Physical,chemical and biological studies on transition metal complexes of chelating tridentate ligand

Summary The interaction of 1-benzoin-4-phenylthiosemicarbazone (H₂ BPS) with some transition metal ions has been investigated. The ligand can function as a tridentate chelating agent, giving M(HBPS)₂ and M(BPS). Potentiometric studies proved that the mechanism of chelation is based on hydrogen ion liberation. Spectral studies in solution show that the ligand could be used for the microdetermination of Cu^IIions. On the basis of magnetic and spectral data, an octahedral structure is proposed for the Co^II and Ni^II complexes and a square-planar structure for the Cu^II complex. The corrosion inhibition of aluminium in Cl₃CCO₂H using H₂BPS is studied. The electrical conductivity of H₂BPS and of its complexes have been measured. The ligand shows an activation energy in the range of semiconducting materials. The antimicrobial activity of all compounds has also been demonstrated.     

L?sungsmitteleinflu? auf das Redoxverhalten des Hexakismethylisonitrilmangan (I) ions

The redox behaviour of hexakismethylisonitrilmanganese(I) [MnL ₆ ⁺] has been studied in acetic acid, dichloromethane, 1,2-dichloroethane, propylenecarbonate, butyrolactone, methanol, ethanol, nitromethane, acetonitrile, N-methyl-2-pyrrolidinone, dimethylformamide, dimethyl sulfoxide and water. The reversible diffusion-controlled oxidation MnL ₆ ⁺/MnL ₆ ²⁺ could be observed in all solvents studied, on both the dropping mercury electrode and the stationary platinum electrode. Employing tetrabutylammonium perchlorate as supporting electrolyte, the oxidation MnL ₆ ²⁺/MnL ₆ ³⁺ was observable only in acetic acid, nitromethane, 1,2-dichloroethane, dichloromethane, propylenecarbonate, butyrolactone and acetonitrile. In all other solvents oxidation of the solvent preceded the oxidation MnL ₆ ²⁺/MnL ₆ ³⁺. Poorly defined polarographic waves attributable to the one electron reduction of the MnL ₆ ⁺ were observed in butyrolactone, propylenecarbonate, acetonitrile, dimethylformamide, N-methyl-2-pyrrolidinone and dimethyl sulfoxide. All potential values were recorded versus bisbiphenylchromium(I)-iodide [BBCr(I)J], the problems of measuring against external aqueous reference electrodes are discussed. The redox potential of the process MnL ₆ ⁺/MnL ₆ ²⁺ was found to be a function of the donor properties of the solvents used; the effects of outer sphere coordination on the redox behaviour of this couple are discussed. No effect of the supporting electrolytes tetrabutylammonium perchlorate, tetraethylammonium nitrate and tetraethylammonium perchlorate on the redox behaviour of MnL ₆ ⁺ was found. The UV-spectrum of MnL ₆(PF₆)₂ has been recorded.     

Medical dosimetry in Hungary

Radiation exposure of medical staff during cardiological and radiological procedures was investigated. The exposure of medical staff is directly connected to patient exposure. The aim of this study was to determine the distribution of doses on uncovered part of body of medical staff using LiF thermoluminescent (TL) dosimeters in seven locations.Individual Kodak film dosimeters (as authorized dosimetry system) were used for the assessment of medical staff's effective dose. Results achieved on dose distribution measurements confirm that wearing only one film badge under the lead apron does not provide enough information on the personal dose.The value of estimated annual doses on eye lens and extremities (fingers) were in good correlation with international publications.     

The Synthesis,Characterization and DC Electrical Conductivity of Polypyrrole‐Zirconium Complex

Polypyrrole‐zirconium complex has been synthesized by reacting 2‐amino‐3,4‐dicyano‐5‐mercaptopyrrole with zirconium nitrate in absolute ethanol under reflux for 24 h. The product has been characterized by elemental analyses, FTIR spectroscopy, in addition to thermal analysis (TGA and DSC) and its solubility has been investigated. The DC electrical conductivity variation of polypyrrole‐zirconium complex has been studied in the temperature range 300–500 K after annealing for 24 h at 100°C and doping with I₂, FeCl₃ and CuCl₂ · H₂O for comparison. An attempt has been made to interpret the DC electrical conductivity behavior and thermal properties to chain length, dopant used, polymer structure and attached groups.     

Synthesis and antibacterial activity of some novel thieno[2,3-c]pyridazines using 3-amino-5-phenyl-2-ethoxycarbonylthieno[2,3-c]pyridazine as a starting material

3-Amino-5-phenyl-2-ethoxycarbonylthieno[2,3-c]pyridazine (6) was prepared by reaction of 4-cyano-6-phenylpyridazine-3(2H)-thione (4) with ethyl chloroacetate in the presence of sodium ethoxide. Hydrazinolysis of compound 6 yielded the corresponding carbohydrazide, (9) which on treatment with acetylacetone and ethyl acetoacetate produced the novel thieno[2,3-c]pyridazines (10 and 11). Treatment of compound 9 with nitrous acid yielded the corresponding carboazide (13), which upon boiling in toluene furnished imidazo[4′,5′:4,5]thieno[2,3-c]pyridazine (15). Pyrimidothienopyridazines (16–18) were achieved by cyclocondensation of compound 9 with some reagents, namely acetic anhydride, formic acid, and triethyl orthoformate. The newly synthesized compounds were confirmed by elemental analyses and spectral data. The antibacterial activities of the new compounds were also evaluated.     

Facile synthesis and antimicrobial evaluations of some novel pyrazolo[3,4-b]selenolo[3,2-e]pyrazines and their related heterocycles

A new series of pyrazolopyrazinoselenolotriazolopyrimidines was synthesized by a facile method based on condensation of 5-amino-3-methyl-1-phenyl-1H-pyrazolo[3,4-b]selenolo[3,2-e]pyrazine-6-carbonitrile ( 3 ) with triethyl orthoformate followed by intramolecular cyclization with hydrazine to afford 7-amino-8-imino-3-methyl-1-phenyl-1,8-dihydro-7H-pyrazolo[3″,4″:5′,6′]pyrazino[2′,3′:4,5] selenolo[3,2-d]pyrimidine ( 5 ). The latter compound was utilized as a multipurpose precursor for the construction of other new triazoles fused to the pyrazolopyrazino- selenolopyrimidine moiety. Alternatively, acetylation and chloro-acetylation of compound 3 using acetic anhydride and chloroacetyl chloride yielded the acetyl amino 11 and chloroacetamido 12 derivatives, respectively. Compound 12 underwent nucleophilic substitution upon reaction with morpholine to provide the morpholinyl acetamide 13 . Furthermore, the pyrazolopyridoselenolopyrazine ring system 14 was synthesized by the reaction of the o-amino-carbonitrile 3 with malononitrile. Assignment of the chemical structures for the new compounds was confirmed depending on elemental and spectral techniques. On the other hand, most of the synthesized compounds revealed promising results against various bacterial and fungal strains.     

Structural,thermal, optical and conductivity studies of Co/ZnO nanoparticles doped CMC polymer for solid state battery applications

In this study, a simple chemical precipitation method was used to synthesize ZnO: Co²⁺ as nanoparticles. The solution casting technique was used for the preparation of polymer films of Carboxymethyl cellulose (CMC) doped with different contents (0.5, 1.5, 3, and 5 wt%) of ZnO/Co NPs. As shown by the X-ray diffraction, the average size of ZnO/Co crystallite of the NPs is 25.6 nm. Meanwhile, the addition of ZnO/Co reduced the semi-crystallinity of CMC. The Fourier transform infrared (FTIR) confirmed the interaction between the ZnO/Co NPs and the polymer CMC. The direct and indirect band gap (Eg) was reduced from (5.32–5.01 eV and 5.20 to 4.99 eV respectively) with the increase in ZnO/Co NPs content up to 3 wt% after this content the Eg is increased as shown by the UV–Vis spectra. In addition, the results of TGA displayed the decomposition of the nanocomposite to be little compared to that of the pure CMC indicating the success of fabrication of products. The improvement of the ionic conductivity was noticed upon the addition of ZnO/Co NPs into the polymer CMC system which can be explained in terms of an increase in amorphicity as shown by the impedance spectroscopic study. It was found that the optimum ionic conductivity (3.209 × 10⁻⁶ Scm⁻¹) at ambient temperature was higher for the sample containing 1.5 wt% ZnO/Co NPs with highest of amorphicity and the lowest total loss of weight. Therefore, the improvements in optical properties, thermal stability, and AC conductivity which were observed represent a strong support for the use of the nanocomposite films in the solid state battery applications.     

Chemical composition variations,allelopathic, and antioxidant activities of Symphyotrichum squamatum (Spreng.) Nesom essential oils growing in heterogeneous habitats

The present study aimed to analyze the chemical composition of Symphyotrichum squamatum EOs growing in two different habitats to explore the ecological implication on the EOs production and evaluate their antioxidant and allelopathic potentialities. The EOs from the aerial parts collected from coastal Mediterranean belt and inland abandoned habitats in the Nile Delta of Egypt, were extracted and analyzed using gas chromatography-mass spectrometry. Sixty compounds were characterized as overall constituents of EOs from both samples. Sesquiterpenes were the main component and represented by 69.77% and 88.68% from coastal and inland sample, respectively. The coastal sample attained a relatively high content of monoterpenes compared to the inland sample. Major compounds from the EOs of the coastal habitat sample, were humulene epoxide, (-)-spathulenol, (-)-caryophyllene oxide, germacrene D, and α-humulene representing 59.72%. However, β-pinene, germacrene D, α-humulene, α-muurolene, humulene epoxide, (-)-caryophyllene oxide, and β-cadinene were the major compounds of EOs of the inland habitat sample, representing 63.70%. The correlation analysis revealed more correlation between the Egyptian inland S. squamatum and the Japanese ecospecies. However, the Egyptian coastal S. squamatum and Turkish ecospecies were more correlated to each other. The present data suggested that chemotypes of S. squamatum maintain their typical pattern despite ecological or climatic differences. The EOs of S. squamatum showed moderate antioxidant activity, wherein coastal and inland EOs have an IC₅₀ value of 382.53 and 559.63 μL L⁻¹, respectively. Also, the EOs from both habitats showed moderate allelopathic activity against the noxious weed Bidens pilosa. However, the activity of the coastal sample was more than inland one and could be attributed to the content of the major compounds, especially the oxygenated terpenes.