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Thermal, Spectral, Fluorescence, and Antimicrobial Studies of Cobalt, Nickel, Copper, and Zinc Complexes Derived from 4-[(5-Bromo-thiophen-2-ylmethylene)-amino]-3-mercapto-6-methyl-5-oxo-[1,2,4]triazine 由4-[(5-溴-噻吩-2-基亚甲基)-氨基]-3-巯基-6-甲基-5-氧-[1,2,4]三嗪衍生的钴、镍、铜和锌配合物的热、光谱、荧光和抗菌研究
Pub Date : 2012-08-02 DOI: 10.1155/2012/873232
Kiran Singh, Y. Kumar, Parvesh Puri, C. Sharma, K. R. Aneja
A new series of cobalt, nickel, copper, and zinc complexes of bidentate Schiff base derived from the condensation of 5-bromothiophene-2-carboxaldehyde with 4-amino-3-mercapto-6-methyl-5-oxo-[1,2,4]triazine were synthesized. Physical (magnetic measurements, molar conductance, TG), spectral (UV-Vis, IR, 1HNMR, fluorescence, ESR), and analytical data have established the structures of synthesized Schiff base and its metal complexes. The presence of coordinated water in metal complexes was confirmed by IR and TG studies. The Schiff base exhibits a strong fluorescence emission, contrast to this partial fluorescence quenching phenomena is observed in its metal complexes. A square planar geometry for Cu(II) and octahedral geometry for Co(II), Ni(II) and Zn(II) complexes have been proposed. The Schiff base and its metal complexes have been screened for antibacterial (Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Pseudomonas aeruginosa) and antifungal activities (Aspergillus niger, A. flavus).
由5-溴噻吩-2-甲醛与4-氨基-3-巯基-6-甲基-5-氧-[1,2,4]三嗪缩合反应合成了一系列新的双齿希夫碱钴、镍、铜和锌配合物。物理(磁测量、摩尔电导、热重)、光谱(紫外可见、红外、核磁共振、荧光、ESR)和分析数据建立了合成的希夫碱及其金属配合物的结构。红外光谱和热重分析证实了金属配合物中存在配位水。希夫碱表现出强烈的荧光发射,相反,在其金属配合物中观察到这种部分荧光猝灭现象。提出了Cu(II)配合物的方形平面几何和Co(II)、Ni(II)和Zn(II)配合物的八面体几何。希夫碱及其金属配合物具有抗菌(金黄色葡萄球菌、枯草芽孢杆菌、大肠杆菌、铜绿假单胞菌)和抗真菌(黑曲霉、黄曲霉)活性。
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引用次数: 22
Synthesis and Characterization of Functionalized Magnetic Nanoparticles for the Detection of Pesticide 用于农药检测的功能化磁性纳米颗粒的合成与表征
Pub Date : 2012-06-05 DOI: 10.1155/2012/439751
S. Taira, D. Kaneko, K. Onuma, Akio Miyazato, Tomoyuki Hiroki, Y. Kawamura-Konishi, Y. Ichiyanagi
We synthesized magnetic nanoparticles (MNPs) by mixing aqueous solutions of 3d transition metal chlorides () and a sodium metasilicate nonahydrate () in order to produce monodispersed MNPs in a single step. The particle size can be controlled by adjusting the annealing temperature. We characterized the MNPs by X-ray diffraction (XRD), superconducting quantum interference device (SQUID), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR), and zeta-potential measurement. Paramagnetic and superparamagnetic behaviors were found for the obtained samples depending on the particle size ( nm). The synthesized MNPs could be modified with the amino-, phenyl-, and carboxy- groups on MNPs' surface by silanization procedure, respectively. The purpose of functionalizing the surface of the nanoscale magnetic particles was to realize subsequent capture and detection with desired other molecules by nanoparticle assisted laser ionization/desorption mass spectrometry.
我们通过混合三维过渡金属氯化物()和非水合偏硅酸钠()的水溶液来合成磁性纳米颗粒(MNPs),以便在一个步骤中产生单分散的MNPs。可通过调节退火温度来控制颗粒大小。我们通过x射线衍射(XRD)、超导量子干涉装置(SQUID)、透射电子显微镜(TEM)、傅里叶变换红外(FT-IR)和ζ电位测量对MNPs进行了表征。所得样品的顺磁性和超顺磁性行为取决于粒径(nm)。合成的MNPs可以分别用硅烷化方法对MNPs表面的氨基、苯基和羧基进行修饰。将纳米级磁性粒子表面功能化的目的是利用纳米粒子辅助激光电离/解吸质谱法实现对所需其他分子的后续捕获和检测。
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引用次数: 13
Crystal Structure and Thermal Behavior of Two New Supramolecular Complexes Templated with 1,2,4,5-Benzenetetracarboxylic Acid 以1,2,4,5-苯四羧酸为模板的两种新型超分子配合物的晶体结构和热行为
Pub Date : 2012-05-21 DOI: 10.1155/2012/291682
Lingling Gao, Y. Liu, Xulu Lv, Jianfeng Liu, Tuoping Hu
Templated coordination polymers [Ni(H2O)4(bipy)](BTA)0.5·H2O (1) and [Co(H2O)4(bipy)](BTA)0.5·H2O (2) (bipy = 4,4′-Bipyridine, H4BTA = 1,2,4,5-Benzenetetracarboxylic Acid) were synthesized and characterized by single-crystal X-ray diffraction, powder diffraction, elemental analysis, IR, and thermogravimetric analysis. Both of complexes 1 and 2 are monoclinic crystal system, C2/c space group, and isostructural. The unit of the structure, the metal ion is coordinated by four water molecules and two bipy molecules, is a slightly distorted octahedral configuration, and the carboxyl group from BTA4- ion doesn't coordinate with the metal ion, the H-bonding interactions further connect the mononuclear molecules to generate a 3D supramolecular complex.
合成了模板化配位聚合物[Ni(H2O)4(bipy)](BTA)0.5·H2O(1)和[Co(H2O)4(bipy)](BTA)0.5·H2O (2) (bipy = 4,4′-联吡啶,H4BTA = 1,2,4,5-苯四羧酸),并通过单晶x射线衍射、粉末衍射、元素分析、红外光谱和热重分析对其进行了表征。配合物1和2均为单斜晶系、C2/c空间群、同构。该结构单元,金属离子由4个水分子和2个双分子配位,呈轻微扭曲的八面体构型,BTA4-离子的羧基不与金属离子配位,氢键相互作用进一步连接单核分子,形成三维超分子复合物。
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引用次数: 1
Polydentate Schiff Base Ligands and Their La(III) Complexes: Synthesis, Characterization, Antibacterial, Thermal, and Electrochemical Properties 多齿席夫碱配体及其La(III)配合物:合成、表征、抗菌、热学和电化学性能
Pub Date : 2012-05-16 DOI: 10.1155/2012/791219
A. Şabik, M. Karabörk, G. Ceyhan, M. Tümer, M. Dığrak
We synthesized the Schiff base ligands H2L1–H2L4 and their La(III) complexes and characterized them by the analytical and spectroscopic methods. We investigated their electrochemical and antimicrobial activity properties. The electrochemical properties of the ligands H2L1–H2L4 and their La(III) complexes were studied at the different scan rates (100 and 200 mV), different pH ranges (pH=2−12), and in the different solvents. The electrooxidation of the Schiff base ligands involves a reversible transfer of two electrons and two protons in solutions of pH up to 5.5, in agreement with the one-step two-electron mechanism. In solutions of pH higher than 5.5, the process of electrooxidation reaction of the Schiff base ligands and their La(III) complexes follows an ECi mechanism. The antimicrobial activities of the ligands and their complexes were studied. The thermal properties of the metal complexes were studied under nitrogen atmosphere in the range of temperature 20–1000°C.
合成了希夫碱配体H2L1-H2L4及其La(III)配合物,并用分析和光谱方法对其进行了表征。研究了它们的电化学和抗菌性能。研究了配体H2L1-H2L4及其La(III)配合物在不同扫描速率(100和200 mV)、不同pH范围(pH=2 ~ 12)和不同溶剂下的电化学性能。席夫碱配体的电氧化涉及两个电子和两个质子在pH高达5.5的溶液中的可逆转移,符合一步双电子机制。在pH大于5.5的溶液中,席夫碱配体及其La(III)配合物的电氧化反应遵循ECi机制。研究了这些配体及其配合物的抗菌活性。在20 ~ 1000℃的氮气气氛下研究了金属配合物的热性能。
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引用次数: 15
Mixed-Ligand Nickel(II) Complexes Containing Sulfathiazole and Cephalosporin Antibiotics: Synthesis, Characterization, and Antibacterial Activity 含磺胺噻唑和头孢菌素类抗生素的混合配体镍(II)配合物:合成、表征和抗菌活性
Pub Date : 2012-05-09 DOI: 10.1155/2012/106187
J. Anacona, Marie Lopez
Nickel(II) reacts with cephalosporins plus sulfathiazole (Hstz) to form the following mixed-ligand complexes of general formulae [Ni(L)(stz) (, ; , ; L = monoanion of cefazolin , cephalothin , cefotaxime , ceftriaxone ) and [Ni()(stz)]Cl (cefepime ), which were characterized by physicochemical and spectroscopic methods. Their spectra indicated that cephalosporins are acting as multidentate chelating agents, via the lactam carbonyl and carboxylate and N-azomoieties. The complexes are insoluble in water and common organic solvents but soluble in DMSO, where the [Ni()(stz)]Cl complex is 1 : 1 electrolyte. They probably have polymeric structures. They have been screened for antibacterial activity, and the results are compared with the activity of commercial cephalosporins.
镍(II)与头孢菌素和磺胺噻唑(Hstz)反应形成通式[Ni(L)(stz) (,;,;L =头孢唑林、头孢噻吩、头孢噻肟、头孢曲松、[Ni()(stz)]Cl(头孢吡肟)的单阴离子,用理化和光谱学方法对其进行了表征。它们的光谱表明,头孢菌素通过内酰胺羰基、羧酸盐和n -偶氮基团发挥多齿螯合剂的作用。该配合物不溶于水和普通有机溶剂,但可溶于DMSO,其中[Ni()(stz)]Cl配合物为1:1电解质。它们可能有聚合结构。对其抗菌活性进行了筛选,并与市售头孢菌素的抗菌活性进行了比较。
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引用次数: 24
Kinetic Study of Organic Dye Degradation Using ZnO Particles with Different Morphologies as a Photocatalyst 不同形貌ZnO光催化剂降解有机染料的动力学研究
Pub Date : 2012-05-08 DOI: 10.1155/2012/608183
S. Pung, Wen-Chuan Lee, A. Aziz
Zinc oxide (ZnO) particles were successfully synthesized via sol-gel approach using zinc acetate dihydrate (Zn(CH3COO)2·2H2O) and ammonia (NH4OH) solution as precursors. By adjusting the reaction parameters such as amount of ammonia and reaction time as well as complexing agent aluminium sulphate Al2(SO4)3, ZnO particles with different morphologies, that is, rodlike, ricelike and disklike could be synthesized. The effectiveness of ZnO particles with different morphologies (rodlike, ricelike and disklike) on the photocatalytic activity has been studied. The results showed that rodlike ZnO particles were the most effective in degrading the Rhodamine B (RhB) solution under the illumination of ultraviolet (UV) light. The rate constant was found to be first order, with rodlike particles the highest (0.06329 min−1), followed by rice-like ZnO particles (0.0431 min−1) and disk-like ZnO particles (0.02448 min−1).
以二水合乙酸锌(Zn(CH3COO)2·2H2O)和氨(NH4OH)溶液为前驱体,采用溶胶-凝胶法制备了氧化锌(ZnO)颗粒。通过调整氨用量、反应时间等反应参数以及络合剂硫酸铝Al2(SO4)3,可以合成棒状、米状、盘状等不同形貌的ZnO颗粒。研究了不同形态(棒状、稻状和盘状)ZnO粒子对光催化活性的影响。结果表明,在紫外光照射下,棒状ZnO颗粒对罗丹明B (RhB)溶液的降解效果最好。速率常数为一级,棒状ZnO颗粒最高(0.06329 min−1),其次是米状ZnO颗粒(0.0431 min−1)和盘状ZnO颗粒(0.02448 min−1)。
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引用次数: 96
Structural and Spectroscopic Properties of Two New IsostructuralComplexes of Lapacholate with Cobalt and Copper 两种新型拉帕酸盐与钴和铜等结构配合物的结构和光谱性质
Pub Date : 2012-04-29 DOI: 10.1155/2012/973238
R. A. Farfán, J. A. Espindola, M. Gómez, M. Jiménez, M. A. Martinez, O. Piro, E. Castellano
The molecular structures of two isostructural complexes of lapacholate (Lap) anion and dimethylformamide (DMF), M(Lap)2(DMF)2 with M: Co Cu, were determined by X-ray diffraction methods. The substances crystallize in the triclinic space group with one molecule per unit cell and cell constants (3), (3), (4) A, (2), (2), and (2)° for the Co complex and (2), (4), (4), (2), (2), and (2)° for the Cu complex. The structures were solved from 2933 (Co) and 2888 (Cu) reflections with (I) and refined by full matrix least squares to agreement R1-factors of 0.041 (Co) and 0.033 (Cu). The metal M(II) ion is sited on a crystallographic inversion center in a MO6 distorted octahedral environment. This ion is coordinated equatorially to two lapacholate anions through their adjacent carbonyl and phenol oxygen atoms [M–O bond distances of 2.134(1) and 2.008(1) A (Co) and 2.301(1) and 1.914(1) A (Cu)] and axially to two DMF molecules through oxygen atoms [M–O bond lengths of 2.143(1) A (Co) and 2.069(1) A (Cu)]. The solid state IR transmittance and solution electronic absorption spectra of both Co and Cu compounds are also reported and compared to each other and to the corresponding spectra of other members of the lapacholate metal family of complexes.
用x射线衍射法测定了拉帕胆酸酯(Lap)阴离子与二甲基甲酰胺(DMF)的M(Lap)2(DMF)2与M: Co - Cu的同构配合物的分子结构。这些物质在三斜空间群中结晶,每个单位细胞有一个分子,Co配合物的细胞常数为(3)、(3)、(4)A、(2)、(2)和(2)°,Cu配合物的细胞常数为(2)、(4)、(4)、(2)、(2)和(2)°。通过2933 (Co)和2888 (Cu)反射(I)对结构进行求解,并通过全矩阵最小二乘法进行细化,使其符合r1因子0.041 (Co)和0.033 (Cu)。在MO6畸变八面体环境中,金属M(II)离子位于晶体反转中心。该离子通过相邻的羰基氧原子和酚氧原子与两个拉帕酸盐阴离子(M-O键距离分别为2.134(1)和2.008(1)A (Co)、2.301(1)和1.914(1)A (Cu))在赤道上配位,通过氧原子与两个DMF分子(M-O键长度分别为2.143(1)A (Co)和2.069(1)A (Cu))在轴向上配位。本文还报道了Co和Cu化合物的固态红外透射光谱和溶液电子吸收光谱,并与其他拉帕孔代金属配合物家族成员的相应光谱进行了比较。
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引用次数: 4
Reversed-Phase Column Extractive Separation of Gd(III) with Poly[dibenzo-18-crown-6] 聚[二苯并-18-冠-6]反相柱萃取分离Gd(III)
Pub Date : 2012-04-22 DOI: 10.1155/2012/515196
K. Mahanwar, S. Sabale, R. B. Kadam, B. Mohite
A poly[dibenzo-18-crown-6] exhibits good chemical stability, reusability, and faster rate equilibrium for the separation of Gd(III). Both uptake and stripping of metal ions were rapid, indicating a better accessibility of the complexing sites. The proposed method has been applied for chromatographic separation of Gd(III) by using picric acid as medium and poly[dibenzo-18-crown-6] as stationary phase. The influences of picric acid concentration, different eluting agents, and so forth, were discussed and the optimum conditions were established. The breakthrough capacity of poly[dibenzo-18-crown-6] for Gd(III) was  mmolg−1 of crown polymer. The proposed method has been applied to sequential chromatographic separation of their binary and multicomponent mixtures. Gd(III) has been determined from real samples with good analytical reliability.
聚[二苯并-18-冠-6]具有良好的化学稳定性、可重复使用性和更快的Gd(III)分离速率平衡。金属离子的吸收和剥离都很快,表明络合位点的可达性更好。该方法以苦味酸为介质,聚二苯并-18-冠-6为固定相,用于Gd(III)的色谱分离。探讨了苦味酸浓度、不同洗脱剂等因素的影响,确定了最佳条件。聚[二苯并-18-冠-6]对Gd(III)的突破容量为mmolg−1。该方法已应用于其二元和多组分混合物的序贯色谱分离。Gd(III)在实际样品中测定,具有良好的分析可靠性。
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引用次数: 1
Synthesis, Characterization, and Antimicrobial and Antispermatogenic Activity of Bismuth(III) and Arsenic(III) Derivatives of Biologically Potent Nitrogen and Sulfur Donor Ligands 生物有效氮和硫供体配体的铋(III)和砷(III)衍生物的合成、表征及其抗菌和抗生精活性
Pub Date : 2012-04-22 DOI: 10.1155/2012/372141
Latika Dawara, S. Joshi, R. Singh
A series of Bi(III) and As(III) complexes with two N∩S donor ligands, 1-(4-chloro-2-oxo-2H-chromen-3-yl)-methylene)-thiosemicarbazide (L1H) and N′-[1-(2-oxo-2H-chrome-3yl-ethylidene]-hydrazinecarbodithionic acid benzyl ester (L2H) have been synthesized by the reaction of BiCl3 and Ph3As with ligands in 1 : 1 and 1 : 2 molar ratios. All the synthesized compounds were characterized by elemental analyses, melting point determinations, and a combination of electronic, IR, 1H NMR, 13C NMR spectroscopic techniques, and X-ray diffraction for structure elucidation. In order to evaluate the effect of metal ions upon chelation, both the ligands and their complexes have been screened for their antimicrobial activity against the various pathogenic bacterial and fungal strains. The metal complexes have shown to be more antimicrobial against the microbial species as compared to free ligands. Both the ligands and their corresponding metal complexes have been tested for their antifertility activity in male albino rats. The marked reduction in sperm motility and density resulted in infertility. Significant alterations were found in biochemical parameters of reproductive organs in treated animals as compared to control group. It is concluded that all these effects may finally impair the fertility of male rats.
采用bil3和Ph3As与配体以1:1和1:1的摩尔比反应,合成了一系列Bi(III)和As(III)配合物,配体为1-(4-氯-2-氧- 2h -铬-3-基)-亚甲基)-硫代氨基脲(L1H)和N ' -[1-(2-氧- 2h -铬-3-乙基]-肼二硫酸苄酯(L2H)。所有合成的化合物都通过元素分析、熔点测定、电子、红外、1H NMR、13C NMR光谱技术和x射线衍射进行了结构表征。为了评价金属离子对螯合作用的影响,筛选了配体及其配合物对各种病原菌和真菌菌株的抑菌活性。与游离配体相比,金属配合物对微生物具有更强的抗菌作用。这两种配体及其相应的金属配合物已在雄性白化大鼠身上进行了抗生育活性测试。精子活力和密度的显著降低导致不育。与对照组相比,治疗组动物生殖器官的生化参数发生了显著变化。这些影响可能最终损害雄性大鼠的生育能力。
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引用次数: 12
Synthesis, Structure, and Thermal Stability of Supramolecular Polymers with 1D Chain: 一维超分子聚合物的合成、结构及热稳定性研究
Pub Date : 2012-04-17 DOI: 10.1155/2012/274508
Y. Liu, Lingling Gao, Xulu Lv, Jianfeng Liu, Tuoping Hu
Two supramolecular polymers have been constructed from 2,3,5,6-tetrabromoterephthalic acid (H2TBTA) and 1,3-bis(4-pyridyl)propane (BPP) ligands in water-methanol dissolvant. Single-crystal X-ray and powder diffraction, IR spectroscopy, thermogravimetric analysis, and elemental analysis were employed to characterize all samples. Both of the complex compounds 1 and 2 belong to triclinic crystal system with P-1 space group. The crystal structures analysis indicates that the metal atom coordinated by two carboxylate groups from different TBTA ligands, two BPP, molecules and two H2O molecules formed a slightly distorted octahedral configuration. The compounds of 1 and 2 are 1D chains made with TBTA spacers, BPP molecules, and H2O molecules.
以2,3,5,6-四溴对苯二甲酸(H2TBTA)和1,3-双(4-吡啶基)丙烷(BPP)为配体,在水-甲醇溶剂中构建了两种超分子聚合物。单晶x射线和粉末衍射、红外光谱、热重分析和元素分析对所有样品进行了表征。配合物1和2均属于具有P-1空间群的三斜晶系。晶体结构分析表明,金属原子由不同TBTA配体的两个羧酸基、两个BPP分子和两个H2O分子配位,形成了轻微畸变的八面体构型。化合物1和2是由TBTA间隔剂、BPP分子和H2O分子组成的一维链。
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引用次数: 1
期刊
International Journal of Inorganic Chemistry
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