邻香兰素对甲苯胺Schiff碱稀土配合物的制备和表征

前文曾报道了香兰素(3-甲氧基-4-羟基苯甲醛)与对甲基苯胺的Schiff碱稀土配合物。本文讨论邻香兰素(2-羟基-3-甲氧基苯甲醛)与对甲基苯胺的Schiff碱稀土配合物[LnL_2Cl·2H_2O]Cl_2(Ln:ce,Pr,Nd,Sm,Eu,Gd,Dy;L:Schiff碱)的制备和表征。 1 实验 1.1 配合物的制备 按文献方法,用等摩尔比的邻香兰素与对甲基苯胺在无水乙醇中先制成Schiff碱,然后按摩尔比1:2将稀土氯化物LnCl_3·nH_2O的无水乙醇溶液滴加到     

Electrochemical Synthesis and Characterization of Tin(IV) Complexes of Dianionic Terdentate Schiff Base Ligands

Tin(IV) complexes of the series of dianionic terdentate Schiff bases N‐[(2‐pyrroyl)methylidene]‐N′‐tosylbenzene‐1,2‐diamine, (H₂L¹), N‐[(2‐hydroxyphenyl)methylidene]‐N′‐tosylbenzene‐1,2‐diamine (H₂L²) and some R substituted 2‐{[(2‐hydroxyphenyl)imino]methyl}phenols [R = H (H₂L³), 4,6‐(OCH₃)₂ (H₂L⁴), 3‐(OC₂H₅) (H₂L⁵) and 3,5‐Br₂ (H₂L⁶)] have been synthesized. The compounds were obtained by the electrochemical oxidation of a tin anode in a cell containing an acetonitrile solution of the corresponding ligand. The complex [SnL¹₂] was also obtained by reaction of SnCl₂·2H₂O and H₂L¹ in methanol in the presence of triethylamine. The crystal structure of the ligand [H₂L⁶] and the complexes [SnL¹₂] (1) , [SnL²₂] (2) , [SnL³₂] (3) and [SnL⁶₂] (6) were determined by X‐ray diffraction. In the complexes, the tin atom is in an octahedral environment coordinated by two dianionic terdentate ligands. Spectroscopic data for the complexes (IR, ¹H and ¹¹⁹Sn NMR and mass spectra) are discussed and related to structural information.     

Synthesis,Characterization and Antimicrobial Activity of Oxovanadium(IV) Complexes of Schiff Base Hydrazones Containing Quinoxaline Moiety

The oxovanadium(IV) complexes of the Schiff base hydrazones, synthesized from 3‐hydrazinoquinoxaline‐2‐one (HQO) with salicylaldehyde (HSHQO), o‐hydroxyacetophenone (HHAHQO), dehydroacetic acid (HDHAHQO) and o‐nitrobenzaldehyde (NBHQO) were synthesized and characterized on the basis of analytical, conductance, magnetic moment, infrared, NMR, ESR and electronic spectral data. The ligands HSHQO, HDHAHQO behaved as monobasic tridentate ONN donors through phenolic oxygen, azomethine nitrogens. The ligand HAHQO acted as a monobasic bidentate ON donor through the phenolic oxygen, azomethine (free) nitrogen and the ligand NBHQO acted as neutral bidentate ON donor through oxygen of the nitro group and azomethine (free) nitrogen.     

酪氨酸希夫碱邻菲咯啉氧钒配合物的合成、结构及其与DNA相互作用研究

合成了一个新的L-酪氨酸萘酚醛希夫碱及邻菲咯啉混配氧钒配合物[VO(Naph-L-Tyr)(Phen)]•CH₃OH (Naph-L-Tyr＝2-羟基-1-萘甲醛与L-酪氨酸形成的希夫碱, Phen＝1,10-邻菲咯啉). 利用元素分析、红外光谱和X射线单晶衍射进行了表征. 晶体结构测定表明, 该晶体属于三斜晶系, P-1空间群, 其晶体学数据: a＝1.00023(11) nm, b＝1.13478(12) nm, c＝1.34076(15) nm, a＝108.118(2)o, b＝96.3920(10)o, g＝92.4010(10)o, V＝1.4326(3) nm³, Z＝2, D_c＝1.420 g/cm³, F(000)＝634, 最终的偏差因子为R₁＝0.0670, wR₂＝0.1324 [I＞2s (I)]. 以钒原子为中心形成了六配位变形的八面体构型, 晶体中相邻分子之间通过氢键和π-π相互作用形成一维链状结构. 利用紫外吸收光谱、荧光光谱、圆二色光谱和粘度测量等研究了配合物与小牛胸腺DNA (CT-DNA)的作用, 结果表明配合物以插入方式与CT-DNA作用. 琼脂糖凝胶电泳法研究表明, 配合物对质粒pBR322 DNA分子具有切割作用.     

The Synthesis and Spectroscopic Characterization of Heterobimetallic Bu2Sn(IV) Complexes Derived from Some Chelating Ligands

The interaction of Bu₂Sn(OPrⁱ)₂ with a trifunctional tetradentate Schiff base (LH₃) (where H₃L = HOC₆H₄CH═NCH₃C(CH₂OH)₂) yields the precursor complex Bu₂Sn(LH) 1, which, on equimolar reactions with different metal alkoxides [Al(OPrⁱ)₃, Bu₃Sn(OPrⁱ), Ge(OEt)₄]; Al(Medea)(OPrⁱ) (where Medea = CH₃N- (CH₂CH₂O)₂); and Me₃SiCl in the presence of Et₃N], affords, respectively, the complexes Bu₂Sn(L)Al(OPrⁱ)₂ 2, Bu₂Sn(L)Al(Medea) 3, Bu₂Sn(L)Bu₃Sn 4, Bu₂Sn(L)Ge(OEt)₃ 5, and Bu₂Sn(L)SiMe₃ 6. The reactions of 2 with 2,5-dimethyl-2,5-hexanediol in a 1:1 ratio and with acetylacetone (acacH) in a 1:2 molar ratio afforded derivatives Bu₂Sn(L)Al(OC(CH₃)₂CH₂CH₂C(CH₃)₂ O) 7 and Bu₂Sn(L)Al(acac)₂ 8, respectively. All of the derivatives 1– 8 have been characterized by elemental analyses, molecular weight measurements, and spectroscopic [IR and NMR (¹H, ¹¹⁹Sn, ²⁹Si, and ²⁷Al)] studies.     

Syntheses and Crystal Structures of Two VO(IV) Schiff Base Complexes with Oxyammonia Ligand

1 INTRODUCTION The insulin-mimetic property of vanadium complexes is the most noteworthy finding and the relationship between vanadium and diabetes mellitus has been extensively studied in the past decades[1～5]. Vanadium complexes are capable of increa…     

Copper(II) Complexes with Asymmetrical Schiff Base Ligands Derived from 2‐Acetylpyrazine

New copper(II) complexes of asymmetrical tetradentate Schiff bases containing pyrazine have been prepared and thoroughly characterised by elemental analysis, IR and electronic spectroscopy, mass spectrometry and magnetic measurements. Two alternative methods were used in the isolation of the complexes: template synthesis in the preparation of Cu(SalDpyz)ClO₄ (HSalDPyz = derived from the condensation of salicylaldehyde, acetylpyrazine and 1,2‐ethylendiamine, 2‐methyl‐1,2‐propylendiamine, 1,2‐phenylendiamine) and direct interaction between copper perchlorate and the corresponding Schiff base, as in the isolation of Cu(AEPyz)(ClO₄) (HAEPyz = (Z)‐4‐[2‐{[2‐{[(E)‐1‐(pyrazinyl)ethylidene]amino} ethyl)amino]‐3‐penten‐2‐one)]. [Cu(SalEn)(py)(OClO₃)][Cu(SalEn)(py)]ClO₄ ( 1 ) (SalEn = 4‐(2‐hydroxyphenyl)‐3‐aza‐3‐buten‐1‐amino, py = pyridine), metal precursor in the preparation of Cu(SalEnpyz)(ClO₄) (HSalEnpyz = 2‐{E(2‐{[(E)‐1‐(2‐pyrazinyl)ethylidene]amino}ethyl)imino]methyl}phenol), was crystallographically characterised. The crystal structure of [Cu(AEpyz)]ClO₄ ( 2 ) is also reported.     

异烟酰肼缩水杨醛Schiff碱配合物的合成与表征

采用直接合成法用异烟酰肼、水杨醛合成了异烟酰肼缩水杨醛Schiff碱,并以此为配体合成了Zn（Ⅱ）、Co（Ⅲ）、Ni（Ⅱ）的配合物．对配合物进行了元素分析,红外光谱,紫外光谱,差热-热重分析及摩尔电导的测试等表征,推测配合物的组成分别为[Zn（H2O）L],[Co（H2O）2（HL）2]NO3-H2O,[Ni（H2O）2HL]NO3,其中L=C13 H9O2N3．     

噻吩醛缩乙二胺席夫碱及其配合物的合成与光催化性能

基于TiO₂光催化性能的染料敏化改性,采用2-噻吩甲醛缩合乙二胺合成了席夫碱配体L,并与金属配合得到了金属配合物[ZnLCl₂](1),[NiL'(NO₃)₂](2)(L'为单噻吩醛缩乙二胺),对配体L、配合物1 和2进行了X射线单晶衍射结构分析。 用合成的配体和配合物修饰TiO₂得到相应的复合光催化剂L-TiO₂、1-TiO₂和2-TiO₂,并进行了红外光谱、紫外-可见漫反射光谱、粉末X射线衍射图谱等表征,研究了这3种光催化剂降解水中有机污染物4-硝基酚(4-NP)和罗丹明B(RhB)的催化活性。 结果表明,1-TiO₂、2-TiO₂可以有效的降解4-NP和RhB,降解率可达90%以上。     

混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱配合物的合成和表征

由混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱反应,合成了24种新的有机锡配合物。经元素分析、NMR、TG-DSC测定和X射线粉末衍射分析,确定有14种是有机锡与Schiff碱的1:1配合物,10种是1:2配合物。配体是以酚羟基氧原子与锡原子配位,摩尔电导率测定表明这些配合物均为非电解质。     

金刚烷胺邻香兰素Schiff碱过渡金属配合物的合成与表征

合成了金刚烷胺邻香兰素Sch iff碱配体(C18H23NO2,以L表示)与过渡金属的6种新的配合物[MC l2L](M=Mn(Ⅱ),Co(Ⅱ),N i(Ⅱ),Cu(Ⅱ),Zn(Ⅱ),Cd(Ⅱ)),用元素分析、摩尔电导、红外光谱和热重分析表征了配合物的结构;讨论了配体与中心金属离子的键合情况并推测了配合物的结构,每一中心金属离子与Sch iff碱配体中的酚羟基氧、甲氧基氧及2个氯离子发生配位,其配位数为4.     

Nontoxic Cobalt(III) Schiff Base Complexes with Broad-Spectrum Antifungal Activity

Resistance to currently available antifungal drugs has quietly been on the rise but overshadowed by the alarming spread of antibacterial resistance. There is a striking lack of attention to the threat of drug-resistant fungal infections, with only a handful of new drugs currently in development. Given that metal complexes have proven to be useful new chemotypes in the fight against diseases such as cancer, malaria, and bacterial infections, it is reasonable to explore their possible utility in treating fungal infections. Herein we report a series of cobalt(III) Schiff base complexes with broad-spectrum antifungal activity. Some of these complexes show minimum inhibitory concentrations (MIC) in the low micro- to nanomolar range against a series of Candida and Cryptococcus yeasts. Additionally, we demonstrate that these compounds show no cytotoxicity against both bacterial and human cells. Finally, we report the first in vivo toxicity data on these compounds in Galleria mellonella, showing that doses as high as 266 mg kg⁻¹ are tolerated without adverse effects, paving the way for further in vivo studies of these complexes.     

席夫碱及其络合物的可逆热致变色材料

对具有可逆的热致变色的席夫碱及其络合物的分类、合成、变色机理以及发展前景等进行了回顾和探讨。     

Pendant-Arm Macrocycles Derived from the Cyclocondensation Reaction of Sodium 2,6-Diformyl-4-substitutedphenolates and Tris-(2-aminoethyl)amine Derivatives. Preparation, Characterization and Properties of their Dinuclear Copper(II) Complexes

A series of pendant-arm Schiff base macrocycles have been obtained via the cyclocondensation reaction between sodium 2,6-diformyl-4-substitutedphenolates and tris-(2-aminoethyl)- amine derivatives followed by transmetallation with Cu(ClO₄)₂·6H₂O. The resulting dinuclear copper(II) complexes have been characterized by elemental analysis, infrared and mass spectra as well as magnetic moments at room temperature. All complexes have been electrochemically investigated, and two typical compounds have been studied with ESR spectra as well.     

3-醛基水杨酸-1,3-丙二胺Schiff碱过渡金属异双核配合物的合成及表征

3-醛基水杨酸与二胺类形成的Schiff碱是有效的双核配体,其配合物的合成和表征已有一些报道,但二胺为1,3-丙二胺的Schiff碱与过渡金属形成的异双核配合物的研究至今未见报道。我们用二(3-羧基水杨醛叉)缩丙撑二胺与过渡金属合成了一些异双核配合物,并用元素分析、IR、UV-Vis,室温磁矩及氧化还原半波电位对配合物的组成和结构进行了表征。     

新型双核席夫碱配合物的合成及谱学性质

Eight novel binuclear tetradentate Schiff base complexes (M=Cu(Ⅱ),Ni(Ⅱ),Zn(Ⅱ)) are synthesized. The structure of complexes is two discrete Schiff base unit bridged. The complexes were condensed from series sub-stituent Ketones (5-chloro-2-hydroxybenzophenone, 5-methyl-2-hydroxy-benzophenone, 5-Bromo-2-hydroxybenzop- henone) and dialdehydes (5,5′-methylene-disalicylaldehyde) with the amino group of 1,2-diaminobenzene, and by Metal ion as template. The compounds were characterized by elemental analyses, FT-infrared spectra, Raman, ¹H NMR, UV-vis electronic spectra, EPR spectra. The FT-infrared spectra and Raman spectra of complexes were compared and discussed. The UV-vis election spectra, ¹H NMR and EPR spectra of complexes have also been attributed and minutely analyzed.     

Synthesis,Characterization, and Antibacterial Studies of Oxovanadium(IV) Complexes with Thiazole-Derived Schiff Bases

Oxovanadium(IV) complexes of Schiff bases, derived from 2-amino-4-phenyl thiazole/substituted 2-amino-4-phenyl thiazoles and thiophene-2-aldehyde have been synthesized and characterized on the basis of elemental analysis, molar conductance measurements, magnetic susceptibility data, and UV-visible, and IR spectral studies. All the complexes are monomeric possessing a 1:2 (metal:ligand) stoichiometry. On the basis of these data, a square pyramidal geometry has been assigned for the complexes. A few complexes have been subjected to thermal decomposition studies. The ligands and their metal complexes have been screened for their antibacterial activities.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

源自天然席夫碱的过渡金属配合物在分光光度法测天然水中的Fe(Ⅲ)的应用

描述了一种新颖、简便的合成含五齿配位基的大环席夫碱配体的方法,制备和表征了该席夫碱的1∶1包合物。用化学和光谱学方法测定了标题配合物的组成,认为在所有配合物中配位金属原子取八面体结构。数据表明:配体起O2N4六齿结构而每个环绕金属原子在八面体环境中。配合物的红外和1H NMR光谱符合中心金属原子的配位结果。用分光光度法测定了配合物的稳定常数。用共轭余量法(CR method)计算了在热分解的不同阶段配合物活化的动力学和热力学参数。此外,用抑菌圈直径法筛选了配体及其金属配合物抑制细菌和真菌的能力。用回收率试验研究了天然螯合配体在不同天然水体中对Fe(Ⅲ)离子配合作用的影响。     

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．     

Synthesis and Characterization of Polynuclear Metal Complexes with Bridging Ketoiminato and Thioiminato Schiff Base Ligands

Bimetallic and trimetallic complexes of stoichiometry [M(acacen)M′Y₂], [M(sacacen)M′Y₂], and {[M(acacen)]₂M′Y₂} have been prepared by reaction of the appropriate square-planar Schiff base metal complex with various secondary metal salts in toluene and/or absolute ethanol. Systems which are reported here include those where M = Cu(II); M′ = Cu(II), Ni(II), Co(II), Mn(lI) and Zn(II); Y^? = Cl^?, Br^?, and NO₃ ^?. Trinuclear complexes have been isolated only for {[Cu(acacen)]₂M′(NO₃)₂} where M′ = Cu(lI) or Mn(II); binuclear complexes result from all other combinations. The geometry of the chelated Cu(II) ion is square-planar in the bimetallic complexes and possibly square-pyramidal in the trimetallic compounds, while that of the secondary metal ion depends on the coordination preference of M′, the nature of Y^? and whether the bridging donor atoms are oxygen or sulfur. Probable structures of the new polynuclear complexes have been deduced from spectral, conductivity and magnetic measurements.