Crystal and Molecular Structures of Two Derivatives of 1, 3a, 5-Trisubstituted-3a ,4,5,11-Tetrahydro-1,2,4-Oxadiazolino[5,4-d] [1, 5]Benzothiazepine

The structures of two derivatives of the title compound [C24H22N2OS, Mr = 386. 5 for (1); C25H22N2O3S, Mr = 430. 5 for (2)] were determined by using X-ray single-crystal strcuture analysis method. The final discrepancies are R = 0. 071 and 0. 077, respectively, for the reflections measured on a four-circle diffractometer. The space group for compound (1) is P bca with a=1. 6639(4), b=2.0286(3), c= 1.1742(1) nm, V = 3. 964(1) nm3, F(000) = 1632 e, Z=8; and (2) belongs to P21/n space group, and the cell dimensions are a=1. 1115(4), b=0. 8932(7), c=2. 186(3) nm, β=97. 52 (1)°? V=2.151(4) nm3, F(000) = 904 e, Z=4.The molecular backbones are very similar, each is a tricyclic system. The central seven-membered ring is in a twisted-boat conformation, and is cis-fused to 1,2,4-oxa-diazolino ring, while the latter moiety is in an envelope form. There are conjugated but non-coplanar effects in each structure. All bond lengths and angles in the molecules are normally acceptable. The crystal structure on the whol     

Tb~(3 )在MO(M=Ca,Sr)中的长余辉发光

长余辉发光材料的研究与应用,已有近100年的历史,目前仍在许多领域中有着重要应用[1].此类材料与其他光致发光材料具有相同的发光性能,只是更注重其发光的衰减过程和热释光性能.如,ZnS:Cu作为黄绿色的长余辉发光材料,在1992年以前是余辉性能最好的长余辉发光材料,一直处于发光研究工作的中心.     

试剂加入次序不同造成镉对肝脂质过氧化的诱导或拮抗作用

采用TBA检测方法，体外观察了CaCl2对大鼠线粒体脂质过氧化产物丙二醛(MDA)生成的毒性作用和对半胱氨酸-Fe^2 诱导的线粒体脂质过氧化的影响。结果表明，1 μmol／L～1mol／L CdCl2均能诱导肝线粒体的脂质过氧化，使MDA含量增加，但只有CdCl2浓度高于1 mmol／L时，诱导作用才与对照组有显著性差异。在Fe^2 -Cd^2 半胱氨酸共同对肝线粒体作用时，由于试剂加入顺序的不同，100～1000 mmol／L CdCl2对线粒体脂质过氧化可产生诱导或拮抗作用。结果提示，CdCl2可直接诱导线粒体脂质过氧化，在做几种金属离子体外协同对肝脂质过氧化影响的实验时，应考虑试剂加入顺序所产生的不同影响。     

六甲氧基甲基三聚氰胺-多元醇-丙烯酸酯混杂聚合体系的研究

六甲氧基甲基三聚氰胺 (HMMM) 多元醇 丙烯酸酯 酸催化剂混杂聚合体系在高温下同时进行缩聚和自由基聚合并表现出协同效应 .体系中的活泼亚甲基在HMMM的催化下被空气氧化成过氧化氢物 ;过氧化氢物在酸催化下分解成自由基进而引发自由基聚合反应 .研究结果表明 ,体系中存在固化加速的协同效应 ;同时体系中还存在热互补效应 ,丙烯酸酯的自由基聚合反应放出的热可以传递给缩聚反应 ,满足缩聚反应吸热的要求 .混杂聚合得到的高分子合金膜具有优良的机械性能和耐溶剂性能 ,这是由于在混杂聚合过程中形成了互穿聚合物网络 (IPN)结构 .使用潜酸催化剂作为酸的来源 ,可以提高体系的储存稳定性 ;交联 引发剂的使用可以拓宽它的使用范围 ;对超枝化聚合物在混杂体系中的应用也进行了初步研究     

顺式-二(乙二胺)二硝基合钴(Ⅲ)苹果酸盐的晶体结构及手性识别

合成了标题化合物，并用X-射线衍射法确定了该分子的晶体结构。化合物Δ（λλ），Λ（δδ）－cis－[Co（en）2（NO2）2]2d，l-C4H4O5，Co2C12N12O13H22，Mr=657．94．晶体属单斜晶系，空间群为P21/c，晶胞参数：a=13．969（4），b=6.440（1），c＝14．408（4）A，β=94.37（1）°，V=1292．3A3，Z=2，Dc=1．69g／cm3，μ=105.833cm－1，F（000）=668.最终偏离因子R=0.066，Rw=0．085。结构分析表明晶体存在无序现象，其阴离子C4H4O52-有两种排列方式。R-构型和S-构型的几率各为50％，手性识别是通过Δ构型的阳离子与阴离子R-构型C原子上羟基氧形成氢键相互作用；Λ构型的阳离子与阴离子S-构型C原子上羟基氧形成氢键相互作用而实现的。     

引入离子基团改善聚苯乙烯和热致液晶聚合物的相容性Ⅰ.热性能和形态

ＤＳＣ和ＳＥＭ研究结果表明聚苯乙烯与一种热致液晶聚合物完全不相容。共混体系具有与组分无关的Ｔｇ，并且表现出明显的两相结构。将ＰＳ进行化学改性，随中和盐离子的变化有；酸式，Ｌｉ，Ｎａ，Ｚｎ和Ｍｎ盐五种形式。用ＤＳＣ和ＳＥＭ对ＬＣＰ与ＳＰＳ共混物的热性能和形态进行了分析和表征。     

A Highly Sensitive Spectrophotometric Assay of Bleomycins Based on the Fading Reaction of Some Halofluorescein Dyes

In weak acidic medium, anticancer antibiotics bleomycin A5 （BLMA5） and bleomycin A2 （BLMA2） can react with halofluorescein dyes such as erythrosin （Ery）, eosin Y （EY）, eosin B （EB） and rose bengal （RB） by virtue of electrostatic attraction and hydrophobic force to form the ion-association complexes, which can result in the fading reactions of four halofluorescein dyes. The maximum fading wavelengths of these four dyes were located at 527 nm for Ery, 515 nm for EY, 517 nm for EB and 546 nm for RB, respectively. The decrements of absorbance （AA） were directly proportional to the concentrations of bleomycin in a certain range. A new method for the determination of bleomycins anticancer drugs based on fading reactions of halofluorescein dyes has been developed. The method was not only highly sensitive but also simple and rapid. The molar absorptivities （ε） ranged from 1.5 × 10^5 to 7.5 × 10^5 L·mol^-1·cm^-1. It was applied to determination of the bleomycins in human serum, urine and rabbit serum samples. In this work, the spectral properties and the optimum reaction conditions were investigated. The structure of ion-association complexes and the reaction mechanism were discussed.     

Rapid Fabrication of Hollow SiO2 Spheres with Novel Morphology

The hydrolysis of tetraethoxysilane (TEOS) occurred on the surface of poly(methyl methacrylate) (PMMA) microshperes immediately after these microshperes were prepared in TEOS. Micron-sized hollow SiO2 spheres were obtained by calcination of the coated PMMA microshperes. It was found that the final hollow spheres were constituted by small SiO2 particles.     

反相微乳液法制备纳米Al2O3颗粒及其形成反应机理的研究

通过聚乙二醇辛基苯基醚(曲拉通X-100)/正丁醇/环己烷/水溶液形成的体系, 采用反相微乳液法合成了Al₂O₃纳米粒子. 对前驱体进行热分析(TG-DTG-DTA), 确定了合适的煅烧温度为1150 ℃. 采用X射线衍射(XRD)、透射电镜(TEM)、紫外可见分光光度法(UV-vis)分别对产物的结构、粒度和形貌进行了表征, 考察了微乳液中水与表面活性剂的物质的量之比(ω_o)、煅烧温度和煅烧时升温速率等关键因素对产物形貌和晶相的影响, 并通过分析进一步揭示了Al₂O₃纳米粒子的形成机理. 结果表明, 控制ω_o为10、煅烧温度为1150 ℃可得到分散性好、粒径分布均匀的Al₂O₃纳米粒子, 且2 ℃/min的升温速率更有利于产物向稳定的α晶相转变.     

有机磷化合物的质谱研究(Ⅵ)——磷酰二胺酯类化合物的电子轰击质谱和化学电离质谱

本文报道了7种新的N-烷基-N′-乙氧羰基甲基-N′-芳磺酰基-O-乙基磷酰二胺酯化合物的电子轰击质谱(EIMS)和化学电离质谱(CIMS,甲烷为反应气)。结果表明,无论是EIMS,还是CIMS均存在较多的骨架重排离子峰;取代基对谱图有较大的影响;EIMS中P—N键的断裂为重要质谱特征,CIMS中MH~+准分子离子为重要特征离子,还存在分子离子反应的产物。