N(1)取代5-氟尿嘧啶乙酸、5-氟尿嘧啶丙酸与Cu(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Zn(Ⅱ)、Mn(Ⅱ)的配合物的合成及表征

合成了N(1)取代5-氟尿嘧啶乙酸、5-氟尿嘧啶丙酸与铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)和锰(Ⅱ)的十种金属配合物。通过元素分析、差热-热重分析确定了它们的化学组成,并对这些化合物进行了红外光谱、氢核磁共振谱,电子光谱的表征。讨论了各配合物中金属离子与配体的配位状态。在Cu(Ⅱ)配合物中,Cu(Ⅱ)是与配体的N~3原子和C~4上的羰基氧原子配位,其他金属配合物中,金属离子是与配体的C~2的羰基氧原子和羧基配位。     

某些酸性磷(膦)酸酯-Co(Ⅱ)、Ni(Ⅱ)、VO(Ⅱ)配合物的电子光谱和ESR波谱

本文对某些酸性磷(膦)酸酯与Co(Ⅱ)、Ni(Ⅱ)、VO(Ⅱ)配合物的电子光谱进行了测定,讨论了这类配合物的构型和光谱参数对萃取性能的影响。实验测得并计算了VO(Ⅱ)配合物的ESR波谱参数和键参数,对这类配合物的成键特性进行了讨论。     

锰(Ⅱ)、钴(Ⅱ)、铜(Ⅱ)和镉(Ⅱ)与吡哆醇配合物的结构研究

本文合成了吡哆醇与锰(Ⅱ)、钴(Ⅱ)、铜(Ⅱ)和镉(Ⅱ)的配合物。通过元素分析确定了配合物的组成。通达摩尔电导、比移值,紫外光谱、红外光谱和核磁共振谱的测定和分析,推断了配合物的结构。     

含草酰胺桥的Cu(Ⅱ)-Fe(Ⅱ)和Cu(Ⅱ)-Zn(Ⅱ)双核配合物的合成、磁性及生物活性

抗菌活性;含草酰胺桥的Cu(Ⅱ)-Fe(Ⅱ)和Cu(Ⅱ)-Zn(Ⅱ)双核配合物的合成、磁性及生物活性     

N(1)取代5-氟尿嘧啶乙酸、5-氟尿嘧啶丙酸与Cu(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Zn(Ⅱ)、Mn(Ⅱ)的配合物的合成及表征

合成了N(1)取代5-氟尿嘧啶乙酸、5-氟尿嘧啶丙酸与铜(Ⅱ)、钴(Ⅱ)、镍(Ⅱ)和锰(Ⅱ)的十种金属配合物。通过元素分析、差热-热重分析确定了它们的化学组成,并对这些化合物进行了红外光谱、氢核磁共振谱,电子光谱的表征。讨论了各配合物中金属离子与配体的配位状态。在Cu(Ⅱ)配合物中,Cu(Ⅱ)是与配体的N³原子和C⁴上的羰基氧原子配位,其他金属配合物中,金属离子是与配体的C²的羰基氧原子和羧基配位。     

氮杂冠醚及其Cu(Ⅱ)、Ni(Ⅱ)、Cd(Ⅱ)、Ag(Ⅰ)配合物的合成及性质研究

用直接合成法合成了一种新配体-1,7-N,N′-二(邻氨基苯基)-1,7-二氮杂-4,10-二氧杂环十二烷[L]。经元素分析~1H、~(13)C核磁共振、质谱、红外光谱等分析证实了其结构。并藉该配体合成了Cu(Ⅱ),Cd(Ⅱ),Ag(Ⅰ),Ni(Ⅱ)四种固体配合物。经元素分析配合物的组成分别为:[CuCl_2]_2·L,[CdCl_2]_2·2L·2H_2O_2[AgNO_3]_2·L,[NiCl_2]_2·L·H_2O.对配合物进行了红外光谱、紫外光谱、摩尔电导和差热分析。配合物的红外特征吸收峰均有明显位移或分裂;紫外特征吸收峰稍有位移。但摩尔吸光系数改变很大;摩尔电导表明配合物为1:1或接近2:1型电解质;差热分析表明配合物的热稳定性顺序为:Cd(Ⅱ)、Ni(Ⅱ)>Cu(Ⅱ)>Ag(Ⅰ)。对Cu(Ⅱ)配合物进行了ESR谱分析,并且对甲醇溶液中Cu(Ⅱ)与配体(L)的掺入反应动力学进行了初步研究,结果表明,掺入反应为典型的二级反应。     

吡啶-3-甲醛缩氨基硫脲合镍(Ⅱ)、锌(Ⅱ)配合物的合成、晶结构及生物活性

本文合成并表征了吡啶-3-甲醛缩氨基硫脲(HL)合镍(Ⅱ)、锌(Ⅱ)配合物.在配合物[NiL2(1)中,镍(Ⅱ)离子与来自2个脱氢配体的2个氮原子和2个硫原子配位.形成四配位的平面正方形构型.在配合物[Zn(HL)2(C2H5OH)2(H2O)2](NO3)2(2)中,锌(Ⅱ)离子与2个中性配体、2个乙醇分子和2个水分子配位,配位原子在锌(Ⅱ)离子周围形成畸变的八面体构型.通过荧光吸收法研究了配合物1、2与小牛胸腺DNA的作用机理.结果表明,这2个配合物均以插入形式进入DNA的碱基对.此外,还研究了配体及2个配合物对金黄色葡萄球菌、乙型溶血性链球菌、肺炎链球菌、炭疽杆菌的抗菌活性.结果表明,配体及配合物1对上述测试菌种无抑制作用.配合物2对前面3种有弱的抑菌作用.     

芳香胺氮氧化物合贵金属配合物的研究——Ⅰ.2,2''-联喹啉—N,N''-二氧化物和金(Ⅲ)、铂(Ⅳ)及钯(Ⅱ)配合物的合成与表征

合成了金(Ⅲ)、铂(Ⅳ)和钯(Ⅱ)与标题化合物形成的五种新配合物,研究了它们的组成与有关性质、可分为含氢键的离子缔合物和含金属一氧键的混配螯合物两类.     

芳香胺氮氧化物合贵金属配合物的研究——Ⅰ.2,2''-联喹啉—N,N''-二氧化物和金(Ⅲ)、铂(Ⅳ)及钯(Ⅱ)配合物的合成与表征

合成了金(Ⅲ)、铂(Ⅳ)和钯(Ⅱ)与标题化合物形成的五种新配合物,研究了它们的组成与有关性质、可分为含氢键的离子缔合物和含金属一氧键的混配螯合物两类.     

大环二羰四胺Ni(Ⅱ)单核和Ni(Ⅱ)-Cu(Ⅱ)双核配合物的合成、表征及电化学性质

合成了一种草酰胺桥联大环二羰四胺Ni(Ⅱ )单核配合物 ,并以此为母体合成了Ni (Ⅱ ) -Cu (Ⅱ )双核配合物 .用元素分析、红外光谱、差热分析、紫外光谱、摩尔电导以及循环伏安等测试手段对配合物进行了表征和电化学性质研究 .经分析 ,标题配合物具有草酰胺桥联结构 ,Ni(Ⅱ )处于平面正方场 ,Cu (Ⅱ )处于八面体场中 .循环伏安测试表明此类配合物能稳定Ni(Ⅲ ) .     

Synthesis, investigation and spectroscopic characterization of piroxicam ternary complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with glycine and DL-phenylalanine

The ternary piroxicam (Pir; 4-hydroxy-2-methyl-N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with various amino acids (AA) such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized by elemental analyses, molar conductance, IR, UV-Vis, magnetic moment, diffuse reflectance and X-ray powder diffraction. The UV-Vis spectra of Pir and the effect of metal chelation on the different interligand transitions are discussed in detailed manner. IR and UV-Vis spectra confirm that Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its carboxylic group, in addition PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its carboxylic and amino groups. All the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. The molar conductance data reveal that most of these chelates are non electrolytes, while Fe(III)-Pir-Gly, Co(II)-, Ni(II)-, Cu(II)- and Zn(II)-Pir-PhA chelates were 1:1 electrolytes. X-ray powder diffraction is used as a new tool to estimate the crystallinity of chelates as well as to elucidate their geometrical structures.     

Studies on oxovanadium(IV), Cr(III), Co(II), Ni(II), and Cu(II) chelates of some bisketimino ligands

The oxovanadium(IV), Cr(III), Ni(II), Co(II), and Cu(II) chelates of some bisketimino Schiff-base ligands (H₂L) obtained by condensation of 4-butyryl-3-methyl-1-phenyl-(or-1,3-diphenyl)-2-pyrazolin-5-ones with thiourea were synthesized and characterized by elemental analyses and thermogravimetric analyses, molar conductivities, magnetic susceptibility measurements, mass, infrared, and electronic spectroscopies. Ligand field parameters, such as splitting energy, Racah parameter, spin–orbit coupling constant, and covalency parameter of the Cr(III), Ni(II), and Co(II) chelates were calculated by band-fitting methods. Based on these studies, tetragonally distorted octahedral environment around OV(IV) and Cu(II) and octahedral Cr(III), Ni(II), and Co(II) have been proposed.     

Transition metal polymeric chelates: Spectral, magnetic, thermal behaviour of polymeric chelates of poly(resacetophenone diyl ethylene)s with Ni(II), Cu(II), Mn(II), Zn(II) and Co(II)

Polymeric chelates of the type [ML₂]_n where M = Ni(II), Cu(II), Zn(II) or Co(II), L = poly(resacetophenone diyl ethylene)s, andn= degree of polymerization, have been synthesized. Their structures have been elucidated on the basis of analytical, magnetic, electronic and IR spectral studies. Electronic spectra in conjunction with magnetic moments are in accord with an octahedral environment around the central metal ion in all polymeric chelates except Cu(II) and Zn(II) polymeric chelates which have been shown to possess square planar and tetrahedral geometries, respectively. IR spectral studies further suggest that the metal ions are coordinated through the oxygens of the carbonyl and the phenolic hydroxyl groups. All the chelates are paramagnetic except Zn(II), which is found to be diamagnetic.     

Studies of Mn(II), Co(II), Ni(II) and Cu(II) Chelates with 3-phenyl-4-(p-methoxy- phenylazo)-5-pyrazolone

Mn(II), Co(II), Ni(II) and Cu(II) chelates with3-phenyl-4-(p-methoxyphenylazo)-5-pyrazolone have been synthesized and were characterized by elemental and thermal analyses as well as by IR, UV-VIS, ¹HNMR, conductometric and magnetic measurements. The first stage in the thermal decomposition process of these complexes shows the presence of water of hydration, the second denotes the removal of the coordinated water molecules. The final decomposition products were found to be the respective metal oxides. The data of the investigated complexes suggest octahedral geometry with respect to Co(II) 1:1, tetrahedral for Ni(II) 1:1and 2:3; square planar for Cu(II) 1:1 and 2:3; the complexes with no coordinated water molecules (2:3) Co(II) and Mn(II) complexes are tetrahedral. This revised version was published online in August 2006 with corrections to the Cover Date.     

Synthetic,spectroscopic, fluorescence,and biological investigation of Co(II), Ni(II), Cu(II), and Zn(II) complexes of Schiff bases derived from 3-formyl-2-mercaptoquinolines (Quinol-2-thiones)

Co(II), Ni(II), Cu(II), and Zn(II) complexes have been prepared with Schiff bases derived from 3-formyl-2-mercaptoquinoline and substituted anilines. The prepared Schiff bases and chelates have been characterized by elemental analysis, molar conductance, magnetic susceptibilities, electronic, IR, ¹H-NMR, ESR, cyclic voltammetry, FAB-mass, and thermal studies. The complexes have stoichiometry of the type ML₂ · 2H₂O coordinating through azomethine nitrogen and thiolate sulfur of 2-mercapto quinoline. An enhancement in fluorescence has been noticed in the Zn(II) complexes whereas quenching occurred in the other complexes. The ligands and their metal complexes have been screened in vitro for antibacterial and antifungal activities by MIC methods with biological activity increasing on complexation. Cu(II) complexes show greater bacterial than fungicidal activities. The brine shrimp bioassay was also carried out to study the in vitro cytotoxicity properties of the ligands and their corresponding complexes. Only four compounds have exhibited potent cytotoxic activity against Artemia salina; the other compounds were almost inactive for this assay.     

Synthesis, spectral characterization, solution equilibria, in vitro antibacterial and cytotoxic activities of Cu(II), Ni(II), Mn(II), Co(II) and Zn(II) complexes with Schiff base derived from 5-bromosalicylaldehyde and 2-aminomethylthiophene

Schiff base namely 2-aminomethylthiophenyl-4-bromosalicylaldehyde (ATS)(4-bromo-2-(thiophen-2-yl-imino)methylphenol) and its metal complexes have been synthesized and characterized by elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance, mass spectra, ESR and thermal analysis (TGA). The analytical data of the complexes show the formation of 1:2 [M:L] ratio of the formula [ML2], where M represents Ni(II), Zn(II) and Cu(II) ions, while L represents the deprotonated Schiff base. IR spectra show that ATS is coordinated to the metal ions in a bidentate manner through azomethine-N and phenolic-oxygen groups. The ligand and their metal chelates have been screened for their antimicrobial activities using the disc diffusion method against the selected bacteria. A cytotoxicity of the compounds against colon (HCT116) and larynx (HEP2) cancer cells have been studied. Protonation constants of (ATS) ligand and stability constants of its Cu2+, Co2+, Mn2+, Zn2+ and Ni2+ complexes were determined by potentiometric titration method in 50% (v/v) DMSO-water solution at ionic strength of 0.1 M NaNO3.     

Synthesis,characterization and antibacterial properties of symmetric 1,1′‐ferrocene derived Schiff‐base ligands and their Co(II), Cu(II), Ni(II) and Zn(II) chelates

Symmetric 1,1′‐dimethylferrocene derived Schiff‐base ligands have been prepared by the condensation reaction of 1,1′‐diacetylferrocene with 2‐aminopyrazine, 2‐aminopyridine and 2‐aminothiazole respectively. Their transition metal chelates, of the type [M(L)]Cl₂ [M = Cu(II)] and [M(L)(Cl₂)] [M = Co(II), Ni(II) and Zn(II)] have been prepared. The synthesized Schiff‐base ligands and their metal(II) chelates have been characterized by their physical, analytical and spectral data. Copyright © 2000 John Wiley & Sons, Ltd.     

Poly(crotonic acid-co-2-acrylamido-2-methyl-1-propanesulfonic acid)-metal complexes with copper(II), cobalt(II), and nickel(II): Synthesis, characterization and antimicrobial activity

Poly(crotonic acid-co-2-acrylamido-2-methyl-1-propanesulfonic acid) [P(CrA-co-AMPS)] (44.22:55.78) copolymer was prepared in N,N-dimethylformamide solution using the benzoyl peroxide (Bz₂O₂) as initiator. Cu(II), Ni(II) and Co(II) chelates of the copolymer were prepared and the formation constants of each complex were determined by the mole-ratio method using UV-vis spectroscopy. UV-vis studies showed that the complex formation tendency increased in the followed order: Cu(II) > Ni(II) > Co(II). The copolymer and its metal chelates were characterized by FTIR, TGA, X-ray diffraction and SEM analysis. Also, in vitro antimicrobial activity of the polymers were tested on various bacteria, and yeast.     

Chelation behaviour of nitroso- pyrazolones with Mn(II), Co(II), Ni(II), Cu(II) AND Zn(II)

Infrared (IR), nuclear magnetic resonance (NMR), thermogravimetric analysis (TG), derivative thermogravimetric analysis (DTG), differential thermal analysis (DTA) and molar conductivity studies have been carried out on the chelates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) with 3-methyl- and 3-phenyl-4-nitroso-5-pyrazolones. The solid chelates were synthesized, separated, analyzed and their structures were elucidated. The data obtained show that almost all of the prepared chelates contain water molecules in their coordination sphere. The initial stage in the thermal decomposition process of these chelates shows the presence of water molecule, the second denotes to the intermediate products. The final decomposition products were found to be the respective metal oxides. The NMR spectrum of 3-methyl-4-nitroso-5-pyrazolone ligand shows the existence of the oxime rather than the nitroso form. 3-phenyl-4-nitroso-5-pyrazolone acts as a neutral bidentate ligand whereas 3-methyl-4-nitroso-5-pyrazolone acts as monobasic bidentate ligand bonded to the metal ions through the two oxygen atoms of the carbonyl and nitroso groups. The solid chelates prepared behave as non-electrolytes in DMF solution. The coordination numbers of the obtained chelates using 3-methyl-4-nitroso-5-pyrazolone are four on applying the mole ratio 1:1 and six on using 1:2 mole ratio. In case of using the ligand 3-phenyl-4-nitroso-5-pyrazolone the coordination number is six in both cases. This revised version was published online in August 2006 with corrections to the Cover Date.     

Reversed-phase HPLC determination of Co(II), Ni(II) and Fe(III) as their 2-(2-thiazolylazo)-5-dimethylaminophenol chelates

The optimum chromatographic separation conditions for Co(II), Ni(II), and Fe(III) chelates with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM) were investigated. The compositions of chelates were also determined by the HPLC method and thus the possible structure of chelates was given. A precolumn derivatization method was used, followed by separation on an octyl-bonded silica stationary phase with a methanol-tetrahydrofuran-water (40:9:51, v/v/v) mobile phase containing pH 5.8 acetate buffer and 1 x 10(-4)M TAM. The detection limits of Co(II), Ni(II), and Fe(III) at 560 nm are 0.03, 0.02 and 0.1 ng (S N = 2 ), respectively. They can be determined by means of the proposed method without interference from other common metal ions and have been determined in five standard alloys with satisfactory results.