钴希夫碱配合物的合成及其氧合机制的研究——Ⅰ.配合物及其氧加合物的合成和表征

本文合成了一系列以水杨醛或萘酚醛同多胺缩合的四齿(N_2O_2)或五齿(N_3O_2)希夫碱为配体的钴希夫碱配合物及它们的氧加合物,用元素分析、红外光谱、磁化率以及ESR谱进行了表征,在续篇中将继续讨论配合物的吸氧行为和氧合机制。     

大黄酸-缬氨酸加合物的合成及初步抗肿瘤活性

以大黄酸为原料,经酯化、烷基化、水解及缩合等反应步骤合成了12个大黄酸-缬氨酸加合物.目标化合物经1H NMR,~(13)C NMR和HRMS进行了结构确证.以顺铂和阿霉素为阳性对照药,采用四甲基偶氮唑盐(MTT)法考察了目标化合物的体外抗肿瘤(Hela,MCF-7,HepG2,KB和HEK293T等5株细胞)活性.结果表明,化合物5l显示出较好的抗肿瘤活性,其IC50值在1.6~9.4μmol/L之间.作用机制研究结果表明,化合物5l能够与DNA发生较强的结合作用.     

加速器质谱法研究尼古丁与小鼠血液蛋白的加合作用

采用加速器质谱法（AMS）研究了小鼠血液中的血红蛋白（Hb),白蛋白（SA）和尼古丁和加合作用，在尼古丁剂量从相应于人吸烟的环境剂量水平0．1μg/kg体重到100μg/kg体重范围内，测量了尼古丁－血红蛋白加合物和尼古丁－白蛋白加合物的剂量效应曲线，两种蛋白的尼古丁加合物水平都随着尼古丁剂量的升高耐线性增加，在实验剂量范围内，两种蛋白质加合物的水平与小鼠肝DNA加合物水平也呈现良好的线性关系，这说两种蛋白质加合可以替代DNA加合物作为尼古丁的生物标记物，在本工作中，蛋白质加合物的测量灵敏度为0．03pmol/g蛋白（即3．2个加合物／10^12氨基酸残基），达到了文献报道的测量蛋白质生物标记物最高的灵敏度。     

Chlorine-radical Induced Oxidation of Glyoxal and Glyoxal-S（IV） Adducts in the Aqueous Phase

A laser flash photolysis study of the reactivity of Clwith glyoxal, glyoxal mono- and dibisulfite adducts, 1-hydroxy-2, 2-diol-ethanesulfonate and 1, 2-dihydroxy-1, 2-ethanedi sulfonate in the aqueous phase was carried out. The obtained rate constants can be used for atmospheric modeling.     

12-钨磷酸钙与丁二酰亚胺加合物的制备和性质研究

本文研究了12-钨磷酸钙与丁二酰亚胺和邻苯二甲酰亚胺的加合反应,制备了12-钨磷酸钙的丁二酰亚胺加合物Ca_(3/2)PW_(12)O_(40)·4(CH_2CO)_2NH·7H_2O,测定了加合物的红外光谱、拉曼光谱和热重差热分析曲线,用X射线粉末衍射方法研究了加合物的结晶学特征.结果表明.配体丁二酰亚胺以一个羰基氧与金属阳离子配位,加合物的形成对杂阴离子的Kcggin结构没有明显影响.但WO_6八面体发生一定的畸变.其中W-O_d键减弱,W-O_c键增强.加合物属单斜晶系,晶胞参数为:a=25.839(6).b=13.223(2),c=18.438(2)(?),β=97.06(2)°,V=6251.88(?)~3,可能的空间群为C_2h~5-P2_1/c或C_2h~2-P2_1/m或C_2~2-P2_1,品质因子F_(30)=54(0.012,45).     

Synthesis and Structure of a New Dinuclear Uranyl Complex

Dinuclear complexes have been widely investigated since 1970s when Robson proposed the conception of dinucleating ligand1,2. These compounds attracted much interests because of their applications as metal-enzemy model in bioinorganic chemistry or promising applications as functional materials. Most of these dinuclear complexes contain d transition metals as central ions. Few dinuclear U complexes have been reported. It is known, in most complexes of axial ion, five donors from ligands shou…     

Synthesis and Crystal Structure of 3-Nitrophthalic Acid·3-methyl-4-nitropyridine N-Oxide Adducts

The title compound, a 1:1 molecular adduct of 3-nitrophthalic acid and 3-methyl-4-nitropyridine N-oxide (PPOM), has been synthesized and characterized by X-ray single-crystal structure analysis. It crystallizes in triclinic, space group P-1 with a = 7.6076(15), b = 7.8180(16), c= 14.546(3) (A), α= 93.90(3), β = 97.21(3), γ= 114.43(3)°, C14H11N3O9, Mr = 365.26,Z=2,V=774.6(3) (A)3, Dc = 1.566 g/m3, u(MoKα) = 0.134 mm-1, F(000) = 376, R = 0.0538 and Wr = 0.1460 for 885 observed reflections (I＞2σ(I)). The protons of the carbonylic acids in the molecule are not transferred and the O-H…O and C-H…O hydrogen bonds form zigzag chains in the molecule.     

水杨醛缩乙醇胺双氧钒席夫碱配合物的合成、晶体结构及热分解研究(英)

A new complex bis[(N-salicylidene-N′-aminoethanol)dioxovandium(Ⅴ)], [V(Ⅴ)O₂(SALAE)]₂, was synthesized by the reaction of salicylaldehyde and aminoethanol with vanadyl sulfate. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the title complex (C₁₈H₂₀N₂O₈V₂, M_r = 494.24) belongs to monoclinic, space group P2₁/c with the following crystallographic parameters: a= 1.7966(6) nm, b= 0.7587(3) nm, c= 2.1539(7) nm, β = 92.551 (6) °, V= 2.9329 (17) nm³, Z= 6, D_c= 1.679 g·cm^-3, μ(MoKα) = 1.006 mm^-1, F(000) =1512, and final R₁ = 0.0563, wR₂= 0.1243 for observed reflections 2861(I> 2σ(I)). The complex is a bis(μ-oxo)-bridged V(Ⅴ) schiff base dimer formed by two dioxovandium units, V(Ⅴ) is six-coordinated and forms a distorted octahedral structure. The thermal decomposition for the complex was studied by TG-DTG curves and the apparent activation energy was obtained by the Kissinger formula. CCDC: 211147.     

12-钨磷酸希土盐DMF、DMSO加合物的合成、性质及其热分解动力学常数研究

合成了8种钨磷酸希土盐LnPW_(12)O_(40)·xH_2O(Ln=Y、La、Nd、Sm、Gd、Dy、Ho、Yb)的DMF、DMSO加合物,对加合物进行了组成分析,通过IR光谱、TG-DTA曲线对加合物进行了性质表征,并着重研究了加合物热分解过程的动力学,给出了热分解反应级数n和活化能E.     

L-精氨酸·氟硼酸加合物的X射线粉末衍射分析

采用X射线粉末衍射法对L-精氨酸·氟硼酸加合物进行了分析.数据收集范围在2θ角从7°到80°(共64个观测点).采用最小二乘法对该加合物粉末衍射的晶胞参数进行了计算,实验表明:该加合物为正交晶系,空间群P212121,晶胞参数a=0.50702(6)nm,b=1.37288(12)nm,c=1.64880(15)nm,V=1.147713nm3;Z=4;ρ=1.52g/cm3,粉末衍射分析的结果与单晶结构数据相吻合.