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Synthesis of New Zirconium(IV) Complexes with Amino Acid Schiff Bases: Spectral, Molecular Modeling, and Fluorescence Studies 含氨基酸席夫碱的新型锆配合物的合成:光谱、分子模拟和荧光研究
Pub Date : 2013-02-21 DOI: 10.1155/2013/847071
H. Singh, J. Singh
New zirconium(IV) complexes were synthesized with bidentate ligands and characterized by elemental analysis, molar conductance measurements, molecular weight determinations, IR, electronic, NMR (1H and 13C), fluorescence and molecular modeling studies. All the complexes are 1 : 2 electrolytes in nature and may be formulated as [Zr(L)2Cl2] (where L is Schiff bases of amino acids and substituted isatin). The analytical data showed that the Schiff-base ligand acts as bidentate toward zirconium ion via the azomethine nitrogen and carboxylate oxygen. The conductivity values between 8.5–12.6 Ω−1, mol−1, cm2 in DMF imply the presence of nonelectrolyte species. On the basis of spectral and molecular modeling studies, the resulting complexes are proposed to have octahedral geometries.
用双齿配体合成了新的锆(IV)配合物,并通过元素分析、摩尔电导测量、分子量测定、IR、电子、NMR (1H和13C)、荧光和分子模型研究对其进行了表征。所有配合物在性质上都是1:2电解质,可配制为[Zr(L)2Cl2](其中L为氨基酸和取代isatin的希夫碱)。分析数据表明,希夫碱配体通过亚甲基氮和羧酸氧对锆离子起双齿作用。DMF的电导率值在8.5-12.6 Ω−1,mol−1,cm2之间,表明存在非电解质物质。在光谱和分子模型研究的基础上,得到的配合物具有八面体的几何形状。
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引用次数: 15
Synthesis, Characterization, and Biological Evaluation of Some 3d-Metal Complexes of Schiff Base Derived from Xipamide Drug 希帕胺类药物席夫碱三维金属配合物的合成、表征及生物学评价
Pub Date : 2013-02-18 DOI: 10.1155/2013/549805
S. Malik, Suparna Ghosh, B. Jain, Archana Singh, M. Bhattacharya
The present paper deals with the synthesis and characterization of metal complexes of Schiff base derived from xipamide, a diuretic drug. The bidentate ligand is derived from the inserted condensation of 5-aminosulfonyl-4-chloro-N-2,6-dimethyl phenyl-2-hydroxybenzamide (Xipamide) with salicylaldehyde in a 1 : 1 molar ratio. Using this bidentate ligand, complexes of Hg(II), Zn(II), and VO(IV) with general formula ML2 have been synthesized. The synthesized complexes were characterized by several techniques using molar conductance, elemental analysis, magnetic susceptibility, FT-IR spectroscopy, electronic spectra, mass spectra, and particle size analysis. The elemental analysis data suggest the stoichiometry to be 1 : 2 [M : L]. All the complexes are nonelectrolytic in nature as suggested by molar conductance measurements. Infrared spectral data indicate the coordination between the ligand and the central metal ion through deprotonated phenolic oxygen and azomethine nitrogen atoms. Spectral studies suggest tetrahedral geometry for Hg(II), Zn(II) complexes, and square pyramidal geometry for VO(IV) complex. The pure drug, synthesized ligand, and metal complexes were screened for their antifungal activities against Aspergillus niger and Aspergillus flavus. The ligand and its Hg(II) and VO(IV) complexes were screened for their diuretic activity too.
本文研究了利尿剂西帕胺席夫碱金属配合物的合成和表征。该双齿配体是由5-氨基磺酰基-4-氯- n -2,6-二甲基苯基-2-羟基苯酰胺(西帕胺)与水杨醛以1:1的摩尔比缩合而成。利用该双齿配体,合成了通式ML2的Hg(II)、Zn(II)和VO(IV)配合物。通过摩尔电导、元素分析、磁化率、红外光谱、电子光谱、质谱和粒度分析等方法对合成的配合物进行了表征。元素分析数据表明,其化学计量比为1:2 [M: L]。摩尔电导测量表明,所有配合物本质上都是非电解的。红外光谱数据表明配体与中心金属离子通过去质子化的酚氧和亚甲基氮原子进行配位。光谱研究表明,Hg(II)、Zn(II)配合物呈四面体结构,VO(IV)配合物呈方锥体结构。对纯药物、合成配体和金属配合物对黑曲霉和黄曲霉的抑菌活性进行了筛选。并对该配体及其Hg(II)和VO(IV)配合物的利尿活性进行了筛选。
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引用次数: 16
Synthesis and Crystal Structure of 的合成及晶体结构
Pub Date : 2013-01-16 DOI: 10.1155/2013/153023
Thampidas V. S, Aisha Basheer, S. Shyla
The title compound was synthesized by the reaction between a manganese(II) carboxylate and the tetradentate Schiff base ligand, 5-Br-salpnH2 [N,N′-bis(5-Br-salicylidene)-1,3-diaminopropane] produced in situ. The complex crystallizes in the P21/c space group with unit cell dimensions (10), (10), (3), , (10), and . The manganese(III) ion is in a distorted octahedral environment with longer axial bonds.
该化合物由锰(II)羧酸盐与原位生成的四齿席夫碱配体5-Br-salpnH2 [N,N ' -双(5- br -水杨基)-1,3-二氨基丙烷]反应合成。该配合物在P21/c空间群中结晶,其胞元尺寸为(10)、(10)、(3)、(10)和。锰(III)离子处于扭曲的八面体环境中,具有较长的轴向键。
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引用次数: 128
Studies on Synthesis and Spectral Characterization of Some Transition Metal Complexes of Azo-Azomethine Derivative of Diaminomaleonitrile 偶氮-偶氮甲腈衍生物过渡金属配合物的合成及光谱表征研究
Pub Date : 2013-01-16 DOI: 10.1155/2013/436275
C. Anitha, C. D. Sheela, P. Tharmaraj, R. Shanmugakala
New complexes of 2,3-bis(5-(4-chlorophenyl)diazenyl)-2-hydroxybenzylideneamino)maleonitrile (CDHBDMN) with VO(II), Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) were synthesized and characterized by analytical and physicochemical techniques, that is, elemental analyses, molar conductivity, UV, IR, EPR, 1H-NMR spectra, magnetic susceptibility and also by aid of scanning electron microscopy (SEM), nonlinear optical study (NLO), fluorescence spectral studies, and solvatochromic behaviors. Electronic and magnetic susceptibility measurements of the complexes indicate square pyramidal geometry for VO(II), octahedral for Ni(II), and square planar geometry for all the other complexes. The EPR spectral data provide information about their structures on the basis of Hamiltonian parameters and the degree of covalency. These metal complexes were also tested for their antibacterial and antifungal activities to assess their inhibiting potential. Metal-mediated fluorescence enhancement is observed on complexation of the azo Schiff base ligand. The synthesized compounds were investigated for nonlinear optical properties, and the surface morphology of the Cu(II) complex was studied by scanning electron microscopy.
合成了与VO(II)、Mn(II)、Co(II)、Ni(II)、Cu(II)和Zn(II)组成的2,3-二(5-(4-氯苯基)二氮基)-2-羟基苄基氨基)马来腈(CDHBDMN)新型配合物,并通过元素分析、摩尔电导率、紫外、红外、EPR、1H-NMR、磁化率、扫描电镜(SEM)、非线性光学研究(NLO)、荧光光谱研究和溶剂致变色行为等分析和物理化学方法对其进行了表征。电子和磁化率测量表明,VO(II)为正方形锥体,Ni(II)为八面体,其他配合物为正方形平面。EPR谱数据提供了基于哈密顿参数和共价度的结构信息。这些金属配合物的抗菌和抗真菌活性也进行了测试,以评估其抑制潜力。在偶氮席夫碱配体的络合上观察到金属介导的荧光增强。研究了所合成化合物的非线性光学性质,并用扫描电镜研究了Cu(II)配合物的表面形貌。
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引用次数: 37
Synthesis and Studies on S-Triazine-Based Ligand and Its Metal Complexes s -三嗪基配体及其金属配合物的合成与研究
Pub Date : 2012-12-17 DOI: 10.1155/2012/301086
R. Shanmugakala, P. Tharmaraj, C. D. Sheela, C. Anitha
Tridentate chelate complexes of ML type (where M = Cu(II), Ni(II), and Co(II)) have been synthesized from triazine-based ligand 4,6-bis(5-mercapto-1,3,4-thiadiazol-amine)2-phenylamino-1,3,5-triazine (BMTDT). Microanalytical data, magnetic susceptibility measurements, IR, 1H NMR, UV-vis, mass, and EPR spectral techniques were used to characterise the structure of chelates. The electronic absorption spectra and magnetic susceptibility measurements suggest that metal complexes show square pyramidal geometry. The electrochemical behavior of copper(II) complex is studied by cyclic voltammetry. All synthesized compounds may serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic generation efficiency (SHG) of the ligand and metal complexes has been found to be higher than that of urea and KDP. The antimicrobial activity of the ligand and metal(II) complexes against the species Shigella, Chromobacterium, Staphylococcus aureus, Candida albicans, and Aspergillus niger has been carried out and compared with the standard one.
以三嗪基配体4,6-二(5-巯基-1,3,4-噻二唑胺)- 2-苯胺-1,3,5-三嗪(BMTDT)为原料合成了ML型(M = Cu(II), Ni(II)和Co(II))的三齿螯合物。采用微量分析数据、磁化率测量、IR、1H NMR、UV-vis、质量和EPR光谱技术表征螯合物的结构。电子吸收光谱和磁化率测量表明,金属配合物呈方锥体形状。采用循环伏安法研究了铜(II)配合物的电化学行为。所有合成的化合物都可以作为潜在的光活性材料,从它们的荧光特性可以看出。发现配体和金属配合物的二次谐波产生效率(SHG)高于尿素和KDP。研究了该配体和金属(II)配合物对志贺氏菌、色杆菌、金黄色葡萄球菌、白色念珠菌和黑曲霉的抑菌活性,并与标准配体进行了比较。
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引用次数: 28
Synthesis, Characterization, and Biological Activity of Some Transition Metal Complexes of N-Benzoyl-N′-2-thiophenethiocarbohydrazide n -苯甲酰- n′-2-噻吩硫代碳酰肼过渡金属配合物的合成、表征及生物活性
Pub Date : 2012-12-02 DOI: 10.1155/2012/269497
M. Yadav
In the present study, Mn(II), Fe(II), Ni(II), and Cu(II) complexes of N-benzoyl -N′-2-thiophenethiocarbohydrazide (H2 BTTH) have been synthesized and characterized by elemental analysis, magnetic susceptibility measurements, infrared, NMR, electronic, and ESR spectral studies. The complexes were found to have compositions [Mn(H BTTH)2], [Ni(BTTH)(H2O)2], [Cu(BTTH)], and [Fe(H BTTH)2EtOH]. The antibacterial and antifungal properties of H2 BTTH and its metal complexes have been screened against several bacteria and fungi.
本研究合成了n -苯甲酰-N′-2-噻吩乙硫代碳酰肼(H2 BTTH)的Mn(II)、Fe(II)、Ni(II)和Cu(II)配合物,并通过元素分析、磁化率、红外、核磁共振、电子和ESR光谱研究对其进行了表征。发现配合物具有[Mn(H BTTH)2], [Ni(BTTH)(H2O)2], [Cu(BTTH)]和[Fe(H BTTH)2EtOH]的成分。H2 BTTH及其金属配合物对多种细菌和真菌具有抗菌和抑菌作用。
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引用次数: 4
Na3MP3O10·12H2O (M = Co, Ni): Crystal Structure and IR Spectroscopy Na3MP3O10·12H2O (M = Co, Ni):晶体结构和红外光谱
Pub Date : 2012-11-27 DOI: 10.1155/2012/702471
K. Azzaoui, R. Essehli, E. Mejdoubi, B. Bali, M. Dušek, K. Fejfarová
Two new dodecahydrate trisodium triphosphates Na3MP3O10·12H2O (M = Co (1), Ni (2)) were synthesized using a wet chemistry route and characterized by X-ray diffraction and FT-IR spectroscopy. They are isotypic, monoclinic (P21/, ), with pseudoorthorhombic unit cell parameters (Ǻ,°): ( (4), (2), (4), (2), for (1) and (3), (2), (3), (16) for (2)). Values of / are 0.0267/0.0738 and 0.0284/0.0907, respectively, for (1) and (2). Both compounds were found to be systematically twinned by 180° rotation around . Their frameworks are made by slabs parallel to plane, resulting from the cohesion of two kinds of metallic chains. IR spectrum confirms the presence of characteristic bands from P3O10 phosphate group.
采用湿化学方法合成了两种新型十二水三磷酸三钠Na3MP3O10·12H2O (M = Co (1), Ni(2)),并用x射线衍射和红外光谱对其进行了表征。它们是同型的,单斜的(P21/,),具有伪正交的单位细胞参数(Ǻ,°):(4),(2),(4),(2)和(3),(2),(3),(16)。(1)和(2)的/值分别为0.0267/0.0738和0.0284/0.0907。这两种化合物在180°旋转时都是系统孪生的。它们的框架是由平行于平面的板构成的,这是两种金属链的凝聚力造成的。红外光谱证实了P3O10磷酸基特征带的存在。
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引用次数: 2
Preparation, Analytical, IR Spectral, and Thermal Studies of Some New Hydrazinium Carboxylates 几种新型羧酸肼酯的制备、分析、红外光谱和热研究
Pub Date : 2012-11-05 DOI: 10.1155/2012/624374
R. Manimekalai, C. Sinduja, K. Kalpanadevi
Hydrazinium salts of 2,4-dichlorophenylacetic acid, phenoxyacetic acid, 2,4-dichlorophenoxyacetic acid, diphenylacetic acid, cinnamic acid, and picolinic and nicotinic acids have been prepared by accomplishing neutralization of aqueous hydrazine hydrate with the respective acids. Formation of these hydrazinium salts has been confirmed by analytical, IR spectral, and thermal studies. IR spectra of the salts register N–N stretching frequencies of ion in the region 963–951 cm−1 and the frequencies of ion in the region 1047–1026 cm−1. Thermal decomposition studies show that the hydrazinium salts undergo melting followed by endothermic decomposition into carbon residue as the endproduct.
通过对水合肼进行中和,制备了2,4-二氯苯乙酸、苯氧乙酸、2,4-二氯苯氧乙酸、二苯基乙酸、肉桂酸、吡啶酸和烟酸的肼盐。这些肼盐的形成已被分析、红外光谱和热研究证实。盐的红外光谱记录了离子在963 ~ 951 cm−1区域的N-N拉伸频率和离子在1047 ~ 1026 cm−1区域的频率。热分解研究表明,肼盐熔融后吸热分解为最终产物碳渣。
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引用次数: 2
Structure and Magnetic Properties of Aerosol Nanoparticles of Fe and Its Alloys 铁及其合金气溶胶纳米颗粒的结构和磁性能
Pub Date : 2012-09-11 DOI: 10.1155/2012/610305
Y. Petrov, E. Shafranovsky
Structure and magnetic properties of aerosol nanoparticles of Fe and its alloys (FeMn, FeNi, FeNiMn, FePt, FeCr, FeCo, and FeCu) have been reviewed. It has been shown that, compared to a bulk material, the particles have a number of specific features being of much fundamental and applied interest. The effect of both a quenched high-temperature Fe modification and its oxides on the structure and magnetism of nanoparticles has been considered in detail. Particular attention has been paid to the recently observed fine structure in the hyperfine field distribution at iron nuclei in Mossbauer spectra for pure iron and its alloys both as a bulk and aerosol nanoparticles. This phenomenon makes it possible to reveal very weak magnetic interactions in the system under study. The plausible origin of these magnetic interactions has been also discussed.
本文综述了铁及其合金(FeMn、FeNi、FeNiMn、FePt、FeCr、FeCo和FeCu)气溶胶纳米颗粒的结构和磁性能。已经证明,与大块材料相比,颗粒具有许多具有基本和应用价值的特定特征。研究了高温淬火铁改性及其氧化物对纳米颗粒结构和磁性的影响。在穆斯堡尔谱中,纯铁及其合金的体纳米粒子和气溶胶纳米粒子在铁核处的超精细场分布中,最近观察到的精细结构得到了特别的关注。这种现象使得揭示所研究的系统中非常弱的磁相互作用成为可能。还讨论了这些磁相互作用的可能起源。
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引用次数: 7
Synthesis and Characterization of Nanosized Fe2O3 Pigments 纳米Fe2O3颜料的合成与表征
Pub Date : 2012-08-13 DOI: 10.1155/2012/989281
M. Fouda, M. El-Kholy, S. Moustafa, A. Hussien, M. Wahba, M. El-shahat
The work in this paper was devoted to investigating some nanosized iron oxide pigments prepared by microemulsion technique. The role of concentration of iron salt and surfactant (cetyltrimethylammonium bromide) on the produced iron oxide was studied. The techniques employed to characterize the samples were thermogravimetric analysis, X-ray diffractometry, transmission electron microscope, infrared spectroscopy, and diffuse reflectance spectroscopy. The results revealed that the particle size of the prepared sample using 0.2 M iron sulfate and 3.2 wt% of surfactant was in the range 7–9 nm. Increasing the concentration of either iron salt or the surfactant increased the particle size of the obtained ferric oxide. The diffuse reflectance measurements showed that the charge transfer/electron pair transition absorption peak, which is closely related to the reddish color of the oxide, was shifted to a longer wavelength (blue shift) by decreasing the dimension of the particles. The samples were tested as pigments. They showed different tints of red color and were found to be promising for applications as pigments in the field of paint manufacturing.
研究了用微乳液法制备的几种纳米氧化铁颜料。研究了铁盐浓度和表面活性剂十六烷基三甲基溴化铵对产物氧化铁的影响。表征样品的技术包括热重分析、x射线衍射、透射电子显微镜、红外光谱和漫反射光谱。结果表明,0.2 M硫酸铁和3.2 wt%表面活性剂制备的样品粒径在7 ~ 9 nm范围内。增加铁盐或表面活性剂的浓度,所得到的氧化铁的粒径增大。漫反射测量表明,随着粒子尺寸的减小,与氧化物红色密切相关的电荷转移/电子对跃迁吸收峰向更长的波长(蓝移)偏移。这些样品作为颜料进行了测试。它们显示出不同的红色色调,被发现在油漆制造领域作为颜料有很大的应用前景。
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引用次数: 22
期刊
International Journal of Inorganic Chemistry
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