Thermal,spectroscopic and structural studies of zinc(II) complex with nicotinamide

The zinc(II) complex with nicotinamide (ncam) was prepared and investigated by single-crystal X-ray diffraction, infrared spectrum (FTIR), conductivity and thermal analysis techniques. The formula of complex is [Zn(ncam)₂(H₂O)₄](NO₃)₂·2H₂O. The nicotinamide molecule has three following donor sites: pyridine ring nitrogen, aminonitrogen and carbonyl group oxygen. In this monomeric complex, the Zn(II) ion is six-coordinated by two pyridine ring N atoms and four water O atoms in a slightly distorted octahedral arrangement. In the crystal structure, intermolecular O-H…O and N-H…O hydrogen bonds link the molecules to form a supramolecular structure. The complex is stable up to 323 and above 360 K it dehydrates in one step losing six water molecules. The dehydration proceeds in the range of 360–438 K, and its enthalpy value is equal to 62.6±1.5 kJ mol⁻¹.     

Synthesis,spectral and thermal properties of macrocyclic zinc(II) complexes

The new zinc ternary complexes [Zn(cyclen)NO₃]ClO4 (I), [Zn₂(cyclen)₂(m-nic)](ClO₄)₃ (II), [Zn₂(cyclen)₂(m-pic)](ClO₄)₃ (III) (cyclen=1,4,7,10-tetraazacyclododecane; nic=nicotinic acid; pic=picolinic acid) were synthesized and their spectral and thermal properties were investigated. The compounds were characterized by elemental analysis, IR spectroscopy and TG/DTG, DTA methods. Moreover, the way of coordination of pyridinecarboxylate anions was proposed on the basis of the spectral data and consequently proved with results of X-ray structure analysis. This revised version was published online in August 2006 with corrections to the Cover Date.     

Thermal study of zinc(II) 4-chlorosalicylate complex compounds with bioactive ligands

Three new complex compounds of general formula Zn{4-ClC₆H₃-2-(OH)COO}₂⋅L₂⋅nH₂O (where L=thiourea (tu), nicotinamide (nam), caffeine (caf), n=2,3), were prepared and characterized by chemical analysis, IR spectroscopy and their thermal properties were studied by TG/DTG, DTA methods. It was found that the thermal decomposition of hydrated compounds starts with the release of water molecules. During the thermal decomposition of anhydrous compounds the release of organic ligands take place followed by the decomposition of salicylate anion. Zinc oxide was found as the final product of the thermal decomposition performed up to 650°C. RTG powder diffraction method, IR spectra and chemical analysis were used for the determination of products of the thermal decomposition.     

Thermal decomposition of nickel(II) complexes under quasi-equilibrium conditions

The stoichiometry of thermal decomposition and the relationship between the thermal parameters (quasi-equilibrium decomposition temperaturesT _D and decomposition entalpies H _D) of NiL₄(NCS)₂ complexes (L=imidazole derivatives) were studied. It was found that changes in the experimental conditions strongly influence the decomposition stoichiometry. TheT _D and H _D can be ordered in the following sequence (according toL): imidazole<2-Me imidazole<2-Et imidazole相似文献   

The physicochemical and biological properties of zinc(II) complexes

Spectroscopic (IR), thermoanalytical (TG/DTG, DTA) and biological methods were applied to investigate physicochemical and biological properties of seven zinc(II) complex compounds of the following formula Zn(HCOO)₂·2H₂O (I), Zn(HCOO)₂·tph (II), Zn(CH₃COO)₂·2H₂O (III), Zn(CH₃COO)₂·tph (IV), Zn(CH₃COO)₂·2phen (V), Zn(CH₃CH₂COO)₂·2H₂O (VI), Zn(CH₃CH₂CH₂COO)₂·2H₂O (VII), where tph=theophylline, phen=phenazone. The formation of various intermediates during thermal decomposition suggests the dependence on the length of aliphatic carboxylic chain and type of N-donor ligand (tph, phen). The final product of the thermal decomposition was ZnO. The antimicrobial activity of these complexes were tested against G⁺ and G^– bacteria. Strong inhibitive effect was observed towards E. coli, salmonellae and Staph. aureus.     

Thermal study of zinc(II) salicylate complex compounds with bioactive ligands

Five new complex compounds of general formula Zn(Hsal)_2·L₂·nH₂O (where Hsal=OHC₆H₄COO^-, L=thiourea (tu), nicotinamide (nam), caffeine (caf), theobromine (tbr), n=2-4), were prepared and characterized by chemical analysis, IR spectroscopy and studied by methods of thermal analysis (TG/DTG, DTA). It was found that the thermal decomposition of hydrated compounds starts with the release of water molecules. During the thermal decomposition of anhydrous compounds the release of organic ligands take place followed by the decomposition of salicylate anion. Zinc oxide was found as the final product of the thermal decomposition heated up to 800°C. RTG powder diffraction method, IR spectra and chemical analysis were used for the determination of products of the thermal decomposition. This revised version was published online in August 2006 with corrections to the Cover Date.     

Preparation and some properties of tetracyano complexes M(en)M′(CN)4 (M=Cd(II), Mn(II);M′=Ni(II), Cd(II))

Two new tetracyano complexes of the composition MnenNi(CN)₄ and MnenCd(CN)₄ were prepared and identified. Their struture and properties were investigated by IR and UV-VIS spectroscopy, X-ray powder diffraction and by measuring magnetic moments. The results were confronted with the structure and properties of the compounds CdenNi(CN)₄ and CdenCd(CN)₄. The results of this study show a considerable similarity between these groups of compounds. The thermal behaviour of all the examined compounds was investigated derivatographically. The following order of thermal stability of the investigated complexes was observed: Cd?Cd(215°C)相似文献   

bis(nicotinamide) and bis(N,N-diethyl nicotinamide) p-hydroxybenzoate complexes of Ni(II), Cu(II) AND Zn(II)

The mixed-ligand p-hydroxybenzoate complexes of Ni(II), Cu(II) and Zn(II) with nicotinamide and N,N-diethylnicotinamide were synthesized and characterized by elemental analysis, magnetic susceptibility measurements and mass spectrometry. The thermal behavior of the complexes was studied by simultaneous TG, DTG and DTA methods in static air atmosphere. The infrared spectral characteristics of the complexes are also discussed. The complexes contain two water molecules, two p-hydroxybenzoato (p-hba) and two nicotinamide (na) (or diethylnicotinamide (dena)) ligands per formula unit. In these complexes, all ligands are coordinated to the metal ion as monodendate ligands. In Zn(II)-na and Cu(II)-dena complexes, thep-hydroxybenzoate behaves as bidentate chelating ligand through carboxylic oxygen atoms. The decomposition pathways and the stability of the complexes are interpreted in the terms of the structural data. The final decomposition products were found to be the respective metal oxides. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal and photochemical behaviour of Zn(II) complexes of some cephalosporins

Zn(II) complexes of some cephalosporin antibiotics namely cephalexin, cephapirin, cefamandole, cefuroxime, cefotaxime and ceftazidime were synthesised and characterized. The stoichiometrics and the mode of bonding of the complexes were deduced from their elemental analysis, IR and electronic spectroscopies. Thermal stabilities and the photochemical behaviour of the complexes were studied. The Zn(II) complex of cephalexin exhibited a high light sensitivity. The remaining Zn(II) complexes behaved similarly to their free antibiotics, upon irradiation.This revised version was published online in November 2005 with corrections to the Cover Date.     

Acetate and malonate complexes of cobalt(II), nickel(II) and zinc(II) with hydrazinium cation

The hydrazinium(1+) metal acetates and malonate dihydrates of the molecular formula [(N₂H₅)₂M(CH₃COO)₄] and (N₂H₅)₂[M(OOCCH₂COO)₂(H₂O)₂] respectively, whereM=Co, Ni or Zn, have been prepared and characterized by chemical analyses, conductance, magnetic, spectral, thermal and X-ray powder diffraction studies. The magnetic moments and electronic spectra indicate that these complexes are of high-spin octahedral variety. The infrared spectra show that the hydrazinium ions are coordinated in the case of acetate complexes, whereas in the malonate complexes the hydrazinium ions are out side the coordination sphere. These complexes undergo exothermic decomposition in the temperature range 150–450°C to give the respective metal oxide as the final residue. The X-ray powder diffraction patterns of the malonate complexes indicate isomorphism among them.     

Thermal,spectral and magnetic studies on glycine complexes of cobalt(II), nickel(II) and zinc(II) with hydrazine

Hydrazinium metal glycinates [(N₂H_{5 2}M(NH₂CH₂COO)₄] and bis(hydrazine)metal glycinates, [M(NH₂CH₂COO)₂(N₂H₄)₂], whereM=Co, Ni or Zn have been prepared and characterized by chemical analyses, magnetic moments and vibrational and electronic spectra. The thermal behaviour of these compounds has been studied by thermogravimetry and differential thermal analyses. These complexes decompose with high exothermicity giving metal powder as the final residue. The X-ray powder data of each set of complexes show isomorphism among themselves.     

Preparation,characterization and biological evaluation of copper(II) and zinc(II) complexes with Schiff bases derived from amoxicillin and cephalexin

Copper(II) and zinc(II) complexes of Schiff bases obtained by condensation of amoxicillin and cephalexin with salicylaldehyde/pyridoxal were prepared and characterized by microanalytical, thermogravimetric, magnetic and spectroscopic data. All the complexes were found to be six‐coordinate and containing two water molecules. The electron paramagnetic resonance spectral lines exhibited rhombic distortion from axial symmetry, with g_|| > g_? > g_e, in the copper(II) complexes. The geometry of the zinc(II) complexes appears to be octahedral. All the compounds under investigation showed antibacterial activity. The antibacterial activity showed the following trend: copper(II) complexes > zinc(II) complexes > Schiff base ligands > parent drugs. The copper(II) complexes with the Schiff bases derived from cephalexin showed substantially enhanced activity against Pseudomonas aeruginosa compared with the parent drug. All the copper complexes were also found to be active against kaolin paw oedema, whereas the parent drugs were inactive. Copyright © 2005 John Wiley & Sons, Ltd.     

Thermal stability of new zinc acetate-based complex compounds

New zinc acetate based complex compounds (of general formula Zn(CH₃COO)₂·1?2L·nH₂O) containing one or two molecules of urea, thiourea, coffeine and phenazone were prepared namely: Zn(CH₃COO)₂·2.5H₂O, Zn(CH₃COO)₂·2u·0.5H₂O, Zn(CH₃COO)₂·tu·0.5H₂O, Zn(CH₃COO)₂·2tu, Zn(CH₃COO)₂·cof·2.5H₂O, Zn(CH₃COO)₂·2cof·3.5H₂O, Zn(CH₃COO)₂·2phen·1.5H₂O. The compounds were characterized by IR spectroscopy, chemical analysis and thermal analysis. Thermal analysis showed that no changes in crystallographic modifications of the compounds take place during (heating in nitrogen before) the thermal decompositions. The temperature interval of the stability of the prepared compounds were determined. It was found that the thermal decomposition of hydrated compounds starts by the release of water molecules. During the thermal decomposition of anhydrous compounds in nitrogen the release of organic ligands take place followed by the decomposition of the acetate anion. Zinc oxide and metallic zinc were found as final products of the thermal decomposition of the zinc acetate based complex compounds studied. Carbon dioxide and acetone were detected in the gaseous products of the decomposition of the compounds if ZnO is formed. Carbon monoxide and acetaldehyde were detected in the gaseous products of the decomposition, if metallic Zn is formed. It is supposed that ZnO and Zn resulting from Zn acetate complex compounds here studied, possess different degree of structural disorder. Annealing takes place by further heating above 600°C.     

Thermal,spectral and biological properties of Zn(II) complex compounds with phenazone

The thermal decomposition of the complexes Zn(form)₂⋅2phen (I), Zn(ac)₂⋅2phen (II), Zn(prop)₂⋅2phen (III), Zn(but)₂⋅2phen (IV), where phen=phenazone, form=formiate, ac=acetate, prop=propionate, but=butyrate has been studied in air by TG/DTG and DTA methods. The possible mechanism of the thermal decomposition was proposed. The final product of thermal decomposition was ZnO. IR data show unidentate coordination of carboxylate group to Zn(II) ion. The complexes were tested against various strains of microorganisms and their efficiency decrease in the sequence yeasts >bacteria>filamentous fungi.     

Copper(II) and zinc(II) complexes with terpene derivatives of ethylenediamine: unexpected ligand transformations

Crystallization of copper and zinc complexes with imino terpene derivatives of ethylenediamine causes unexpected chemical transformation of the ligand. Copper(II) chloride catalyzes the hydrolysis of the imine and also acts as a halogenating agent. Crystallization of the zinc complex in acetone is accompanied by the condensation of the ketone with the primary amino group of the ligand.     

Thermal and Spectral Characterization of 5-Cholro-2-methoxybenzoates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II)

The thermal stabilities of 5-chloro-2-methoxybenzoates of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) were studied in air and nitrogen atmospheres. The complexes were obtained as mono-, di-, tetra-and pentahydrates with a metal to ligand ratio of 1:2 and with colours typical for M²⁺ ions (Mn-slightly pink, Co-pink, Ni-green, Cu-blue and Zn-white) and as polycrystalline compounds. When heated they dehydrate to form anhydrous salts which nextare decomposed to the oxides of the respective metals in air while in nitrogen to the mixtures of metal oxides and oxychlorides and carbon. The most thermally stable in air, nitrogen and argon atmospheres is 5-chloro-2-methoxybenzoate of Cu(II) while the least thermally stable is that of Co(II). This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal properties of cyanatocopper(II) complexes with pyridine,bipyridine and phenanthroline

The thermal properties of cyanatocopper complexes with pyridine, bipyridine and phenanthroline are described in this paper. It was found that the thermal stabilities of the complexes were found to increase in the order pybipy2(NCS)₂ (L=pyridine and its methyl derivates) which are composed of the liberation of ligandsL and redox reactions of thiocyanate ligands with the central Cu(II) atom [1, 2]. The decomposition temperature of thiocyanate ligands depends on the properties of the ligandsL present in the coordination sphere. An analogous course of thermal decomposition was also observed for [Cu(bipy)₂(NCX)](NCX) (X=S or Se) [3]. For the phenanthroline complexes [Cu(phen)₂(NCX)₂] (X=S or Se) the thermal stability was found to increase significantly (by about 140C) and the decomposition stoichiometry was also changed [3].The present paper contains the results of thermoanalytical studies on bipyridine and phenanthroline cyanatocopper complexes, and a comparison of the thermal properties of pyridine cyanato and isothiocyanatocopper complexes.     

Thermal and other properties of complexes of Mn(II), Co(II) and Ni(II) with 2,2'-bipyridine and trichloroacetates

Complexes of the general formulae Mn(2-bpy)₂(CCl₃COO)₂, Co(2-bpy)₂(CCl₃COO)₂·H₂O and Ni(2-bpy)₂(CCl₃COO)₂·2H₂O (where: 2-bpy=2,2'-bipyridine) have been prepared and characterized by VIS and IR spectroscopy, conductivity and magnetic measurements. The thermal properties of complexes in the solid state were studied under non-isothermal conditions in air atmosphere. During heating the complexes decompose via different intermediate products to the oxides Mn₃O₄, CoO and NiO. A coupled TG-MS system was used to detection the principal volatile products of thermal decomposition and fragmentation processes of obtained compounds. The principal volatile products of thermal decomposition of complexes are: H₂O⁺, CO₂ ⁺, Cl₂ ⁺ and other. This revised version was published online in August 2006 with corrections to the Cover Date.     

Thermal characterization of new complexes of Zn(II) and Cd(II) with some bipyridine isomers and propionates

New mixed ligand complexes of the following stoichiometric formulae: M(2-bpy)₂(RCOO)₂·nH₂O, M(4-bpy)(RCOO)₂·H₂O and M(2,4’-bpy)₂(RCOO)₂·H₂O (where M(II)=Zn, Cd; 2-bpy=2,2’-bipyridine, 4-bpy=4,4′-bipyridine, 2,4′-bpy=2,4′-bipyridine; R=C₂H₅; n=2 or 4) were prepared in pure solid-state. These complexes were characterized by chemical and elemental analysis, IR and conductivity studies. Thermal behaviour of compounds was studied by means of DTA, DTG, TG techniques under static conditions in air. The final products of pyrolysis of Cd(II) and Zn(II) compounds were metal oxides MO. A coupled TG/MS system was used to analyse of principal volatile products of thermal decomposition or fragmentation of Zn(4-bpy)(RCOO)2·H2O under dynamic air and argon atmosphere. The principal species correspond to: C⁺, CH⁺, CH₃ ⁺, C₂H₂ ⁺, HCN⁺, C₂H₅ ⁺ or CHO⁺, CH₂O⁺ or NO⁺, CO₂ ⁺, ¹³C¹⁶O₂ ⁺ and ¹²C¹⁶O¹⁸O⁺ and others; additionally CO⁺ in argon atmosphere.     

Thermal and spectral analyses of complexes of zinc(II)tetra-tertbutylphthalocyanine with amines

Spectral and thermochemical studies of complexes of zinc(II)tetra-tertbutylphthalocyanine (Zn(t-Bu)₄Pc) with some amines have been carried out. Spectral effects of the complex formation of the metallophthalocyanine with amines have been established. It has been found that an ability of Zn(t-Bu)₄Pc to coordinate amines depends on both their nature and conditions of preparation. Similarity of the crystal structures of biligand and monoligand of Zn(t-Bu)₄Pc complexes to individual β- and α-polymorphs of Zn(t-Bu)₄Pc, respectively is proved by IR spectroscopy and X-ray diffraction method.