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Synthesis and Characterization of Metal Complexes of Acebutolol, Atenolol, and Propranolol Antihypertension Drugs 乙酰布洛尔、阿替洛尔和心得安抗高血压药物金属配合物的合成与表征
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039270
A. Gölcü, Cem Yücesoy, S. Serin
Abstract The complexation of two transition metal ions with the β‐blocker drugs acebutolol (HL1), atenolol (HL2), and propranolol (HL3) was studied in methanol and acetonitrile media at M:L (metal:ligand) molar ratio from 1:1 to 1:10. Cu(II) complexes with ligands having the stoichiometric ratio 1:4 (mononuclear copper(II) complexes) and 1:1 (binuclear copper(II) complexes) were prepared. The analytical data show that the metal to ligand ratio in the mononuclear Co(II) complexes was 1:2. The complexes were characterized on the basis of analytical data, magnetic moments, atomic absorption, infrared and electronic spectral data. Molar conductivities of the complexes at room temperature were measured. The conductivity values of the mononuclear Cu(II) complexes indicate weak electrolyte behavior, whereas the binuclear Cu(II) and mononuclear Co(II) complexes are non‐electrolytes. The thermal properties of all complexes have been studied by the DTA and TG.
摘要研究了两种过渡金属离子与β受体阻滞剂乙酰丁醇(HL1)、阿替洛尔(HL2)和心得洛尔(HL3)在甲醇和乙腈介质中,金属与配体摩尔比为1:1 ~ 1:10时的络合反应。制备了配体化学计量比为1:4(单核铜(II)配合物)和1:1(双核铜(II)配合物)的铜(II)配合物。分析数据表明,单核Co(II)配合物中金属与配体的比例为1:2。根据分析数据、磁矩、原子吸收、红外和电子光谱数据对配合物进行了表征。测量了配合物在室温下的摩尔电导率。单核Cu(II)配合物的电导率值显示出弱电解质行为,而双核Cu(II)和单核Co(II)配合物是非电解质。用差热分析(DTA)和热重分析(TG)研究了所有配合物的热性能。
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引用次数: 17
Synthesis, Spectral, and Cyclic Voltammetric Studies of Tetraaza Copper(II), Oxovanadium(IV), and Zinc(II) Complexes Derived from 1,2‐(Diimino‐4′‐antipyrinyl)‐1,2‐diphenylethane and para‐Substituted Anilines 由1,2‐(二亚胺‐4′‐安替吡啶基)‐1,2‐二苯乙烷和对取代苯胺衍生的四氮铜(II)、氧化钒(IV)和锌(II)配合物的合成、光谱和循环伏安研究
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039266
N. Raman, A. Kulandaisamy, C. Thangaraja
Abstract Tetraaza acyclic Schiff bases, prepared from 1,2‐(diimino‐4′‐antipyrinyl)‐1,2‐diphenylethane and p‐substituted anilines, act as tetradentate ligands and form solid cationic solid complexes with Cu(II), Zn(II), and VO(IV) salts in ethanol. Microanalytical data, magnetic susceptibility measurements, IR, UV‐VIS, mass, 1H and 13C NMR, and ESR spectral techniques were used to characterize the structures of synthesized compounds. IR and UV‐VIS spectra of the complexes suggest that all the copper complexes exhibit square–planar geometry while the oxovanadium complexes are of square–pyramidal geometry. Mass, 1H and 13C NMR spectra of the Schiff bases and their complexes suggest that the general formula of the complexes is [ML]Y (where L = L1, L2 or L3, Y = Cl2 or SO4). Electrolytic behaviour of the chelates was assessed from their higher conductance data. Monomeric nature of the chelates was confirmed from their magnetic susceptibility values. Redox studies by cyclic voltammetry of copper complexes in MeCN suggest the existence of unusual oxidation states such as Cu(III), Cu(I), and Cu(0) which are stabilized by the ligand systems. The cyclic voltammogram of the oxovanadium complexes in MeCN shows two quasi‐reversible peak for the VO(IV)/VO(V) and VO(IV)/VO(III) couples. The X‐band ESR spectra of copper and oxovanadium complexes in DMSO solution at 300 and 77 K were recorded and their salient features are discussed.
摘要由1,2‐(二亚氨基‐4′‐安替吡啶基)‐1,2‐二苯乙烷和对取代苯胺制备的四氮杂无环席夫碱作为四齿配体,在乙醇中与Cu(II)、Zn(II)和VO(IV)盐形成固体阳离子配合物。利用微量分析数据、磁化率测量、IR、UV - VIS、质量、1H和13C NMR以及ESR光谱技术对合成化合物的结构进行了表征。配合物的IR和UV - VIS光谱表明,所有铜配合物都呈方平面几何形状,而氧化钒配合物则呈方锥体几何形状。席夫碱及其配合物的质量、1H和13C核磁共振谱表明,配合物的通式为[ML]Y(其中L = L1、L2或L3, Y = Cl2或SO4)。根据其高电导数据评估了螯合物的电解行为。通过磁化率值确定了螯合物的单体性质。通过循环伏安法对MeCN中铜配合物的氧化还原研究表明,存在不寻常的氧化态,如Cu(III), Cu(I)和Cu(0),这些氧化态被配体系统稳定。MeCN中氧化钒配合物的循环伏安图显示VO(IV)/VO(V)和VO(IV)/VO(III)对有两个准可逆峰。记录了铜和钒氧配合物在DMSO溶液中300和77 K的X波段ESR光谱,并讨论了它们的显著特征。
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引用次数: 10
Synthesis, Structural Characterization, and Antibacterial Studies of Some Mixed‐Ligand First Row d‐Transition Metal Complexes 一些混合配体第一行过渡金属配合物的合成、结构表征和抗菌研究
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039271
P. K. Panchal, M. Patel
Abstract Some mixed‐ligand complexes of the transition metal ions Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II) with the potassium salt of salicylideneglycine and 2,2′‐bipyridylamine or di(benzylidene)‐1,8‐diaminonaphthalene have been prepared. The coordination behavior of the mixed‐ligand complexes was characterized on the basis of elemental analyses, IR, and electronic spectra. The magnetic measurements have been obtained by a vibrating sample magnetometer. It is observed that the mixed‐ligand complexes of Mn(II), Co(II), Ni(II), Cu(II) are paramagnetic, while the Zn(II) and Cd(II) complexes are diamagnetic. All of these mixed‐ligand complexes are colored crystalline solids. Octahedral geometries have been assigned to all of the prepared mixed‐ligand complexes. The antibacterial activities of the ligands, the metal chlorides, the mixed‐ligand complexes, the standard drug (tetracycline), and control (dimethyl sulfoxide) were tested on the pathogenic bacteria S. typhi, E. coli, and Serratia marcescens using the “disc diffusion method,” and the results are discussed.
摘要制备了过渡金属离子Mn(II)、Co(II)、Ni(II)、Cu(II)、Zn(II)和Cd(II)与水杨基甘氨酸钾盐和2,2′‐联吡啶胺或二(苄基)‐1,8‐二氨基萘的混合配体配合物。混合配体配合物的配位行为通过元素分析、红外光谱和电子光谱进行了表征。磁性测量是用振动样品磁强计测得的。结果表明,Mn(II)、Co(II)、Ni(II)、Cu(II)的混合配体配合物具有顺磁性,而Zn(II)和Cd(II)配合物具有反磁性。所有这些混合配体配合物都是彩色的结晶固体。所有制备的混合配体配合物都具有八面体几何形状。采用“圆盘扩散法”测定了配体、金属氯化物、混合配体配合物、标准药(四环素)和对照药(二甲亚砜)对致病菌伤寒沙门氏菌、大肠杆菌和粘质沙雷氏菌的抑菌活性,并对结果进行了讨论。
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引用次数: 45
Synthesis and Spectroscopic Studies of Metal Complexes of N,N′‐p‐Phenylenedimethylenebis(pyridin‐4‐one) with d‐ and f‐Block Metal Ions N,N′-对苯基二甲基双(吡啶- 4 - 1)与d -和f -嵌段金属离子配合物的合成和光谱研究
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039269
D. Goodgame, Amanda M Menzer
Abstract The preparations are reported for a range of complexes of the ligand N,N′‐p‐phenylenedimethylenebis(pyridin‐4‐one) (XBP) with the d‐block ions Mn(II) to Zn(II) and also with Cd(II), Y(III), and the lanthanide ions. Relevant solid state EPR, electronic and far‐IR spectra are reported and interpreted in terms of the metal ion coordination geometries and, where appropriate, the likely long‐range polymeric structures of the compounds. The value of the zero‐field splitting (zfs) parameter, D = 0.069 cm−1, obtained from the S = 1 type EPR spectrum of the compound {[Cu2(XBP)3(NO3)2](NO3)2 · 2H2O} n is compared with those of other compounds involving discrete Cu · Cu dimer interaction. The results of luminescence measurements on the complexes of Sm(III), Eu(III), Tb(III), and Dy(III) are also given.
摘要报道了一系列配体N,N′-对苯基二亚甲基双(吡啶- 4 - 1)(XBP)与d -嵌段离子Mn(II)至Zn(II)以及与Cd(II)、Y(III)和镧系离子的配合物的制备。相关的固态EPR、电子和远红外光谱被报道并解释为金属离子配位几何形状,在适当的情况下,化合物可能的远程聚合物结构。本文比较了化合物{[Cu2(XBP)3(NO3)2](NO3)2·2H2O} n的S = 1型EPR谱的零场分裂(zfs)参数D = 0.069 cm−1与其他涉及离散Cu·Cu二聚体相互作用的化合物的值。给出了Sm(III)、Eu(III)、Tb(III)和Dy(III)配合物的发光测量结果。
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引用次数: 2
Hydroxyphenoxyethyl Ether Dye: Synthesis, Complexation, and Alkali Metal Transport 羟基苯氧乙醚染料:合成、络合和碱金属运输
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039273
B. Pandya, S. Menon, Y. Agrawal
Abstract The synthesis and laser behavior of bis[4‐(2‐benzothiazole‐azo)‐(2‐(o‐hydroxyphenoxy)ethyl)] ether (BTHE) dye has been studied. Its complexation with alkali and alkaline earth metal ions is reported. The extent of complexations, i.e., percentage extraction, extraction constant, distribution ratio, and stability constant were determined and discussed. The liquid membrane transport of sodium and potassium ions with BTHE was also studied.
摘要研究了双[4‐(2‐苯并噻唑‐偶氮)‐(2‐(o‐羟基苯氧基)乙基)]醚(BTHE)染料的合成及其激光性能。报道了其与碱和碱土金属离子的络合作用。测定并讨论了络合程度,即萃取率、萃取常数、配位比和稳定性常数。研究了BTHE对钠离子和钾离子的液膜转运。
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引用次数: 1
Preparation and Thermal, Spectroscopic, and Antibacterial Studies of Some Mixed‐Ligand Complexes 一些混合配体配合物的制备、热、光谱和抗菌研究
Pub Date : 2004-08-01 DOI: 10.1081/SIM-120039268
P. K. Panchal, D. Patel, M. Patel
Abstract The present investigation reports the synthesis, characterization, and antibacterial activities of some mixed‐ligand complexes of the type [ML(SB)H2O], where M = Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II), SB1 = bis(benzylidene)ethylenediamine (benen) or SB2 = bis(acetophenone)ethylenediamine (acphen) and KHL = potassium salt of salicylideneglycine (salgly). Their structures have been elucidated on the basis of elemental analyses, thermogravimetric analyses, magnetic measurements, reflectance spectra, and IR spectra. The results are in accord with an octahedral environment around the central metal ion. The mixed‐ligand complexes of Mn(II), Co(II), Ni(II), and Cu(II) are paramagnetic while the Zn(II) and Cd(II) complexes are diamagnetic. The mixed‐ligand complexes have been tested against bacteria and the results are compared with a standard drug (tetracycline) and control (dimethyl sulfoxide).
摘要本文报道了M = Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), SB1 =双(苯二烯)乙二胺(benen)或SB2 =双(苯乙酮)乙二胺(acphen)和KHL =水杨基氨基甘氨酸(salgly)钾盐[ML(SB)H2O]型混合配体配合物的合成、表征和抗菌活性。根据元素分析、热重分析、磁测量、反射光谱和红外光谱对其结构进行了表征。结果符合中心金属离子周围的八面体环境。Mn(II)、Co(II)、Ni(II)和Cu(II)的混合配体配合物是顺磁性的,而Zn(II)和Cd(II)配合物是反磁性的。已经对混合配体复合物进行了抑菌试验,并将结果与标准药物(四环素)和对照药物(二甲亚砜)进行了比较。
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引用次数: 13
Synthesis and Magnetism of {[Cu(II)]2Ln(III)} Heterotrinuclear Complexes Bridged by N,N'‐bis(3‐Amino‐2‐methylpropyl)oxamidocopper(II) N,N′-二(3‐氨基‐2‐甲基丙基)氧胺铜(II)桥接{[Cu(II)]2Ln(III)}杂三核配合物的合成及磁性研究
Pub Date : 2004-07-01 DOI: 10.1081/SIM-120037522
Yan-Tuan Li, Cui‐Wei Yan, Chunyuan Zhu
Abstract Ten new μ‐oxamido‐bridged {[Cu(II)]2Ln(III)}‐type heterotrinuclear complexes described by the overall formula Cu2(Meoxpn)2Ln(NO3)3 (Ln = Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er), where Meoxpn denotes the N,N′‐bis(3‐amino‐2‐methylpropyl)oxamido dianion, have been synthesized and characterized by elemental analyses, molar conductivity measurements, and spectroscopic (IR, UV, and ESR) characterization. Magnetic susceptibility (4.2–300 K) studies of the Cu2(Meoxpn)2–Gd(NO3)3 complex have revealed that the central gadolinium(III) and terminal copper(II) ions are ferromagnetically coupled with the exchange integral J (Cu–Gd) = +3.85 cm−1, while an antiferromagnetic coupling is detected between the two terminal copper(II) ions with the exchange integral J′(Cu–Cu) = −0.98 cm−1, on the basis of the spin Hamiltonian operator [ Ĥ = −2J (Ŝ Cu1 Ŝ Gd + Ŝ Cu2 Ŝ Gd) − 2J′(Ŝ Cu1 Ŝ Cu2)].
摘要合成了10个新的μ -氧胺-桥接{[Cu(II)]2Ln(III)} -型杂三核配合物,其分子式为Cu2(Meoxpn)2Ln(NO3)3 (Ln = Y, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er),其中Meoxpn表示N,N ' -二(3 -氨基- 2 -甲基丙基)氧胺二离子,并通过元素分析、摩尔电导率测量和光谱(IR, UV和ESR)表征进行了表征。磁化率(4.2 -300 K)的研究的忍耐力(Meoxpn) 2-Gd(3号)3复杂显示,中央钆(III)和终端铜(II)离子ferromagnetically加上交换积分J (Cu-Gd) =−1 + 3.85厘米,而反铁磁性耦合检测到两个终端之间的铜(II)离子交换积分J的(Cu-Cu) =−0.98厘米−1的基础上自旋哈密顿算符[Ĥ=−2 J(ŜCu1ŜGd +ŜCu2ŜGd)−2 J”(ŜCu1Ŝ忍耐力]。
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引用次数: 0
Synthesis and Physico‐chemical Studies on a 15‐Membered Hexaaza Macrocyclic Ligand Derived from Hydrazine and Its Complexes with Co(II), Ni(II), Cu(II), and Zn(II) 联氨衍生15元六联体大环配体及其Co(II)、Ni(II)、Cu(II)、Zn(II)配合物的合成与物理化学研究
Pub Date : 2004-07-01 DOI: 10.1081/SIM-120039262
M. Shakir, Nishat Begum, S. Parveen, P. Chingsubam, S. Tabassum
Abstract The macrocyclic ligand, 1,2,6,9,13,14‐hexaaza‐3,5,10,12‐tetramethylcyclopentadecane‐2,5,9,12‐tetraene (L), has been prepared by the condensation reaction of hydrazine, formaldehyde, ethylenediamine, and 2,4‐pentanedione in 2:1:1:2 molar ratio. Metal complexes of the type [MLX2] (M = Co(II), Ni(II), Cu(II), and Zn(II); X = Cl or NO3) have been synthesized by the reaction of L with the corresponding metal salts in methanol. The macrocyclic ligand (L) and its metal complexes have been characterized by elemental analyses, FT‐IR and 1H and 13C NMR spectral studies. The stereochemistry of the metal complexes have been deduced from magnetic moments and band positions in the electronic spectra.
摘要以肼、甲醛、乙二胺和2,4 -戊二酮为原料,以2:1:1:2的摩尔比缩合反应制备了大环配体1,2,6,9,13,14‐六aza‐3,5,10,12‐四甲基环戊烷‐2,5,9,12‐四烯(L)。[MLX2]型金属配合物(M = Co(II), Ni(II), Cu(II), Zn(II));L与相应的金属盐在甲醇中反应合成了X = Cl或NO3)。大环配体(L)及其金属配合物已通过元素分析、FT - IR、1H和13C NMR谱研究进行了表征。根据电子能谱中的磁矩和能带位置,推导出金属配合物的立体化学性质。
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引用次数: 14
Synthesis, Crystal Structure, and Properties of Novel Five‐Coordinate Complexes of Zinc(II) and Copper(II) with tris(2‐Benzimidazolylmethyl)amine 锌(II)和铜(II)与三(2‐苯并咪唑甲基)胺新型五配位配合物的合成、晶体结构和性质
Pub Date : 2004-07-01 DOI: 10.1081/SIM-120037524
Hui‐lu Wu, Wei Ying, L. Pen, Yici. Gao, Kai-bei Yu
Abstract Two complexes of zinc(II) and copper(II) with tris(2‐benzimidazolylmethyl)amine (ntb) and the anion of acrylic acid of the compositions [M(ntb)(acrylate)](acrylate) · 2.5H2O (M = Zn or Cu) were synthesized and characterized by means of elemental analyses, thermal analyses, IR and H1 NMR spectra. The crystal structure of the novel compound [Zn(ntb)(acrylate)](acrylate) · 1.63H2O has been determined by a single‐crystal x‐ray diffraction method and shows that each zinc ion is linked to tris(2‐benzimidazolylmethyl)amine (ntb) and an acrylate; but another acrylate is the anion of the complex. The zinc ion is five‐coordinate with a N4O ligand set. The coordination geometries of the zinc ion maybe best described as a distorted trigonal‐bipyramid of site symmetry C3.
摘要合成了锌(II)和铜(II)与三(2‐苯并咪唑甲基)胺(ntb)和丙烯酸阴离子[M(ntb)(丙烯酸酯)](丙烯酸酯)·2.5H2O (M = Zn或Cu)的配合物,并用元素分析、热分析、红外光谱和H1核磁共振光谱对其进行了表征。用单晶x射线衍射法测定了新化合物[Zn(ntb)(丙烯酸酯)](丙烯酸酯)·1.63H2O的晶体结构,结果表明,每个锌离子与三(2‐苯并咪唑甲基)胺(ntb)和丙烯酸酯相连;但另一种丙烯酸酯是复合物的阴离子。锌离子为五配位,配位为n40o。锌离子的配位几何可能最好描述为C3位对称的扭曲三角-双金字塔。
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引用次数: 28
Synthesis, Characterization, and Photochemical Studies of Some Copper Complexes of Schiff Bases Derived from 3‐Hydrazino‐6‐methyl[1,2,4]triazin‐5(4H)one 3‐Hydrazino‐6‐methyl[1,2,4]triazin‐5(4H)one衍生Schiff碱铜配合物的合成、表征及光化学研究
Pub Date : 2004-07-01 DOI: 10.1081/SIM-120039258
A. Osman, M. Saleh, S. Mahmoud
Abstract Cu(II) complexes of new bidentate and tridentate Schiff bases derived from the condensation of 3‐hydrazino‐6‐methyl[1,2,4]triazin‐5(4H)one and aromatic aldehyde derivatives were synthesized and characterized. The structure of the complexes proposed according to elemental analyses, molar conductance, IR UV‐Visible absorption spectra is square‐planar. The thermodecomposition kinetics of the complexes were investigated under non‐isothermal condition. TG and DTG curves indicated that the complexes decompose in three to six steps. The photochemical behavior of the complexes depends on the substituted group on the aromatic aldehyde. A mechanism has been suggested to account for the recorded results.
摘要合成了由3‐肼基- 6‐甲基[1,2,4]三嗪- 5(4H) 1与芳香醛衍生物缩合而成的新型双齿和三齿席夫碱配合物Cu(II)。根据元素分析、摩尔电导、红外-紫外-可见吸收光谱,提出了配合物的方平面结构。在非等温条件下研究了配合物的热分解动力学。TG和DTG曲线表明,配合物的分解分为3 ~ 6步。配合物的光化学行为取决于芳香醛上的取代基。已经提出了一种机制来解释记录的结果。
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引用次数: 13
期刊
Synthesis and Reactivity in Inorganic and Metal-organic Chemistry
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