Synthesis and Crystal Structure of 2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)-methyl]-phenol-copper(Ⅱ)

2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)-methyl]-phenol-copper(Ⅱ) has been designed and synthesized.The structure was determined by UV,IR and single-crystal X-ray study.The title complex crystallizes in the triclinic system,space group P1 with a=6.6090(13),b=10.377(2),c=12.550(3),α=113.29(3),β=93.84(3),γ=98.31(3)°,V=774.9(3)3,Dc=2.215g/cm3,C26H30CuO4N4I4,Mr=1033.68,F(000)=487,μ=4.726 mm-1,Z=1,the final R=0.0563 and wR=0.1475 for 2101 observed reflections(I2σ(I)).The central copper(Ⅱ) is four-coordinated by two nitrogen atoms and two oxygen atoms from two 3,5-diiodosalicylaldehyde-2-morpholinoethylamine Schiff bases.The complex is linked into a column by π-π stacking interaction.The complex was assayed for antibacterial activities against three Gram positive bacterial strains(B.subtilis,S.aureus and S.faecalis) and three Gram negative bacterial strains(E.coli,P.aeruginosa and E.cloacae) by MTT method.Fortunately,the title complex shows potent antibacterial activity against these six bacterial strains.     

催化动力学光度法测定痕量锰--Mn(Ⅱ)-NTA-茜素紫3B-KIO4体系

在硼砂介质中 ,利用氨三乙酸活化 Mn( )催化 KIO4 氧化茜素紫 3B褪色的指示反应 ,建立了催化光度法测定痕量锰的新方法。方法的线性范围为 0 .0 30— 6 .0μg/ L ,检出限为 1.0× 10 -11g/ m L ,用于水样和茶叶中锰的测定 ,结果令人满意。     

3,5-二碘水杨醛缩苯胺合锌(Ⅱ)配合物的微波固相合成、结构及表征

采用微波固相法制备了3,5-二碘水杨醛缩苯胺合锌(Ⅱ)配合物,利用红外光谱、元素分析进行了表征,并利用单晶X射线衍射仪测定了该配合物的结构.结构解析表明,目标配合物为单斜晶系,C2/c空间群,晶胞参数a=2.2287(2) nm,b=1.1699(4) nm,c =2.6065(3) nm,β=94.579(3)°,V=6.5667(12) nm3,Z=8,F(000)=3872,最终偏差因子(对I＞2σ(I)的衍射点),R1=0.0547,wR2 =0.1316,S=1.024.目标配合物结构中,中心Zn(Ⅱ)离子分别与来自两个3,5-二碘水杨醛缩苯胺的两个N原子和两个O原子配位,形成一个稍微扭曲的四面体.     

Synthesis and Crystal Structure of the Copper（Ⅱ） Complex [Cu2Cl2（HEMDP）2]·THF

One dinuclear complex [Cu2Cl2(HEMDP) 2]·THF 1(H2EMDP = 2-[(2-hydroxyethylimino)-methyl]-4,6-diiodo-phenol,THF = tetrahydrofuran) has been designed and synthesized by H2EMDP with CuCl2·2H2O in THF solvent. Complex 1 was characterized by UV,IR,ESI-MS,and elemental analyses. 1 was characterized by X-ray crystallography. The crystal belongs to the monoclinic system,space group C2/c with a = 27.886(3) ,b = 8.6890(12) ,c = 26.698(2) ,β = 105.521(2) o,V = 6233.1(12) 3,Z = 8,Mr = 1102.01,μ = 5.533 mm-1,Dc = 2.349 Mg/m3,F(000) = 4112,the final R = 0.0486 and wR = 0.1175(I > 2σ(I)) . In addition,further investigation revealed that the central copper(Ⅱ) atom in the complex is five-coordinated by one nitrogen atom and two oxygen atoms from H2EMDP and two chlorine atoms from chlorid. The 3,5-diiodosalicylaldehyde Schiff base acts as a tridentate ligand. H2EMDP and 1 were assayed for antibacterial(B. subtilis,S. aureus,S. faecalis,P. aeruginosa,E. coli and E. cloacae) activities by MTT(3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl trtrazolium bromide) method. 1 showed the most favorable antimicrobial activity with MICs of 3.125,6.25,6.25,12.5,3.125 and 6.25 μg/mL against B. subtilis,S. aureus,S. faecalis,P. aeruginosa,E. coli and E.cloacae,respectively.     

5-氯水杨醛缩乙醇胺合铜(Ⅱ)的微波直接合成、晶体结构及抑菌活性

以5-氯水杨醛、乙醇胺和氯化铜为原料,在微波作用下合成了5-氯水杨醛缩乙醇胺合铜(Ⅱ)配合物。 利用红外光谱、元素分析和单晶X射线衍射方法对目标化合物进行了表征,标题配合物为单斜晶系,P21/n空间群。晶胞参数：a=0.49793(6) nm,b=1.7037(2) nm,c=1.07120(12) nm,β=94.579(3)°,F(000)=470,Z=2,V=0.905(8) nm3,Dc=1.689 mg/m3,R[I＞2σ(I)],R1=0.0624,ωR2=0.1555。 配合物分子中,2种Schiff碱配体中的2个O原子和2个N原子参与配位,Cu(Ⅱ)处于四边形配位中心。 用MTT法测得标题配合物对6种革兰氏细菌（B.subtilis、S.aureus、S.faecalis、P.aeruginosa、E.coli和E.cloacae）的最小抑制浓度分别为12.25、25、12.5、12.5、6.25和6.25 mg/L。     

Syntheses and Crystal Structures of 3,5-Diiodo-salicylalidehyde and 3,5-Diiodo-salicylalidene-4-nitroaniline

The title compounds, C7H4I2O2 1 and C13H7I2N2O3 2, have been synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 9.802（2）, b = 13.867（3）, c = 7.364（2） A, β = 109.74（3）°, V= 942.1（3） A^3, Dc= 2.636 g/cm^3, C7H4I2O2, Mr= 373.90, F（000） = 672, μ = 6.627 mm^-1, Z = 4, R = 0.0459 and wR = 0.1018 for 1805 observed reflections （I 〉 2 σ（I））. Compound 2 belongs to the monoclinic system, space group P21/n with a = 9.015（2）, b = 12.024（2）, c = 14.072（3） A, β = 103.91（3）°, V = 1480.6（5） A^3, Dc= 2.216 g/cm^3, C13H7I2N2O3, Mr= 494.01, F（000） = 920, p = 4.255 mm^-1, Z = 4, R = 0.0777 and wR = 0.1757 for 2896 observed reflections （I 〉 2σ（I））. Compounds 1 and 2 were assayed for antibacterial activities against three Gram positive bacterial strains （B. subtilis, S. aureus and S. faecalis） and three Gram negative bacterial strains （E. coli, P. aeruginosa and E. cloacae） by MTr method. Fortunately, compound 2 is found to show potent antibacterial activity against these six bacterial strains.     

硝酸铅沉淀/ICP-MS法测定高纯铅中18种杂质

通过硝酸铅沉淀分离基体铅、有效富集高纯铅中镁、铝、钙、铁、镍、钴、锰、铜、锌、砷、硒、镉、铟、锡、锑、碲、铊、铋等18种杂质,通过电感耦合等离子体质谱测定高纯铅中18种杂质,测定下限在0.04～0.32μg/mL,加标回收率为80%～108%,测定精密度(RSD)为2.5%～14%。