Synthesis and Structure of Dimolybdenum Carbonyl Thiolate Compound [Et4N]2[Mo2（CO）8（SC6H4—CH3—m）2]

1 INTRODUCTION In 1984, thiolate ligand was successfully introduced into molybdenum carbonyl compound by the reaction of Mo(CO)6 with [Et4N]SR( R = C6H5, But) in a moderate condition[1]. From then on, a series of dinuclear molybdenum(0) carbonyl thiolate compounds have been synthesized and characterized by using a variety of thiolate ligands in our research group. It was found that a planar Mo2S2 unit is in the compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-p)2][2] (2) and a "butterfly" t…     

α—Keggin结构钼硅酸两电子还原杂多蓝的合成及晶体结构

用电解还原法制得标题化合物H6SiMoγ2Moи10O10·10H2O,该晶体为深蓝色,属三斜晶系,P1空间群,晶胞参数:a=1.4077(3)nm,b=1.4176(3)nm,c=1.3752(2)nm;α=111.04(1)°;β=93.99(1)°,γ=119.09(1)°;Z=2,R=0.52.分析结果表明,钼硅酸还原后八面体有所畸变.     

单核铁(Ⅲ)双卟啉配合物在溶液中的构象平衡及其对环己烷羟化反应的催化活性的影响

合成及表征了一系列以柔韧碳氢链相连不同长度的ｐ／ｐ型单核铁（Ⅲ）双卟啉配合物，以可见光谱首次观察到该系列配合物在氯仿溶液中开放式及闭合式构象的平衡，发现６８０ｎｍ处吸收峰强度与这种构象平衡有关，烷氧链越长，该吸收峰强度越大．利用该类配合物模拟了细胞色素Ｐ４５０单加氧酶对环己烷的羟化作用，催化结果表明，在以分子氧为氧源及还原剂存在的温和条件下，该类配合物的催化活性显著高于单核铁卟啉（ＦｅＴＰＰＣｌ），随着柔韧碳氢链长度的增加，双卟啉的催化活性依次增加．高的催化活性与双卟啉配合物在溶液中的构象平衡，即闭合式构象引起的立体位阻及电子转移有关．     

疏水缔合型增稠剂聚(丙烯酰胺-丙烯酸高级酯)的合成及增稠性能研究

采用沉淀聚合法合成了聚（丙烯酰胺－丙烯酸十四酯），聚（丙烯酰胺－丙烯酸十六酯）和聚（丙烯酰胺－丙烯酸十八酯），重点讨论了共聚物中疏水基团数量及疏水基团链长对增稠性能的影响。采用凯达尔定氮法和动态热分析（DMTA）测定了共聚物的组成及玻璃化温度。     

D,L-1,2,2-三甲基环戊烷-1,3-二胺硝酸镍配合物的合成、结构及其和手性D-(+)-1,2,2-三甲基环戊烷-1,3-二胺氯化镍配合物的对比分析(英)

A nickel(Ⅱ) complex [Ni(La)₂](NO₃)₂ (1) with bidentate racemic 1,2,2-trimethylcyclopentane-1,3-diamine ligand has been synthesized and characterized by IR, EA, ES-MS, and its X-ray diffraction study reveals that the nickel(Ⅱ) center is tetra-coordinated by one D- and one L- diamine ligands, and a three-dimensional hydrogen-bond-sustained network is formed in the solid state by means of the eight-membered N-H…O hydrogen bond cycle. This compound also supplies a good comparison to the chiral complex [Ni(L_b)₂]Cl₂·2H₂O (2) (L_b=D-(+)-1,2,2-trimethylcyclopentane-1,3-diamine). CCDC: 218122.     

用1H-和13C-NMR方法研究聚对苯二甲酸乙二酯/聚一氧基苯甲酸酯共聚酯的序列分布

 测定了PET/30PHB和PET/60PHB共聚酯的高分辨¹H和¹³C谱,并采用INEPT方法和部分弛豫FT技术确定了季碳吸收峰,对NMR谱进行了归属.应用我们先前提出的方法对共聚酯的序列分布进行了表征.结果表明,两种共聚酯的无规度B_q值均小于1,序列分布不象Jackson等认为的那样为完全无规的.此外,文中还指出,某些研究者套用Flory公式判别PET/PHB共聚酯是否为无规的不妥之处.     

LB膜诱导Ba(NO3)2晶体取向生长

In this work, Ba(NO₃)₂ crystals with single crystal face were induced by using the the method of bio-mimetic mineralization and double LB films of behenic acid (BA) as the template. The crystals were characterized by Scanning Electron Microscope (SEM) and X-Ray Diffraction (XRD). The crystals were observed in regular square shape with uniform size about 5～8 μm by SEM, and they were found by XRD to grow along the (111) plane. From these experiments, we can conclude that the good selection of the (111) crystal face of Ba(NO₃)₂ is due to the electrostatic interactions , the match between this crystal face and the definite lattice structure of the LB films.     

反相高效液相色谱法测定3种中成药中的葛根素

 建立了测定小儿清感灵片、步长新脑心通胶囊和感冒清热颗粒 3种中成药中葛根素含量的反相高效液相色谱方法。采用APEXODS色谱柱 ,以醋酸铵缓冲液 (10 0mmol/L ,pH 5 0 ) 甲醇 (体积比为 75∶2 5 )的混合溶液为流动相 ,检测波长为 2 5 0nm ,流速为 0 8mL/min。葛根素在 2mg/L～ 2 0mg/L时其色谱峰面积与质量浓度的线性关系良好 (r =0 9999) ;上述 3种中成药中的葛根素含量分别为 3 48mg/g ,1 0 8mg/ g及 1 5 2mg/ g(蔗糖型 ) ;其加样回收率分别为 99 0 % ,93 4%和 97 5 %。该法简便、快速、专属性强 ,可以作为多种中药制剂中葛根素含量的测定方法。     

阳极氧化膜WO3（Ⅱ）：电显色的介质效应

用循环计时电量法、循环伏安法、电化学现场(in-situ)紫外可见反射光谱技术和光电流谱技术研究了溶剂和阳离子(H~+,Li~+)对阳极氧化膜WO_3电显色稳定性和过程的影响。从循环计时电量图可以测定表征膜稳定性的氢或锂的累积量和暂态周期数。实验发现W/WO_3/LiCLO_4乙腈溶液体系具有高的电显色稳定性。引起WO_3膜可逆电显色的H~+和Li~+离子的嵌-脱过程的界面电化学机理不同。着色态WO_3膜的色心是自由电子,其密度超过10~(21)/cm~3,生色机理是等离子体振荡。     

联萘冠醚的合成新方法

一种用于合成含联萘基冠醚的新方法。以消旋，手性联萘酚为起始原料，先与氯乙醇反应制得2,2'-二（2－羟基乙氧基）－1,1'－联二苯，再与二甘醇或三甘醇对二对甲苯磺酸酯反应，成功制得了4种联萘冠醚。