A.A.M. Belal

Supramolecular structure, mixed ligands and substituents effect on the spectral studies of oxovanadium(IV) complexes of bioinorganic and medicinal relevance.

An interesting series of heterocyclic mixed ligand of oxovanadium(IV) complexes have been synthesized by the reaction of vanadium(IV) sulfate with rhodanine azo (HL(n)) in the presence of β-diketon (LH). The elemental analysis, magnetic moments, spectral (UV-Vis, IR, (1)HNMR and ESR) with thermal studies were used to characterize the isolated complexes. The IR showed that the ligands (HL(n) and LH) act as a monobasic bidentate through the (NN), oxygen keto moiety and oxygen atom of the two enolate groups thereby forming a six-membered. The molar conductivities show that all the complexes are non-electrolytes. The ESR spectra indicate that the free electron is in d(xy) orbital. The calculated bonding parameter indicates that in-plane σ-bonding is more covalent than in-plane π-bonding. The coordination geometry around oxovanadium(IV) in all complexes is a hex-coordinated trans octahedral, with one bidentate ligand (L(n)), and one bidentate ligand (L). Electronic and magnetic data proposed the octahedral structure for all complexes under investigation. ESR spectra of VO(2+) reveal data that confirmed the proposed structure. The value of covalency factor (β(1)(∗))(2) and orbital reduction factor K accounts for the covalent nature of the complexes. All electronic transitions were assigned. The Hammetts constant is also discussed.

Supramolecular structure and spectral studies on mixed-ligand complexes derived from β-diketone with azodye rhodanine derivatives

A novel method to synthesize some mononuclear ternary palladium(II) complexes of the general formula [Pd(L(n))L] (where LH=diketone=acetylacetone, HL(n)=azorhodanine) has been synthesize. The structure of the new mononuclear ternary palladium(II) complexes was characterized using elemental analysis, spectral (electronic, infrared and (1)H &(13)C NMR) studies, magnetic susceptibility measurements and thermal studies. The IR showed that the ligands (HL(n) & LH) act as monobasic bidentate through the azodye nitrogen, oxygen keto moiety and two enolato oxygen atoms. The molar conductivities show that all the complexes are non-electrolytes. Bidentate chelating nature of β-diketone and azorhodanine anions in the complexes was characterized by (electronic, infrared and (1)H &(13)C NMR) spectra. Square planar geometry around palladium has been assigned in all complexes. Various ligand and nephelouxetic parameter have been calculated for the complexes. The thermal decomposition for complexes was studied.

Polymer complexes. LVIII. Structures of supramolecular assemblies of vanadium with chelating groups

Oxovanadium(IV) polymer complexes of formulation {[(VO)L](2)}(n) (1) and [(VO)LB](n) (2-4), where H(2)L is tridentate and dianionic ligand (allylazorhodanine) and B is planar heterocyclic and aliphatic base have been prepared and characterized by elemental analyses, IR, (1)H NMR, electronic spin resonance spectra, magnetic susceptibility measurements, molar conductance and thermal studies. The molecular structure shows the presence of a vanadyl group in six-coordinate VNO(3)/VN(3)O(3) coordination geometry. The N,N-donor heterocyclic and aliphatic bas displays a chelating mode of binding with an N-donor site trans to the vanadyl oxo-group. In all polymeric complexes (1-4) the ligand coordinates through oxygen of phenolic/enolic and azodye nitrogen. The molar conductivity data show them to be non-electrolytes. All the polymer complexes are ESR active due to the presence of an unpaired electron. The calculated bonding parameters indicate that in-plane σ bonding is more covalent than in-plane π bonding. From the electronic, magnetic and ESR spectral data suggest that all the oxovanadium(IV) polymer complexes have distorted octahedral geometry. The thermal decomposition process of the polymeric complexes involves three decomposition steps.

Synthesis, spectroscopic, coordination and biological activities of some transition metal complexes containing ONO tridentate Schiff base ligand

The main target of this paper is to get an interesting data for the preparation and characterizations of metal oxide (MO) nanoparticles using H2L Schiff base complexes as precursors through the thermal decomposition procedure. Five Schiff base complexes of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) metal ions were synthesized from 2-[(2-hydroxy-naphthalen-1-ylmethylene)-amino]-benzoic acid new adduct (H2L). Theses complexes were characterized using infrared, electronic, mass and (1)H NMR spectroscopic techniques. The elemental analysis data was confirmed that the stoichiometry of (metal:H2L) is 1:1 molar ratio. The molar conductance indicates that all of complexes are non electrolytic. The general chemical formulas of these complexes is [M(L)(NH3)]·nH2O. All complexes are tetrahedral geometry. The thermal decomposition behavior of H2L hydrated and anhydrous complexes has been discussed using thermogravimetric analysis (TG/DTG) and differential thermal analyses (DTA) under nitrogen atmosphere. The crystalline phases of the reaction products were checked using X-ray diffractometer (XRD) and scanning electron microscopy (SEM).

Structure investigation of three hydrazones Schiff’s bases by spectroscopic, thermal and molecular orbital calculations and their biological activities

Three Schiffs bases AI (2(1-hydrazonoethyl)phenol), AII (2, 4-dibromo 6-(hydrazonomethyl)phenol) and AIII (2(hydrazonomethyl)phenol) were prepared as new hydrazone compounds via condensation reactions with molar ratio (1:1) of reactants. Firstly by reaction of 2-hydroxy acetophenone solution and hydrazine hydrate; it gives AI. Secondly condensation between 3,5-dibromo-salicylaldehyde and hydrazine hydrate gives AII. Thirdly condensation between salicylaldehyde and hydrazine hydrate gives AIII. The structures of AI-AIII were characterized by elemental analysis (EA), mass (MS), FT-IR and (1)H NMR spectra, and thermal analyses (TG, DTG, and DTA). The activation thermodynamic parameters, such as, ΔE(∗), ΔH(∗), ΔS(∗) and ΔG(∗) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bond responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

Molecular complexes of iron violurate with donor amines.

The acceptor character of iron violurate complex was studied by examining the electronic, vibrational and 1H-nmr spectra of the charge transfer molecular complexes formed between the iron violurate as pi-acceptor and some amines as n-donors. Elemental analysis and spectral results establishes 1:2 stoichiometry of the adducts. The study has been conducted at different temperatures. Values of delta G degree, delta H degree and delta S degree have been calculated from the self-consistent values of the formation constants (KCT). Ionization potentials of the donors have been calculated and the solvent effect on the KCT values is discussed. The antibacterial and antifungal effects of the molecular complexes were studied.

Role of myeloperoxidase in early diagnosis of acute myocardial infarction in patients admitted with chest pain

ABSTRACT Myeloperoxidase (MPO) is an inflammatory marker, elevated in acute coronary syndromes (ACSs), especially in acute myocardial infarction (AMI) cases. This study aimed to evaluate the diagnostic power of MPO in AMI patients. MPO, creatine kinase (CK) MB, and Troponin I (cTn I) were performed for all study patients. Area under the curves (AUCs) and 95% confidence intervals (CI); P values of baseline levels of MPO for discriminating AMI patients from noncoronary chest pain (NCCP) patients, stable angina (SA) patients, and unstable angina (UA) patients were 0.91, 95% CI: 0.82–0.99; P < 0.0001, 0.87, 95% CI: 0.77–0.98; P < 0.0001, and 0.72, 95% CI: 0.58–0.85; P = 0.002, respectively. For diagnosing AMI from ACS patients, MPO was the most efficient marker than others markers with efficiency 82.5% within 0–6 hr after the onset time of chest pain. A predictive score that depends on a combination of baseline levels of three markers (MPO, CK-MB, and TnI) was correctly discriminated 91% of the AMI patients with high specificity 76%. In conclusion, the use of baseline levels of three biomarkers in combination could confer the information that is required for best available early diagnosis of AMI.