配合物[MnL(2,2''''-bipy)(H2O)]·2H2O的合成及其晶体结构

N-苯基亚氨基二乙酸(H2L),Mn(Ⅱ)和2,2'-联吡啶(2,2'-bipy)在50%甲醇中组装得标题配合物[MnL(2,2'-bipy)(H2O)]·2H2O(1),其结构经IR,元素分析和X-射线单晶衍射表征.1属单斜晶系,空间群P2(1)/n,晶胞参数:a=0.885 9(3)nm,b=1.826 9(6)nm,c=1.385 7(5)nm,β=106.200(6)°,V=2.153 6(13)nm3,Z=4,F(000)=980,Dc=1.457 Mg·m-3.在1的晶体结构中,Mn(Ⅱ)为六配位的畸变八面体构型,其中2,2'-bipy的2个氮原子和羧基的2个氧原子位于赤道平面,L的氮原子和一个配位水分子处于轴向位置.1分子之间存在的氢键与π-π芳香堆积作用将其连接成三维超分子结构.     

A CLUSTER COMPOUND WITH DI-ENDOXYGEN LIGANDS——THE CRYSTAL AND MOLECULAR STRUCTURE OF [Fe(MOS_4O)_2][N(C_2H_5)_4]3

[Fe(MoS_4O)_2] [N(C_2H_3)_4]_3 cluster compound with di-end-oxygen ligands has been prepared and characterized by the X-ray diffraction method. The compound crystallizes in a monoclinic space group P2_1/n with lattice parameters a=13.019(4), b=16.959(5), c=18.234(5), β=97.34(2)(°), Z=4. The final agreement factors are R=0.0740, Rw=0.0598. The terminal bond length, Mo-S_t and bridged one, MO-S_b for the compound are much longer than the counterpart without end-oxygen ligand. It possibly suggests that low valence of molybdenum and smaller electronegativity of sulphur than oxygen lead to the charge transfer as S→Mo→O.     

多目标逐步回归设计在反相色谱三元流动相组分最佳化中的应用

 〕本文首次将多目标优化与逐步回归设计相结合对反相色谱三元流动相的最佳组分进行了选择，并以去痛片组分与内标物的分离为例对方法和编制的程序进行考核。实验证明本方法简易、可靠。     

含氢甲基硅油含氢量的质谱法测定

含氢甲基硅油是高分子量的多聚物，用质谱方法对其Ｓｉ－Ｈ键上的氢含量的测定，仅用测定其分子量的办法不易实现。实验中发现，用其两个碎片离子ＳｉＯ９ＣＨ３）２和ＳｉＯ－ＨＣＨ＾＋３作为代表性离子，以它们的丰度比定出甲基含氢硅油的含氢量「Ｈ」。结果与用化学方法所测值十分接近。     

具有咖啡酰基和没食子酰基的β-二酮酸及喹噁啉酮类HIV整合酶抑制剂的设计合成及其对Cu2+的选择性识别

An efficient procedure for the synthesis of caffeoyl-and galloyl-containing β-diketoacid derivatives linked byarylamide was reported by,in the key step,dissolving the corresponding phenyl methyl ketone in THF/DME in thepresence of NaOMe as base and dimethyl oxalate as oxalylation reagent,and then separating the sodium ketoe-nolate ester.The resulting β-diketoacids underwent further condensation reaction with o-phenylenediamine to gen-erate quinoxalone derivatives in good yield,rather than 2-benzimidazol.The preliminary ion binding properties ofquinoxalone derivatives were also investigated.UV-Vis spectra showed that these compounds could selectively rec-ognize Cu~(2 )ion in ethanol and form a 1∶2 complex.     

Microcalorimetric Evaluation of the Effect of Kanamycin： An Analysis Based on the Median-Effect Principle

A study of the effect of drug, kanamycin, on the growth metabolism of recombinant Escherichia coli B 1 was carded out by microcalorimeter monitoring of the metabolic activity of treated cells. Power-time curves of growing recombinant Escherichia coli cell suspensions, treated with different kanamycin doses, were recorded. The extent of the effect was evaluated by changes in the slopes of the microcalorimetric curves and the kinetics of the drug action was interpreted from the time at which these changes reached their maximum values and maintained their maximum values. Experimental dose-effect relationships conform to the median-effect principle of the mass-action law： fa/（1-fa）=（D/D50）^m. A plot of y=lg[（fa）^1-1]^-1 versus x=lg D gives the slope m, D50 and R∞. The experimental results revealed that high concentration of kanamycin had an inhibitory effect on the growth of recombinant Escherichia coli B 1 in the lg phase, and had a promoting effect in the stationary period. Moreover, it was demonstrated that microcalorimetry was a reliable method for the detection of modulatory effects in biology.     

Li2O-TiO2-SiO2-P2O5和Li2O-TiO2-Al2O3-P2O5体系锂离子固体电解质的制备及性能研究

一些具有NASICON型网格结构的固体电解质具有高的电导率和好的稳定性,NASICON的意思是Na Super Ionic Conductor[1]。当NaZr2(PO4)3中P5 被Si4 部分取代时便可以得到具有NASICON结构的Na1 xZr2SixP3-xO12体系,其具有高的钠离子电导率。然而有相同结构的Li1 xZr2SixP3-xO12体系的离子电导率却很低,这是因为Li 半径太小,而NASICON三维网格结构的离子通道太大,两者不匹配而使电导率下降[2]。但当LiZr2(PO4)3中Zr4 被离子半径小些的Ti4 取代,所得LiTi2(PO4)3的通道就与Li 半径相匹配,适合于锂离子的迁移,从而使其电导率…     

Mo（W）－Co（Ni，Fe）簇合物的加氢脱硫催化活性

对线型、立方烷型和笼状３种不同构型的Ｍｏ（Ｗ）－Ｃｏ（Ｎｉ，Ｆｅ）－Ｓ（Ｏ）簇共１２种化合物进行了噻吩加氢脱硫和环己烯加氢的催化活性研究．讨论了簇合物的组成，金属原子的配比、价态与催化活性的关系．探讨了不同构型对活性的影响．     

金属氧化物电化学电容器

电化学电容器是一类利用电化学双电层或电极材料在电极表面及体相发生的氧化还原反应而存储能量的装置，具有高比能量、良好的可逆性和长循环寿命。金属氧化物电极目前主要有贵金属氧化物和过渡金属氧化物。本文简要介绍了金属氧化物电化学电容器的储能机理、特点及应用，总结了电极材料的制备及改性方法；并简要评述了电极材料的研究进展。