并压缩沉积得到LB(Langmuir-Blodget)膜. 利用表面压-表面积(π-A)曲线、原子力显微镜(AFM)和石英晶体微天平(QCM)研究了阳离子Gemini表面活性剂([C₁₈H₃₇(CH₃)₂N⁺-(CH₂)_s-N⁺(CH₃)₂C₁₈H₃₇]·2Br^-, 简写为18-s-18, s=3, 4, 6, 8, 10, 12)与DNA(双链DNA(dsDNA), 单链DNA(ssDNA))之间的相互作用, 并对18-s-18在不同下相表面的分子面积进行了比较. 实验结果表明连接基团和下相的DNA对Gemini表面活性剂在气/液界面上的性质有很大影响. 此外, Gemini表面活性剂在界面上对DNA的吸附能力与它们之间的相互作用方式密切相关.     

660.

苯并咪唑类离子液体及其铅(Ⅱ)配位聚合物的合成、晶体结构及电学性质研究     

刘勇  张有明  华茂堂  刘明霞  魏太保 《无机化学学报》2011,27(8):1569-1573

合成了新的离子液体金属配合物[Pb(m-HNA)(H2O)].NO3.3H2O(m-HNA为N,N′-二-羧甲基-2-丙基苯并咪唑盐),并通过元素分析,红外光谱,对其进行了表征,通过X射线单晶衍射测定了其晶体结构,在晶体结构中,标题物通过π-π相互作用、分子间氢键和配位键自组装成了三维网状结构。另外,电化学性质表明,该配合物的电解过程为准可逆过程。     

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Synthesis,Structure and Properties of a Novel Copper（II）-2,2- biimidazole Complex-supported Compound： [Cu（H2biim）2] { [Cu（H2biim）2]2 [H10W12O44] }.8H2O

A new copper（II）-2,2＇-biimidazole metal-organic POMs-supported compound [Cu（H2biim）2]{[Cu（H2biim）212[H10W12O44]}＇8H2O （H2biim = 2,2＇-biimidazole） has been success- fully synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and TG. The crystal adopts space group Pi with a = 11.800（2）, b = 13.437（3）, c = 13.685（3） A, V = 1922.5（7） A3, D,. = 3.507 g/cm3, C36H62Cu3N24W12O52, M,. = 4059.92, F（000） = 1837,μ = 18.796 mm-1, Z = 1, R = 0.0579 and wR = 0.1465 for 8734 observed reflections （I 〉 2σ（I））. X-ray crystallography analysis exhibits that the title compound consists of one [H10W12044]6- polyanion and three [Cu（H2biim）2] units. And significant π-π stacking interactions and intermolecular O-H-,.O or N-H.＇-O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework. Thermal stability and magnetic property of the complex have also been investigated.     

Inclusion Properties and Crystal Structure of Clathrates Constructed Based on “π-sandwich”

Abstract

Inclusion behavior of structurally similar host compounds, 1,4-bis[1-(9-anthryl)-3-propen-1-on-3-yl]benzene (1) and 1,4-bis[3-(9-anthryl)-3-propen-1-on-1-yl]benzene (2), has been studied. Both hosts preferred cyclic, non-branched small molecules as a guest component, to yield 1:2 clathrates specifically. X-ray powder diffraction studies revealed that those 1:2 clathrates of 1 and 2 were respectively isostructural. X-ray analyses of (1)(THF)₂ (P 1, a = 10.910(2), b = 19.656(5), c = 9.172(4) Å, α = 95.58(3), β = 93.67(2), γ = 103.30(2)°, D _calc = 1.195 g cm^?3, Z = 2, and R = 0.067 for 8644 observed reflections) and (2)(1,4-dioxane)₂, (P2₁/n, a = 5.661(1), b = 17.971(3), c = 18.619(3) Å, β = 91.37(2)°, D _calc = 1.254 g cm^?3, Z = 2, and R = 0.097 for 4353 observed reflections) illuminated that their guest preference should be ascribed to the commonly observed π-sandwich” structure, in which guest molecules are enclathrated between two anthracene planes of the host molecules.     

Catalytic reactions of bis-π-allylpalladium generated from allyltrifluoroborate

Bis-π-allylpalladium-catalyzed nucleophilic allylations to aldehydes 2 and imines 3 have been achieved by replacing allylstannanes with allyltrifluoroborate. Amphiphilic bisallylation of activated olefins 6 with allyltrifluoroborate and allyl acetate also proceeded smoothly in the presence of Pd₂(dba)₃·CHCl₃ and tricyclohexylphosphine catalysts.     

Synthesis, Crystal Structure and Luminescent Properties of [Zn（bipy）_2（H_2O）_4]·L·3H_2O

A novel coordination complex [Zn(bipy)2(H2O)4]·L·3H2O (1, bipy = 4,4'-bipyridine, LHNa = aniline-2,5-disulfonic acid monosodium salt) has been synthesized from LHNa by using hydrothermal method and structurally characterized. The result indicates that complex 1 belongs to the monoclinic system, space group P21/c with a = 20.392(3), b = 7.4052(12), c = 23.843(3) , β = 116.253(10)°, V = 3.2291(8) 3, Z = 4, Dc = 1.553 g·cm-3, μ = 0.962 mm-1, F(000) = 1568, and the final R = 0.0497 and wR = 0.1290. The complex 1 has a 0-D discrete structure, and generates an infinite 3-D network with the aid of O–H…O hydrogen bonds and π-π interactions.     

The nonclassical noncovalent interactions control: A case study of the crystal structure of 3,5-dibromo-2-amino-4,6-dimethylpyridinium tetrahalocuprate [3,5-DBr-2-A-4,6-DMPH]2CuX4 (X = Cl, and Br)

The compound [3,5-dibromo-2-amino-4,6-dimethylpyridinium]₂CuCl₄, (1), was prepared from acidic hydrochloric acetonitrilic medium containing CuCl₂ and 3,5-dibromo-2-amino-4,6-dimethylpyridinium bromide while [3,5-dibromo-2-amino-4,6-dimethylpyridinium]₂CuBr₄, (2), from acidic HBr/Br₂ ethanolic medium containing 4,6-dimethylpyridine and CuBr₂. The ring got dibrominated at 3 and 5 positions in situ. Single-crystal X-ray diffraction proved the compounds to be isomorphous in P − 1. A systematic study of the crystallographic parameters in dibrominated and nonbrominated 2-amino-4,6-dimethylpyridine salts will explain the role of nonclassical noncovalent interaction between aryl bromine and ionic metal bromide in the control of structure.     

Gemini表面活性剂与DNA在气/液界面上的相互作用

在气/液界面上, 阳离子表面活性剂可以通过静电作用与阴离子型的脱氧核糖核酸(DNA)分子形成复合膜, 并压缩沉积得到LB(Langmuir-Blodget)膜. 利用表面压-表面积(π-A)曲线、原子力显微镜(AFM)和石英晶体微天平(QCM)研究了阳离子Gemini表面活性剂([C₁₈H₃₇(CH₃)₂N⁺-(CH₂)_s-N⁺(CH₃)₂C₁₈H₃₇]·2Br^-, 简写为18-s-18, s=3, 4, 6, 8, 10, 12)与DNA(双链DNA(dsDNA), 单链DNA(ssDNA))之间的相互作用, 并对18-s-18在不同下相表面的分子面积进行了比较. 实验结果表明连接基团和下相的DNA对Gemini表面活性剂在气/液界面上的性质有很大影响. 此外, Gemini表面活性剂在界面上对DNA的吸附能力与它们之间的相互作用方式密切相关.     

苯并咪唑类离子液体及其铅(Ⅱ)配位聚合物的合成、晶体结构及电学性质研究

合成了新的离子液体金属配合物[Pb(m-HNA)(H2O)].NO3.3H2O(m-HNA为N,N′-二-羧甲基-2-丙基苯并咪唑盐),并通过元素分析,红外光谱,对其进行了表征,通过X射线单晶衍射测定了其晶体结构,在晶体结构中,标题物通过π-π相互作用、分子间氢键和配位键自组装成了三维网状结构。另外,电化学性质表明,该配合物的电解过程为准可逆过程。