SYNTHESIS AND CHARACTERIZATION OF METAL COMPLEXES WITH AMPICILLIN

Abstract

The reaction, in water, of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) ions with sodium ampicillinate at room temperature has allowed isolation of dimers with the following general formula [M(amp)Cl]₂ × nH₂O (n = 1.5?3.2). The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibilities and spectroscopic methods (IR, Raman, EPR and UV-Visible). A dinuclear structure based on octahedrally coordinated metal ions is proposed.     

SYNTHESIS,CHARACTERIZATION AND STRUCTURAL ANALYSES OF THREE LANTHANIDE CYANIDE-BRIDGED COMPLEXES

Abstract

Three lanthanide (Ln) complexes (DMF)₄(H₂O)₃LnFe(CN)₆ · H₂O, where Ln = Er, Yb, and Lu, were structurally determined by means of three-dimensional single-crystal X-ray diffraction analysis. These systems crystallize in the centrosymmetric monoclinic space group P2₁/c (No. 14) with Z = 4 and respective lattice constants of a = 13.956(2), 13.952(1), 13.937(3); b = 8.867(4), 8.864(1), 8.862(2); c = 24.857(3), 24.812(2), 24.770(5) Å; and β = 96.30(1)°, 96.33(1)°, 96.30(3)°. Final least-squares full-matrix refinements based on 3499, 3367, and 2555 unique reflections yielded reliability (R) index factors of 0.071, 0.051, and 0.032, respectively. In each complex, the coordination about the central Ln ion is eight in a square-antiprism arrangement and the coordination about the Fe ions is six, oriented octahedrally. Cyanide bridging links the Ln ions to the FeC₆ groups. Molecules in the crystal lattice of each complex are held together by van der Waals forces and a network of hydrogen bonding. Characterization includes physical property determinations, conoscopical studies, thermal gravimetric analyses, and IR spectrometric identifications. Selected bond lengths and angles are tabularized and a synthesis of these compounds is presented.     

二(1,3-二硫杂环戊烯-2-硫酮-4,5-二巯基)镉-季铵类配合物的合成与表征

二（１，３－二硫杂环戊烯－２－硫酮－４，５－二巯基）镉－季铵类配合物的合成与表征李洪启宋燕西＊周宏英王爱勤姚钟麒俞贤达（中国科学院兰州化学物理研究所，兰州７３００００；＊兰州大学化学系，兰州７３００００）关键词二（１，３－二硫杂环戊烯－２－硫酮－４，...     

SYNTHESIS AND CHARACTERIZATION OF TRIS(ALKYLISOCYANIDE) BIS(TRIARYL-PHOSPHINE)COBALT(II) COMPLEXES

Abstract

A series of complexes having the general formula, [Co(CNR)₃(PR₃)₂]X₂, X = ClO₄, BF₄ with CNR = CNCMe₃, CNCHMe₂, CNC₆H₁₁. CNCH₂Ph and PR₃ = PPh₃, P(C₆H₄Me-p)₃, P(C₆H₄OMe-p)₃ has been synthesized and characterized. Synthesis can be achieved by reaction of [Co(CNR)₄(AsPh₃)₂]X₂ complexes with controlled excess of PR₃ ligands, and by AgClO₄/AgBF₄ oxidation of the [Co(CNR)₃(PR₃)₂]X complexes. The latter procedure is preferable. Alternate syntheses of the [Co(CNR)₃(PR₃)₂]X complexes have also been employed. Five-coordinate Co(II) complexes have not been obtained using CNCMe₃ with P(C₆H₄Me-p)₃ ligands, CNCH₂Ph with P(C₆H₄OMe-p)₃ ligands, or CNC₄H_9-n with PPh₃ ligands. [Co(CNC-Me₃)₃{P(C₆H₄Cl-p)₃}₂]ClO₄ produced only [Co{CNCMe₃)₄H₂O](ClO₄)₂ upon forced oxidation with excess AgClO₄. [Co(CNR)₃(PR₃)₂]X₂ complexes appear to undergo varying degrees of distortion from regular (i.e., D _3h symmetry) axially-disubstituted trigonal bipyramidal coordination in the solid state, as evidenced by v(-N°C) IR patterns, but to assume regular trigonal bipyramidal coordination in solution. Effective magnetic moments indicate one-electron paramagnetism, and solution electronic spectra are compatible with trigonal bipyramidal coordination.     

镧系金属杂—2,3,4,5—四苯基环戊二烯环状化合物的合成及其表征

二苯乙炔和金属锂在乙醚中反应得到1,4-二锂四苯基丁二烯,再与无水氧化希土反应得到了两种系金属条-2,3,4,5-四苯基环戊二烯环状化合物。通过元素分析、红外光谱、核磁共振谱、热失重及电子能谱的分析,对所合成的化合物进行了表征;并对化合物的水解产物作了红外光谱、质谱和核磁共振谱分析,确认下列两种化合物的存在:     

SYNTHESIS AND CHARACTERIZATION OF POLYMER DERIVATIVES OF cis-PLATINUM COMPLEXES

Cis-platinum complexes used as antitumor drugs were attached onto preformed polymers toreduce the toxicity. Either alternating copolymer of styrene and maleic anhydride (CPSMA) orpolyacrylic acid (PAA) is readily dissolved in alkaline solution. The cis-platinum complexes areeasily converted into water soluble species when treated by silver nitrate in water. The expectedproducts could be obtained when the two aqueous solutions were brought together. The productswere characterized by elementary analysis, IR and XPS.The polymer derivatives could exchange Jigands with nucleophilic groups in biological environment and also exhibit antineoplastic activity.     

SYNTHESIS AND CHARACTERIZATION OF Fe(III), Co(III), Cu(II) AND Zn(II) COMPLEXES OF N-2,4-HYDROXYBENZAL-D-GLUCOSAMINE

Abstract

The Schiff base N-2,4-dihydroxybenzal-D-glucosamine (L), and its Fe(III), Co(III), Cu(II) and Zn(II) complexes have been synthesized and characterized. Magnetic moments suggest that all complexes are high-spin. The Cu(II) chelate in DMF solution has a distorted tetrahedral structure, as shown by ESR and electronic spectra. Detailed studies have been made concerning the solution equilibrium of L with transition metal ions. Stabilities of the complexes are in accord with the Irving-Williams series.     

8-羟基喹啉-邻菲罗啉-稀土三元固体配合物的合成和表征

近年来 ,稀土三元配合物的种类和数目增加很快 ,有关具有特殊性质和结构的稀土三元配合物的合成报道日益增多 ,这些研究促进了稀土配位化学的发展。稀土含氮杂环化合物的合成、结构、荧光性质的研究很多 ,其中以Ｐｈｅｎ的稀土配合物研究占有较大的比例。我们知道 ,稀土离子与氮的亲和力小于与氧的亲和力 ,因此在水溶液中 ,作为弱碱性的氮给予体 ,即有机含氮杂环配体难与水竞争而取代水 ,故难以得到稀土含氮杂环化合物。直到二十世纪六十年代 ,人们利用非水溶剂为介质 ,合成了稀土与Ｐｈｅｎ的配合物[1 ] 。由于Ｐｈｅｎ含有较大范围的的共…     

SYNTHESIS AND CHARACTERIZATION OF DVE-CO-MA DERIVATIVES OF CIS- PLATINUM COMPLEXES

<正> Copolymer of divinyl ether and maleic anhydride （DVE-co-MA） derivatives of cis-platinum complexes were synthesized and characterized by elementary analysis, IR and XPS （ X-ray photoelectron spectroscopy）. The behavior of the products in biological environment was also studied. UV-visible and fluorescence spectra show that these polymer derivatives are able to exchange ligands with selected nucleophilic groups in biological environment.     

香草醛异烟酰腙与钴、镍、铜、锌和镉配合物的合成和性质研究

本文合成了香草醛异烟酰腙(H_2L~Ⅰ)和邻香草醛异烟酰腙(H_2L~Ⅱ)与钴(Ⅱ)、镍(Ⅱ)、铜(Ⅱ)、锌(Ⅱ)和镉(Ⅱ)的九个新配合物:M(HL~Ⅰ)_2·nH_2O[M(Ⅱ)=Co、Ni、Cu、Zn和Cd,n=0,2]和M(HL~Ⅱ)_2·nH_2O[M(Ⅱ)=Co、Ni、Cu和Zn,n=0-3]。采用元素分析、红外光谱、电子光谱、电导、磁化率、X-射线粉末衍射和热分析研究了两系列配合物的组成和性质。     

SYNTHESIS AND STRUCTURE OF Pd(II) COMPLEXES OF 1,2,3-TRIPHENYLGUANIDINE

Abstract

The formation of two complexes by reaction of [PdCl₄]^2- with 1,2,3-triphenylguanidine (PhNH)₂C=NPh under different metal/ligand ratios has been observed and the structure of the complex [(1,2,3-triphenylguanidine)₂PdCl₂] has been determined by X-ray diffraction methods. The ligands are coordinated as neutral monodentate molecules to the metal centre through their imine nitrogen atoms. The second Pd(II) complex is [Pd(1,2,3-triphenylguanidine)₄]²⁺ and was isolated by precipitation with ClO^? ₄.     

二氧化硅负载聚（丙烯腈－乙烯基三乙氧基硅烷）钯（Ⅱ）配合物的合成和结构表征

本文合成了二氧化硅负载聚（丙烯腈－乙烯基三乙氧基硅烷）钯（Ⅱ）络合物并对该加氢摧化剂及其载体进行了结构表征。证明钯与氰基络合。     

2-(N-十六烷基氨基甲酰基)-8-羟基喹啉金属配合物的制备及红外光谱研究

合成了新的十一个２－（Ｎ－十六烷基氨基甲酰基）－８－羟基喹啉（Ｃ２６Ｈ３９Ｎ２Ｏ２，简写为ＨＬ）的配合物［ＭＬ２］，（Ｍ＝Ｍｎ（Ⅱ）、Ｃｏ（Ⅱ）、Ｎｉ（Ⅱ）、Ｚｎ（Ⅱ）、Ｃｄ（Ⅱ）、Ｐｄ（Ⅱ）、Ｍｇ（Ⅱ）和Ｃａ（Ⅱ））、［ＭＬ２Ｃｌ（Ｈ２Ｏ）４］（Ｍ＝Ｌａ（Ⅲ）、Ｇａ（Ⅲ））和［ＣｕＬＣｌ］，并经元素分析、摩尔电导、磁性和红外光谱所表征。红外光谱表明：配合物是以三齿形式与金属离子配位。配合物中Ｃ－Ｏ键伸缩振动频率与中心金属离子的相对原子质量或中心离子的电离势呈双线性关系。     

SYNTHESIS,CHARACTERIZATION AND SOLUTION CHEMISTRY OF NEW Re(V) DIOXO COMPLEXES

Abstract

In this work, we report the synthesis, characterization and potentiometric studies of new Re(V) complexes of general formula [ReO₂(amine)₂]⁺ (amine = 1,2-diaminopropane, 1,4-diaminobutane, N,N′-diethylethylenediamine, diethylenetriamine, triethylenetetramine and N-tris(2-aminoethyl)amine). Compounds were prepared starting from [ReO₂I(PPh₃)₂] and characterized by several techniques. The presence of different substituent groups in the diamines (including alkyl and amine groups) allows the presence of pendant arms. When these groups are free amino groups, they can react with acids such as H⁺ and M²⁺ cations and studied by potentiometry. The formation of very stable binuclear species was demonstrated.     

用固体核磁共振和电子能谱研究我国高硫煤的结构

用固体ＮＭＲ和ＸＰＳ技术研究了我国三种（广西合山煤、湖南辰溪煤、浙江长广煤）高硫煤的结构特征。由固体ＮＭＲ测试结果计算出煤的十二种结构参数和芳香簇团的大小，获得了三个样品的结构特征及变化规律，由ＸＰＳ测试结果得到了煤中各种不同形态硫、氮的结合能数值。根据前入所做的模型化合物的结果，得知三咱煤中硫元素主要以噻吩硫形态存在，氮元素主要以吡啶和中的形态存在。     

SYNTHESIS AND STEREOCHEMISTRY OF PENTACARBONYL(PHOSPHOLE)METAL(0)- AND TETRACARBONYLBIS(PHOSPHOLE)METAL(0) COMPLEXES OF 6B ELEMENTS

Abstract

Pentacarbonylphospholemetal(0) and cis-tetracarbonylbis(phosphole)metal(0) complexes were synthesized from the thermal reaction of M(CO)₃(THF) and M(CO)₄(COD) (M: Cr, Mo, W) with corresponding phosphole (1-phenyl-3,4-dimethylphosphole, 1-phenyl-3-methylphosphole, and 1-phenylphosphole). These complexes were isolated as orange crystals by column chromatography on silicagel at 253 K and crystallization from n-hexane at 223 K and characterized by means of IR and NMR (¹H, ¹³C, and ³¹P). Spectroscopic data shows that the phosphole is coordinated to the transition metal through its phosphorus atom rather than through the conjugated diene unit in the both types of complexes. The tetracarbonylbis(phosphole)metal(0) complexes were found to have cis-arrangement of two phosphole ligands. Comparing ¹³C-NMR chemical shifts of the complexes with the free ligands, one can deduce that the involvement of the phosphorus atom in the ring π-electron delocalization is drastically reduced upon coordination. This is attributed to the stronger [sgrave]-donation but weaker π-accepting ability of the phosphorus atom in the phosphole ligands compared to the carbonyl groups.     

SYNTHESIS AND ANTIBACTERIAL ACTIVITY OF SOME METAL COMPLEXES OF BETA-LACTAMIC ANTIBIOTICS

Abstract

An overview of the results of the interaction of β-lactamic antibiotics with some transition metal ions is given. Several complexes have been synthesized and characterized by physicochemical and spectroscopic methods. Some exhibit very promising antibacterial activity. Clavulanic acid (L₁), penicillin (L₂), ampicillin (L₃), cephalexin (L₄), cefazolin (L₅) and cephalothin (L₆) were allowed to react with metal ions in methanol under nitrogen. IR spectra of clavulanic acid, penicillin and ampicillin complexes showed strong modifications of the carbonyl group located on the lactamic ring, indicating that this oxygen participates in the coordination to the metal ions along with the carboxylate group. Thus L₁ and L₂ behave as monoanionic bidentate ligands while L₃ behaves as a monoanionic tridentate ligand. The IR spectra of cephalexin, cefazolin and cephalotin chelates show that the beta lactamic carbonyl group does not participate in coordination to the metal ions. A relationship between the structure of the complexes and their antibacterial activity can be observed.

In vitro antibacterial activity of the antibiotics and the complexes were tested using the filter paper diffusion method and the chosen strains include Escherichia coli ATCC 10536, Pseudomonas aeruginosa ATCC 9027, Salmonella typhimorium ATCC 14028, Staphylococcus aureus ATCC 6538, Bacillus cereus ATCC 9634, Proteus mirabilis 35659, Proteus vulgaris ATCC 9920, Klebsiella pneumoniae ATCC 10031, Salmonella sp, Shigella sp ATCC 11126, Streptococcus viridans and Salmonella enteritidis ATCC 497.