Crystal structure and thermal stability of A μ1,1-(OMe)-bridged dimeric Schiff base iron(III) complex

A new μ_1,1-OMe-bridged dimeric iron(III) complex, [Fe₂L₂(μ_1,1-OMe)₂(NCS)₂], where L is the deprotonated form of 2-[(2-ethylaminoethylimino)methyl]-5-methoxyphenol, has been prepared and structural characterized by elemental analysis, IR spectrum, and single crystal X-ray crystallography. The complex crystallizes in the monoclinic space group P2₁/c, with unit cell dimensions a = 10.156(1) Å, b = 11.972(1) Å, c = 14.256(2) Å, β = 102.643(3)°, V = 1691.3(3) ų, Z = 2, R ₁ = 0.0394, and wR ₂ = 0.0922. Each Fe atom in the complex is in an octahedral coordination. The Fe...Fe distance is 3.102(1) Å. The thermal stability of the complex was studied.     

Synthesis of a Nine-atom Germanium Cluster K_(0.5)[K(18-crown-6)]_(1.5)Ge_9·1.5en with Unprecedented “up” and “down” Chain Arrangement of Unit [-(Ge_9-K-Ge_9)~(3-)-]

A new complex K0.5[K(18-crown-6)]1.5Ge9·1.5en(1) which contains unprecedented "up" and "down" chain arrangement of unit [-(Ge-9-K-Ge9)3-] has been prepared by the reaction of K4Ge9 with HgS in ethylenediamine(en) in the presence of 18-crown-6(1,4,7,10,13,16-hexaoxacyclooctadecane), and characterized by X-ray structure analysis. The color of the title crystals(black), which is darker than that of the reported three compounds with chains of germanium clusters, may result from the naked K+ and their interactions with the chain. And the structure differences between 1 and the reported three compounds with chains of germanium have also been discussed.     

水介质中ATRP法制备PDMAEMA及其温敏性

在30℃下以溴化亚铜-溴化铜混合物为催化剂,五甲基二乙烯三胺(PMDETA)为配体,在水介质中利用原子转移自由基聚合法(ATRP)合成聚合度达到300的聚甲基丙烯酸N,N-二甲基氨基乙酯(PDMAEMA)。核磁共振结果显示,聚合反应符合一级反应动力学描述。利用紫外可见分光光度计(UV-Vis)表征该聚合物的温敏性,结果表明,随着PDMAEMA聚合物链长的增加,其最低临界溶解温度(LCST)可降低至31.4℃。     

Tuning the Reactivity of Cyclopropenes from Living Ring‐Opening Metathesis Polymerization (ROMP) to Single‐Addition and Alternating ROMP

Ring‐opening metathesis polymerization (ROMP) has become one of the most important living polymerizations. Cyclopropenes (CPEs) remain underexplored for ROMP. Described here is that the simple swap of 1‐methyl to 1‐phenyl on 1‐(benzoyloxymethyl)CPEs elicited strikingly different modes of reactivity, switching from living polymerization to either selective single‐addition or living alternating ROMP. The distinct reactivity stems from differences in steric repulsions at the Ru alkylidene after CPE ring opening. Possible olefin or oxygen chelation from ring‐opened CPE substituents was also observed to significantly affect the rate of propagation. These results demonstrate the versatility of CPEs as a new class of monomers for ROMP, provide mechanistic insights for designing new monomers with rare single‐addition reactivity, and generate a new functionalizable alternating copolymer scaffold with controlled molecular weight and low dispersity.     

原子荧光光谱法直接测定二甲基二硒

硒位于第六主族,为准金属元素。在自然界中硒的存在形式按其结合形态分为无机硒和有机硒[1,2]。有机硒较无机硒具有更高的生物活性,因此准确测定各种样品中的有机硒具有重要意义。对于挥发性有机硒,一般采用洗脱富集将其与样品基体分离,采用固相吸附[3,4]或液氮冷阱捕集[5,6],热解析或溶剂萃取后用气相色谱测定[7,8]。这些方法可以提供许多有机硒的信息,但其不足之处是程序较为繁琐。原子荧光光谱分析法(AFS)具有准确度高、灵敏度高、线性范围宽、干扰少等优点,故本文利用AFS的特点及二甲基二硒(DMDSe)的挥发性,在不加任何试剂的条件下,…     

Synthesis and Crystal Structure of N-Phenylbis（ferrocenecarboxyl）imide

The ferrocenyl compound,N-phenylbis(ferrocenecarboxyl)imide (C28H23NO2Fe2,Mr=517.17),was synthesized and structurally characterized by means of X-ray single-crystal dif-fraction. It crystallizes in monoclinic,space group C2/c with a=21.374(14),b=10.430(7),c= 10.741(7) ,β=114.184(8)°,V=2184(2) 3,Z=4,Dc=1.573 g/cm3,F(000)=1064,μ(MoKα)= 1.355 mm–1,T=291(2) K,the final R=0.0548 and wR=0.1437 for 1524 observed reflections with I > 2σ(I). In this compound,the nitrogen atom links two ferrocenyl groups and one phenyl group forming a novel imido derivative.     

纸吸管中非挥发性迁移物的非靶向筛查及风险评估

根据欧盟法规推荐的两种食物模拟物对纸吸管样品进行模拟迁移试验,并基于超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF MS)对样品中的迁移物进行非靶向筛查,得到包括润滑剂、施胶剂、抗氧剂降解产物、消泡剂在内的31种有意添加物和非有意添加物。利用该课题组前期建立的风险矩阵,即风险=危害(毒性水平+Cramer分级+4×致突变性)×暴露(4×水溶性+4×渗透性),对纸吸管中31种迁移物进行风险分级。结果表明,未发现Ⅰ级高风险物质,Ⅱ级风险物质中得分较高的来自润滑剂(十六酸酰胺等)、施胶剂(海松酸等)和消泡剂(聚乙二醇等)中的成分,对Ⅱ级风险物质进行半定量分析,通过对比暴露量和TTC阈值,发现酰胺类润滑剂(尤其是芥酸酰胺)存在健康风险,应在纸吸管生产加工过程中引起关注。     

基于表面增强拉曼光谱技术的心肌生物标志物检测

心血管疾病(CVD)是全球最主要的死亡原因,急性心肌梗死(AMI)是心血管疾病致死的主要病因,安全快速地诊断AMI对于降低患者的死亡率至关重要。因常用的检测方法如心电图(ECG)缺乏足够的敏感性,寻找并针对AMI生物标志物开展高灵敏检测已成为早期检测AMI重要手段。心肌肌钙蛋白I(cTnI)、肌酸激酶同工酶(CK-MB)和肌红蛋白(Myo)是目前公认的检测AMI的重要心肌生物标志物。在过去的几十年里,许多生物传感器被开发出来用于检测心肌生物标志物,其中基于表面增强拉曼光谱(SERS)的心肌生物标志物检测技术迅速发展,并表现出独特的技术优势和广阔的应用前景。本文首先介绍了多种心肌生物标志物及其与AMI的关联,在此基础上概述主要的心肌生物标志物检测方法的原理、优势及局限性,重点介绍近年来新兴的SERS技术及其在心肌生物标志物传感方面的最新研究进展,并对该技术在AMI诊断方面的应用前景以及有待突破的瓶颈进行了讨论和展望。     

正交相MoO3的制备、表征及其电化学嵌锂性质

用化学沉淀-水热法在较低的温度下制备了片状正交相MoO3,由XRD、FT-IR、XPS和SEM表征了产物的相态、结构、成分和形貌。电化学测试表明,在0.1mA.cm-2的电流密度和1.2~3.5V电压范围,其初始放电容量为663mA.h.g-1,有望成为理想的锂离子插层材料。     

Synthesis and Bioactivity of Novel Fluorinated Heteroaromatic Ureas

In order to find new urea cytokinins, a series of novel fluorinated heteroaromatic ureas have been designed and synthesized. The crystal structure of 3g was further determined by single crystal X-ray diffraction to obtain the structural feature of this class of urea compounds. The preliminary bioassay showed that some title compounds have good cytokinin activity.