四核钴羰基簇合物Co4(CO)8(μ-CO)2(μ4-PSR)2的合成和晶体结构

The title compounds Co4(CO)8(μ-CO)2 (μ4-PSR) [R=-CH3, -C2H5, -C(CH3)3,-(CHa)4CH3] were synthesized by the reaction of Co2(CO)8 with RSPCl2. They were characterized by IR, 1HNMR, elemental analysis. The crystal and molecular structure of Co4(Co)8(μ-CO)2 (μ4-PSC2H5) has been determined by single crystal diffraction method. Crystal data: monoclinic, space group P21 /c, with a=8-445(3), 6=8.562(3), c= 17.125(6)Å, β=104.26 (3)' 9 V=1200.1Å3, Z=2, Dc=1.937gcm-3. Its molecular structure contains an octahedral Co4P2 skeleton which consists of a rectangular four cobalt atoms core and the Co4 core is capped above and below by two quadruply bridging PSR ligands.     

Molecular films of water-miscible ionic liquids formed on glassy carbon electrodes: characterization and electrochemical applications

This letter describes the formation and possible electrochemical applications of molecular films of water-miscible imidazolium-based ionic liquids (ILs) on glassy carbon (GC) electrodes. X-ray photoelectron spectroscopy (XPS) and electrochemical results indicate that the water-miscible ILs used in this study can interact with the GC electrode and form molecular films on the electrode surface. The formed molecular films are found to possess striking electrochemical properties such as electrocatalysis toward ascorbic acid (AA) and the capability to facilitate direct electron transfer of horseradish peroxidase (HRP). This demonstration would pave the way for new electrochemical applications of water-miscible ILs and is envisaged to be useful for the investigation of the electrochemical properties of water-miscible ILs in aqueous media provided the same counteranion is used as the supporting electrolyte.     

土壤中绿黄隆残留量分析方法的研究

本文确立了土壤中绿黄隆残留量的间接气相色谱分析方法，用０．１５ｍｏｌ／Ｌ ＮａＨＣＯ３提取土样，二氯甲烷洗涤初步纯化后，在水浴上加热水解，再用二氯甲烷萃取，弗罗里硅土柱净化，最后用气相色谱－电子捕获检测器检测水解产物邻氯苯磺酰胺。土壤中添加回收率７８．５％－９０．８％，检测极限０．３ｎｇ／ｇ。     

17电子钒开环夹心羰基配合物的合成及XRD,IR,EPR研究

以４种甲基取代戊二烯基为配体合成了４个过渡金属钒开环夹心羰基配合物［２，４－（ＣＨ３）２Ｃ５Ｈ５］２ＶＣＯ（Ｉ），［２，３－（ＣＨ３）２Ｃ５Ｈ５］ＶＣＯ（Ⅱ），［２－ＣＨ３Ｃ５Ｈ６］２ＶＣＯ（Ⅲ）和［３－ＣＨ３Ｃ５Ｈ６］２ＶＣＯ（Ⅳ），其中Ⅱ，Ⅲ，Ⅳ为新配合物，用Ｘ射线单晶衍射，ＩＲ，ＥＰＲ法对所合成配合物进行了结构表征，发现Ｉ具有两种晶相。     

An in situ STM study on the long-range surface restructuring of Au(1 1 1) in a non-chloroaluminumated ionic liquid

We report an in situ STM study of a potential-dependent long-range surface restructuring of Au(1 1 1) electrode in neat 1-butyl-3-methylimidazolium tetrafluoroborates (BMIBF₄) ionic liquid. Au(1 1 1) undergoes a significant long-range surface restructuring upon cathodic excursion to −1.0 V vs. Pt quasi-reference. The restructuring involves the formation of tiny pits, which then develops into a stable worm-like network with an average width of the network grids 2 nm. Electrochemical annealing occurs at the cathodic limit with the presence of a reduction product of cation BMI⁺. A smooth surface is recovered with the appearance of the typical (√3 × 22) reconstruction of Au(1 1 1). The surface restructuring is reestablished upon anodic excursion to −1.3 V after the adsorbed reduction product is oxidized. The long-range surface restructuring phenomenon is tentatively explained as a result of partial charge transfer to the weakly adsorbed BMI⁺, which reduces the metal–metal cohesive energy. In addition, the synergetic effect of the counter anion BF₄⁻ may also be involved. The results provide a knowledge of Au(1 1 1) electrode behavior in the neat ionic liquid and are beneficial to understanding in situ STM results involving surface morphological changes in such a media.     

手性5-l-(艹孟)氧基丁内酯并[3,4-d]-3-取代基-异(口恶)唑啉类化合物的合成

研究了手性元5-(R)-(l-(艹孟)氧基)-2(5H)-呋喃酮与取代苯甲醛肟以次氯酸钙作为氧化剂进行的区域选择性原位1,3-偶极环加成反应,同步生成两个新的手性中心,得到了一系列光学纯丁内酯并[3,4-d]-3-取代基-异(口恶)唑啉类化合物;应用波谱学手段及X射线单晶衍射法确证了产物的绝对构型,并对产物的核磁共振氢谱规律性加以总结.     

互通多孔碳/二氧化锰纳米复合材料的原位水热合成及电化学性能

以互通多孔碳（IPC）为载体，水热条件下在碳表面原位反应生成纳米结构的二氧化锰（MnO₂），制备互通多孔碳/二氧化锰纳米（IPC/MnO₂）复合电极材料. 采用扫描电镜（SEM），透射电镜（TEM），X射线衍射（XRD），热重分析（TGA）对其结构进行表征；采用循环伏安法、恒流充放电和交流阻抗对其电化学性能进行研究. 结果表明：生成的MnO₂均匀地负载在碳的表面，形成多层次结构，并且随着温度的升高IPC表面负载的MnO₂由纳米颗粒变为纳米片状结构；MnO₂纳米片具有典型的K-Birnessite 型晶体结构；复合物中MnO₂的含量约为34%（w）. 在100 ℃制备的IPC/MnO₂复合材料在三电极系统中最高比电容达到了411 F·g^-1；随着反应温度的升高,比容量先增长后基本保持不变. 以IPC/MnO₂为正极，活性炭（AC）为负极，1 mol·L^-1 Na₂SO₄溶液为电解液组装成IPC/MnO₂//AC 混合超级电容器，发现IPC/MnO₂电极的电容器其电位窗口从1 V扩展到1.8 V，容量可达86F·g^-1，且表现出良好的电容特性和大电流放电性能.     

微波作用下2,5-二取代-1,3,4-噁二唑的合成

2 ,5 二取代 1 ,3 ,4 二唑可用作药品 ,光敏物质 ,闪烁体 ,激光材料 ,高分子液晶单体等[1- 5] 。一种是以芳香酸与水合肼作为原料用多聚磷酸作为脱水环合剂来合成此类化合物[6 ] ,另一种是由芳香酸转变为芳香酰氯或酯 ,再与水合肼反应得到单酰肼或二酰肼 ,最后用三氯氧磷[7] ,五氧化二磷和五氯化磷[8] ,一氯三甲硅[9] 脱水环合 ;此外 ,用水合肼和尿素合成得到的氨基脲代替水合肼 ,与芳香酸缩合合成二唑[10 ] ,这些方法共同的缺陷是 :环合时间较长 ,少者 4～ 5ｈ ,多则 8ｈ。近年来 ,微波技术在有机合成及其杂环化合物的合成中得到了广…     

Diaqua­bis[2′‐(4,5‐diaza­fluoren‐9‐yl­idene)picolinohydrazidato‐κ2N,O]zinc(II) tetra­hydrate: a metal–water chain complex containing cyclic water hexa­mers

In the title compound, [Zn(C₁₇H₁₀N₅O)₂(H₂O)₂]·4H₂O, cyclic water hexa­mers forming one‐dimensional metal–water chains are observed. The water clusters are trapped by the co‐operative association of coordination inter­actions and hydrogen bonds. The Zn^II ion resides on a centre of symmetry and is in an octa­hedral coordination environment comprising two O atoms and two N atoms from two 2′‐(4,5‐diaza­fluoren‐9‐yl­idene)picolinohydrazidate ligands and two water mol­ecules.     

Cu（I）/Diamine-catalyzed Aryl-alkyne Coupling Reactions

Arylalkynes are important building blocks for the synthesis of natural products,pharmaceuticals,and artificial molecular devices1.They are often synthesized via the Pd-catalyzed Sonogashira coupling reactions between aryl halides and terminal alkynes2,3.Unfortunately,it remains difficult to apply the Sonogashira reaction to industrial scale and/or pharmaceutical synthesis,due to the high cost of Pd and the difficulty in removing the toxic Pd residues from the reaction products.Thus it is wor…