5-溴水杨醛缩三乙烯四胺Schiff碱配合物的合成与表征

合成了5-溴水杨醛缩三乙烯四胺Schiff碱（H2Y）,并制备了Cu（Ⅱ）,Co（Ⅱ）和Mn（Ⅱ）的配合物[Cu2Y（H2O）2]（NO3）2（1）,[Co2Y（H2O）。（NO3）2]（2）,[Cu2ClY]Cl·H2O（3）和[MnY]（4）,利用元素分析、摩尔电导、IR和UV光谱对配合物的结构进行了表征,研究了它们的热稳定性．     

5-溴水杨醛亚胺合铜(Ⅱ)类配合物的合成与抑菌活性

希夫碱类药物由于其良好的抗肿瘤、抗细菌、抗病毒、抗真菌等多种生物活性而日益受到人们的重视[1,2].近年来我们合成了一系列水杨醛亚胺希夫碱药物[3,4],发现取代水杨醛亚胺希夫碱药物的杀菌抑霉活性更高,抗菌谱更广.故又设计合成了5-溴水杨醛缩苯胺、邻甲(间氯)苯胺新希夫碱及其Cu(Ⅱ)配合物,并由元素分析和红外光谱所表征.合成路线如下:     

牛磺酸缩3,5-二溴水杨醛席夫碱镁配合物[Mg(Br_2TSSB)(Phen)(H_2O)]·H_2O的合成及晶体结构

0引言含硫席夫碱及其金属配合物具有抑菌、抗癌和抗病毒的生物活性[1￣3],有些含O、N席夫碱金属配合物具有仿酶催化活性[4,5]。而氨基酸席夫碱配合物具有良好的生物生理活性,近年来得到人们的普遍重视[6,7]。同α-氨基酸席夫碱相比,β-氨基酸席夫碱由于氨基位置的变化而引起不同的配位特征,但研究此类席夫碱的报道目前还不多[8￣10]。2-氨基乙磺酸(牛磺酸)作为生物体内一种特殊的氨基酸,目前对它的研究主要集中在生理和病理方面,它的席夫碱及其配合物的研究或牛磺酸金属配合物的研究刚起步[2,10￣17]。研究表明,-SO32-可以与碱金属、碱土…     

2-氨甲基吡啶配体锌配合物的合成、晶体结构及催化性能

以2-氨甲基吡啶为配体与醋酸锌反应合成了一种新型锌金属配合物[Zn(AMPy)2(OAc)]2·[Zn(OAc)4](AMPy=2-氨甲基吡啶),通过核磁共振谱、红外光谱、元素分析和X射线单晶衍射对其结构进行了表征.晶体结构显示,该配合物属于三斜晶系,空间群为P1,晶胞参数为a=1.07360(19)nm,b=1.2491(2)nm,c=1.8976(3)nm,α=83.809(2)°,β=89.595(2)°,γ=65.708(2)°,V=2.3039(7)nm3,Z=2;配合物分子由3个不同的配位Zn离子通过分子内氢键连成一个完整的分子,分子间氢键再将其连成一个二维网状结构.研究了该金属配合物在Henry催化反应方面的性能,并优化出最佳催化条件.     

Zn的3，5-二溴水杨醛水杨酰腙配合物的合成、表征及晶体结构

The title complex [Zn(C₁₄H₈N₂O₃Br₂)(C₅H₅N)₃] was synthesized in DMF and pyridine. It has been characterized by IR, element analysis and X-ray diffraction analysis. The crystal structure of the title complex belongs to monoclinic space group P2₁/c with cell parameters: a=0.999 78(6) nm, b=1.951 11(13) nm, c=1.496 02(10) nm, β=97.126 0(10)°, and V=2.895 7(3) nm³, Dc=1.639 g·cm^-3, Z=4, F(000)=1 424, μ=3.647 mm^-1, the final R=0.061 0 and wR=0.140 2 for 3 528 observed reflections with I>2σ(I). The X-ray crystal structure analysis revealed that the center zinc(Ⅱ) is bonded to two oxygen atoms and one nitrogen atom from a tridentate ligand and three nitrogen atoms from three solvent pyridine molecules to form a six-coordinate octahedron. CCDC: 261047.     

牛磺酸缩3，5-二溴水杨醛席夫碱镁配合物[Mg(Br2TSSB)(Phen)(H2O)]·H2O的合成及晶体结构

Reactions of bitter salt with taurine-3,5-dibromo-salicylaldehyde schiff base gave one new Complex [Mg(Br₂TSSB)(Phen)(H₂O)]·H₂O (Br₂TSSB=Taurine 3,5-dibromo-Salicylaldehyde Schiff Base, phen=o-phenanthroline), which was characterized by elemental analysis, IR and X-ray diffraction. The chemical formula weight of the complex is 625.58. It′s crystal belongs to monoclinic system with space group P2₁/c. The cell parameters are: a=1.814 2(3) nm, b=0.814 75(14) nm, c=1.641 7(3) nm, β=90.571(4)°, and Z=4, V=2.426 4(7) nm³, Dc=1.712 g·cm^-3, F(000)=1 248, μ=3.496 mm^-1. The complexes form a 3D net structure in which they are connected with hydrogen bonds and π-π stacking. The Mg(II) formed a distorted coordination tetragonal pyramid. CCDC: 286194.     

5-溴水杨醛缩乙醇胺Schiff碱Cu(II)配合物的合成和晶体结构

The title complex Cu(L)₂ [HL=N-(5-bromosalicylidene)-2-aminoethanol] was synthesized by the reaction of Cu(CH₃COO)₂·H₂O with N-(5-bromosalicylidene)-2-aminoethanol in the ethanol. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the title complex [Cu(C₉H₉BrNO₂)₂] belongs to monoclinic, space group P2₁/n with a=1.319 1(5) nm, b=0.444 58(16) nm, c=1.656 7(6) nm, β=91.226(5)°, V=0.971 46(6) nm³, Z=2, D_c=1.879 Mg·m^-3, μ=5.264 mm^-1, F(000)=542, and final R₁=0.045 6, wR₂=0.097 0. The complex comprises a four-coordinated copper(II) center, with an N₂O₂ planar coordination environment. The molecules are connected by hydrogen bonds to form two-dimensional layered structure. CCDC: 274180.     

非天然氨基酸水杨醛席夫碱铜配合物的合成与表征

合成了N-亚水杨基β-丙氨酸铜(1)和N-亚水杨基牛磺酸铜(2)两种新配合物,用元素分析、摩尔电导、红外光谱、热重差分析、X-射线粉末衍射对所合成的配合物进行了表征,并对X-射线粉末衍射数据进行了指标化.两种配合物的组成分别为Cu(sal-β-ala)*H2O(1),Cu(sal-tau)*2H2O(2),X-射线粉末衍射数据指标化结果表明,两种配合物均属于正交晶系,晶胞参数分别是1a=1.4981nm,b=1.8246nm,c=2.1985nm;2a=0.9454,b=1.7092nm,c=2.2254.     

乙二胺双缩5-甲基-3-羧基水杨醛镍(Ⅱ)配合物的合成与晶体结构

合成了乙二胺双缩5-甲基-3-羧基水杨醛Schiff碱(H2EMS)镍(Ⅱ)配合物Ni(EMS),利用红外光谱、紫外-可见光谱和单晶X射线衍射分析了配合物的组成和结构.结果表明,合成的配合物Ni(EMS)属于单斜晶系,空间群为C2/c,其晶胞参数为:a=1.933 85(17)nm,b=0.974 24(9)nm,c=0.951 86(9)nm,β=91.084(2)°,V=1.793 02(28)nm3,Z=4,Mr=441.07,Dc=1.633 83g/cm3,F(000)=912,μ=1.126mm-1,R1=0.035 2,wR2=0.081 5,S=1.027.配合物中的镍离子采取四配位方式,处于平面正方形配位环境中.     

氨基酸水杨醛席夫碱与铜(Ⅱ)配合物的合成及其抗菌活性和稳定性、结构间的关系

n-Salicylideneamino acids and their Cu(Ⅱ) complexes are synthesized. The structures of the compounds are characterized by elementary analysis, molar conductance, magnetic susceptibility, electronic and infrared spectra. The stability constants and the antibacterial activities have been determined. The relativity between antibacterial activities and structures of ligands and stability of complexes has been preliminarily studied.     

Synthesis, structural characterization and electrochemical studies of new macrocyclic Schiff base containing pyridine head and its metal complexes

A new macrocyclic ligand, 1,3,5-triaza-2,4:7,8:13,14-tribenzo-9,12-dioksa-cyclopentadeca-1,5-diene was synthesized by reaction of 2,6-diaminopyridine and 1,2-bis(2-carboxyaldehyde phenoxy)ethane. Then, its Cu(II), Ni(II), Pb(II), Co(III) and La(III) complexes were synthesized by the template effect by the reaction of 2,6-diaminopyridine and 1,2-bis(2-carboxyaldehyde phenoxy)ethane and Cu(NO₃)₂ · 3H₂O, Ni(NO₃)₂ · 6H₂O, Pb(NO₃)₂, Co(NO₃)₂ · 6H₂O, La(NO₃)₃ · 6H₂O, respectively. The ligand and its metal complexes have been characterized by elemental analysis, IR, ¹H and ¹³C NMR, UV-Vis spectra, magnetic susceptibility, thermal gravimetric analysis, conductivity measurements, mass spectra, and cyclic voltammetry. All complexes are diamagnetic and Cu(II) complex is binuclear. The Co(II) was oxidized to Co(III). The comparative electrochemical studies show that the nickel complex exhibited a quasi-reversible one-electron reduction process, while copper and cobalt complexes gave irreversible reduction processes in DMSO solution.     

Synthesis,structural characterization,antimicrobial, antioxidant and DNA binding studies of some novel homo‐binuclear Schiff base metal (II) complexes

A novel bi‐nucleating Schiff base ligand, 6,6′‐(((1E,1′E)‐thiophene‐2,5‐diylbis (methaneylylidene))bis (azaneylylidene))bis (3,4‐dimethylaniline), and five binuclear M (II) complexes were synthesized. The bi‐nucleating Schiff base ligand and its metal complexes were characterized using various physicochemical techniques, e.g. elemental analyses, spectroscopic methods, conductivity and magnetic moment measurements. The low molar conductance of the complexes in dimethylsulfoxide shows their non‐electrolytic nature. The antibacterial activities were screened against pathogenic bacteria (Staphylococcus aureus, Escherichia coli, Pseudomonas putida and Bacillus subtilis). The antifungal activity was screened against Aspergillus niger, Aspergillus flavus and Rhizoctonia bataicola. The antimicrobial activity data showed that the metal complexes are more potent than the parent Schiff base ligand against microorganisms. The antioxidant activities of the synthesized compounds were investigated through scavenging activity against 2,2‐diphenyl‐2‐picrylhydrazyl, superoxide anion, hydroxyl and 2,2′‐ azinobis (3‐ethylbenzothiazoline‐6‐sulfonic acid) radicals. The complexes have superior radical scavenging activity than the free ligand and the scavenging effects of the Cu (II) complex are stronger than those of the other complexes. DNA binding studies were performed using electronic spectroscopy, fluorometric competition studies and viscosity measurements. The data indicated that there is a marked enhancement in biocidal activity of the ligand under similar experimental conditions because of coordination with metal ions.     

Synthesis, spectroscopy, electrochemistry and thermal study of vanadyl tridentate Schiff base complexes

The VO(IV) complexes of tridentate ONO Schiff ligands were synthesised and characterized by IR, UV–vis and elemental analysis. The electrochemical properties of the vanadyl complexes were investigated by cyclic voltammetry. A good correlation was observed between the oxidation potentials and the electron withdrawing character of the substituents on the Schiff base ligands, showing the following trend: MeO < H < Br < NO₂ and H < Cl. The thermogravimetry (TG) and differential thermoanalysis (DTA) of the VO(IV) complexes were carried out in the range of 20–700 °C. The VOL¹(OH₂) decomposed in two steps whereas the remaining six complexes decomposed in three steps. The thermal decomposition of these complexes is closely related to the nature of the Schiff base ligands and proceeds via first order kinetics.     

Transition metal complexes of a Schiff base: synthesis,characterization, and antibacterial studies

Synthesis of a new Schiff base derived from 2-hydroxy-5-methylacetophenone and glycine and its coordination with compounds Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and UO₂(VI) are described. The ligand and complexes have been characterized on the basis of analytical, electrical conductance, infrared, ESR and electronic spectra, magnetic susceptibility measurements, and thermogravimetric analysis. The ligand is a dibasic tridentate (ONO) donor in all the complexes except Zn(II), where it is a monobasic bidentate (OO) donor. The solid state DC electrical conductivity of ligand and its complexes have been measured over 313–398 K, and the complexes were semiconducting. Antibacterial activities of ligand and its metal complexes have been determined by screening the compounds against various Gram (+) and Gram (?) bacterial strains.     

Synthesis,characterization and antimicrobial activity of a bidentate NS Schiff base of S-benzyl dithiocarbazate and its divalent complexes

The reaction of S-benzyl dithiocarbazate (SBDTC) with 2,4,5-trimethoxybenzaldehyde afforded a bidentate NS Schiff base 1 (benzyl-3-N-(2,4,5-trimethoxyphenylmethylenehydrazine carbodithioate), which on further reaction with M(II) (where M(II) = nickel(II), zinc(II), palladium(II) and copper(II)) in ethanol under reflux yielded bis-chelated inner complexes [ML₂] 2–5 with deprotonated L. The ligand and its complexes were characterized by physicochemical techniques, viz., molar conductance, magnetic susceptibility measurement, IR, NMR, UV–Vis and mass spectroscopic techniques. The crystal structures of 1 and 5 were also determined by single-crystal X-ray crystallography. The crystal structure analysis showed that the ligand exists in its thione tautomeric form. In the complexes, each of the two deprotonated ligands chelated the metal ions through the β-nitrogen and the thione sulfur forming five-membered rings. The copper(II) complex (5) exhibited a square-planar geometry, where the two N₂S₂ chromophores are arranged trans. All the compounds showed strong antibacterial activity against S.-β-hemolyticus, Klebsiella pneumoni, and Escherichia coli. The compounds also showed strong antifungal activity against Aspergillus fumigatus, Aspergillus niger, Aspergillus flavus, and Candida albicans with the exception of the palladium(II) complex (4) which showed no activity, while all the compounds showed no activity against Fusarium vasinfectum.     

Synthesis and characterization studies of 3-formyl chromone Schiff base complexes and their application as antitumor,antioxidant and antimicrobial

A novel Schiff base namely (E)-3-((2,6-dihydroxypyrimidin-4-ylimino)methyl)-4H-chromen-4-one and its Co (II), N (II)i, Cu (II) and Cd (II) complexes have been synthesized and proved by elemental analysis, molar conductance, thermal analysis (TGA), Inductive Coupled plasma (ICP), magnetic moment measurements, X-ray powder diffraction, IR, EI-mass,¹H NMR, ¹³C NMR,UV–Vis. and ESR spectral studies. On the basis of these data, it is evident that the Schiff base acts as bidentate via oxygen atom of carbonyl group and azomethine nitrogen atom for Co (II) complex; monobasic bidentate ligand for Ni (II), Cu (II) and Cd (II) complexes via oxygen atom of hydroxyl group and nitrogen atom of pyrimidine ring. The results showed all complexes have octahedral geometry. The average particle size of the ligand and its complexes were found to be 1.010–0.343 nm. The pharmacological action (antioxidant, antimicrobial and anticancer) of the prepared compounds is studied. The antitumor activity of the ligand and its metal complexes is evaluated against human liver carcinoma (HEPG2) cell. The data displayed the Co (II) complexes strong cytotoxicity where IC₅₀ values of Co (II) complex and 5-fluorouracil (stander drug) are 9.33 and 7.86 μg/ml respectively. The Co (II) and Cd (II) complexes have antibacterial activity more than ampicillin (stander drug). The interaction of the synthesized compounds with calf-thymus DNA (CT-DNA) has been performed via absorption spectra and viscosity technique. The DNA- binding constants have been determined.     

Synthesis,characterization, molecular docking studies and in vitro screening of new metal complexes with Schiff base as antimicrobial and antiproliferative agents

A series of Cu(II), Co(II), Pd(II), Pt(II), Zn(II), Cd(II) and Fe(III) complexes were designed and synthesized using Schiff base 1‐phenyl‐2,3‐dimethyl‐4‐(N‐3‐formyl‐6‐methylchromone)‐3‐pyrazolin‐5‐one (HL). The new metal complexes were investigated using various physicochemical techniques including elemental and thermal analyses, molar electric conductivity and magnetic susceptibility measurements, as well as spectroscopic methods. Also, the crystal structures of ligand HL and the Pd(II) complex were determined using single‐crystal X‐ray diffraction analysis. For all compounds, the antimicrobial activity was studied against a series of standard strains: Staphylococcus aureus, Bacillus cereus, Enterococcus faecalis, Escherichia coli, Acinetobacter baumannii, Candida albicans, Candida krusei and Cryptococcus neoformans. The in vitro antiproliferative activity of the ligand and complexes was evaluated against ten cancer cell lines: MSC, A375, B16 4A5, HT‐29, MCF‐7, HEp‐2, BxPC‐3, RD, MDCK and L20B. At 10 μM concentration a significant cytotoxic effect of the Co(II), Pd(II) and Cd(II) complexes was observed against B16 4A5 murine melanoma cells. The Zn(II) complex is active against HEp‐2, RD and MDCK cancer cell lines, where IC₅₀ values vary between 1.0 and 77.6 and for BxPC‐3 the activity index versus doxorubicin is 3.7 times higher.     

Synthesis and characterization of Schiff base metal complexes: their antimicrobial,genotoxicity and electrochemical properties

We have synthesized the three Schiff-base ligands H₂L¹–H₂L³ and their Co^II, Fe^III and Ru^III metal complexes. All compounds have been characterized by analytical and spectroscopic methods. Oxidation of cyclohexane has been done by the metal complexes in CH₃CN using H₂O₂ and/or t-butylhydroperoxide (TBHP) as a co-catalyst. The keto-enol tautomeric forms of the ligands have been studied in polar and non-polar organic solvents. Electrochemical properties of the complexes have been studied at different scan rates. Thermal studies were carried out for the compounds. The ligands H₂L¹–H₂L³ were mutagenic on Salmonella Typhimurium TA 98 strain in the presence and/or absence of S9 mix. While the ligands H₂L¹ and H₂L² showed mutagenic activity on the strain TA 100 with and without S9 mix, the ligand H₂L³ was not mutagenic for TA 100. Antimicrobial activity studies of the compounds have also been carried out.     

Synthesis,characterization and cytotoxic activity of diorganotin complexes with Schiff base derived from salicylaldehyde and l-tyrosine

Seven diorganotin complexes with the Schiff bases derived from salicylaldehyde and l-tyrosine, R₂Sn[2-O-5-XC₆H₃CH?=?NCH(CH₂C₆ H₄OH-4)COO] (X?=?H (1), Br (2); R?=?Me (a), Et (b), Bu (c), Cy (cyclohexyl) (d)), were synthesized and characterized by elemental analysis, IR, ¹H and ¹³C NMR spectra, and the single-crystal X-ray diffraction. In methanol, the racemization of chiral center of l-tyrosinate fragment occurred and the racemic products were obtained. X-ray analyses of 1c, 1d, and 2a–2c showed that the tin atoms of the complexes exhibit distorted trigonal-bipyramidal geometries. In 1c, 1d, and 2c, the intermolecular O–H???O hydrogen bonds connected the molecules into 1-D supramolecular chain or a R₂²(20) macrocyclic dimer, and 2a and 2b formed the 2-D supramolecular network by the intermolecular Sn???O and O–H???O interactions. Bioassay results indicated that 1a, 1c, and 1d had moderate antibacterial activity against Escherichia coli and 1c, 1d, and 2c belonged to the efficient cytostatic agents against two human tumor cell lines (A549 and HeLa) and the activity tends to follow the order Cy > Bu?>?Et?>?Me for the R group attached to tin.