scholarly journals Preparation and Spectroscopic Studies of Cadmium(II), Zinc(II),Mercury(II) and Vanadium(IV) Chelates Azo Ligand Derived from 4-Methyl-7-hydroxycoumarin

2021 ◽  
Vol 21 (4) ◽  
pp. 912
Author(s):  
Bayader Fathil Abass ◽  
Taghreed Mohy Al-Deen Musa ◽  
Mahmoud Najim Aljibouri

The present paper demonstrates the synthesis and characterization of some transition elements complexes derived from (E)-7-hydroxy-6-((4-methoxyphenyl)diazenyl)-4-methyl-2H-chromen-2-one. The ligand was prepared in the general route of azo dyes by coupling the diazonium salt of 4-methoxyaniline with 4-methyl-7-hydroxycoumarin in sodium hydroxide 10% (w/v) solution. The azo ligand was identified on the basis of elemental analyses, MS, H-NMR and FT-IR spectra. The products of complexes with the new azo dye were isolated by the direct reactions of the metal chlorides of cadmium(II), zinc(II), vanadium(IV) and mercury(II) ions with the alkaline solution of free ligand to afford the colored in the following formulas, complexes[ML2]2H2O formula, M=Cd(II) and Zn(II). However the vanadium(IV) complex was square pyramid in [VOL2]SO42H2O chemical formula. As well as the tetrahedral environment was suggested for mercury(II) complex in formula [HgL2]. The time and mole ratio factors were studied to obtain the optimized conditions of metal complexes formations and the observed data investigated the deprotonation of the azo-dye at pH to range (7–7.5) with 30 min as time of reaction to get pure metal chelates. The TG-DSC study confirmed the thermal stability of complexes at a wide range of average heating in inert gas of analysis and the results observed from loss weight percent investigated the proposed structures of the prepared metal complexes.

2020 ◽  
Vol 2020 ◽  
pp. 1-19
Author(s):  
Gehad G. Mohamed ◽  
Walaa H. Mahmoud ◽  
Ahmed M. Refaat

Metal complexes of the 2,2'-(1,3-phenylenebis(diazene-2,1-diyl))bis(4-aminobenzoic acid) diazo ligand (H2L) derived from m-phenylenediamine and p-aminobenzoic acid were synthesized and characterized by different spectral, thermal, and analytical tools. The H2L ligand reacted with the metal ions Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II) as 1 : 1 stoichiometry. All complexes displayed an octahedral geometry according to the electronic and magnetic moment measurements. The IR spectra revealed the binding of the azo ligand to the metal ions via two azo nitrogen atoms and protonated carboxylate O in a neutral tetradentate manner. Both IR and 1H NMR spectra documented the involvement of the carboxylate group without proton displacement. The thermal studies pointed out that the complexes had higher thermal stability comparable with that of the free ligand. SEM images revealed the presence of the diazo ligand and its Cd(II) complex in a nanostructure form. The contact angle measurements proved that the Cd(II) complex can be considered as a superhydrophobic material. The molecular and electronic structure of H2L and [Cd(H2L)Cl2].H2O were optimized theoretically, and the quantum chemical parameters were calculated. The biological activities of the ligand, as well as its metal complexes, have been tested in vitro against some bacteria and fungi species. The results showed that all the tested compounds have significant biological activities with different sensitivity levels. The binding between H2L and its Cd(II) complex with receptors of the crystal structure of S. aureus (PDB ID: 3Q8U), crystal structure of protein phosphatase (PPZ1) of Candida albicans (PDB ID: 5JPE), receptors of breast cancer mutant oxidoreductase (PDB ID: 3HB5), and crystal structure of Escherichia coli (PDB ID: 3T88) was predicted and given in detail using molecular docking.


2020 ◽  
Vol 15 (2) ◽  
pp. 61-72

New pyrazine carbohydra zone ligand N'-(1-(5-chloro-2-hydroxyphenyl) ethylidene) pyrazine-2-carbohydrazide (H2L), prepared by the condensation of equimolar amounts of pyrazine-2-carbohydrazide with 2-hydroxy-5-chloroacetophenone in methanol, reacts with suitable metal salt precursors to give complexes of two general formulae: [M(HL)(Cl)(H2O)2] {M = Mn(II), Co(II), Ni(II) and Cu(II)} and [M(L)(H2O)] {M = Zn(II) and Cd(II)}. Structure of ligand was confirmed by elemental analysis, IR, 1H and 13C NMR and mass spectroscopy, while synthesized complexes were additionally characterized by magnetic susceptibility measurements, molar conductivity measurements, XRD, ESR (for Cu(II)), SEM and thermogravimetric analysis. Spectroscopic studies confirmed a tridentate ONO donor behavior of the ligand towards the central metal ion. The molar conductance (12–17 W–1 cm2 mol–1) measurements in DMSO indicated non-electrolytic nature. Thermal behavior of the complexes suggests their extended stability and the thermal decomposition generally proceeds via partial loss of the organic moiety and ends with the formation of respective metal oxide as a final product. Various kinetic and thermodynamic parameters were evaluated using the Coats-Redfern method. The solid-state electrical conductivity of the complexes measured in the temperature range 303-463 K suggested their semiconducting behavior. The ligand and its metal complexes were screened in vitro for their antibacterial activity against the Gram-positive bacteria S. aureus and B. subtilis, the Gram-negative bacteria E. coli and S. typhi and the fungi C. albicans and A. niger. The obtained results indicated improved activity of the complexes compared to the free ligand against all studied bacterial and fungal species.


2017 ◽  
Author(s):  
Nasir Abbas ◽  
Syed Ahmad Tirmizi ◽  
Ghulam Shabir

A series of metal complexes has been synthesized from 1-(p-sulphophenyl)-3-methyl-4-amino pyrazolone with different phenol derivatives at high temperature for chromium.· Investigated metal complexes have been applied on leather which exhibit high light fastness, wash fastness and rubbing fastness.· DNA interaction has also been accomplished.Chromium (III) complexes of Azo dyes ligands envisaged on novel synthesized 4-Amino-1-(p-sulphophenyl)-3-methyl-5-pyrazolone diazonium salt coupled with different phenolic couplers appended on diverse substituents. The complexes have been characterized by elemental analysis, UV, FTIR and NMR studies. The DNA studies have been investigated for complexes by electronic absorption spectroscopy. The results have shown that chromium (III) complexes bind to DNA through intercalation mode. Synthesized Chromium complexes have been applied on leather to check their serviceability and they exhibited moderate to high values of light fastness and perspiration fastness (4–5).


2009 ◽  
Vol 131 (29) ◽  
pp. 9916-9917 ◽  
Author(s):  
Matteo P. Placidi ◽  
Aaron Joseph L. Villaraza ◽  
Louise S. Natrajan ◽  
Daniel Sykes ◽  
Alan M. Kenwright ◽  
...  

2018 ◽  
Vol 69 (7) ◽  
pp. 1678-1681
Author(s):  
Amina Mumtaz ◽  
Tariq Mahmud ◽  
M. R. J. Elsegood ◽  
G. W. Weaver

New series of copper (II), cobalt (II), zinc (II), nickel (II), manganese (II), iron (II) complexes of a novel Schiff base were prepared by the condensation of sulphadizine and pyridoxal hydrochloride. The ligand and metal complexes were characterized by utilizing different instrumental procedures like microanalysis, thermogravimetric examination and spectroscopy. The integrated ligand and transition metal complexes were screened against various bacteria and fungus. The studies demonstrated the enhanced activity of metal complexes against reported microbes when compared with free ligand.


Author(s):  
Thoria Diab ◽  
Tarek M. Mohamed ◽  
Alaa Hamed ◽  
Mohamed Gaber

Background: Chemotherapy is currently the most utilized treatment for cancer. Therapeutic potential of metal complexes in cancer therapy has attracted a lot of interest. The mechanisms of action of most organometallic complexes are poorly understood. Objective: This study was designed to explore the mechanisms governing the anti-proliferative effect of the free ligand N1,N6‐bis((2‐hydroxynaphthalin‐1‐yl)methinyl)) adipohydrazone (H2L) and its complexes of Mn(II), Co(II), Ni(II) and Cu(II). Methods: Cells were exposed to H2L or its metal complexes where cell viability determined by MTT assay. Cell cycle was analysed by flow cytometry. In addition, qRT-PCR was used to monitor the expression of Bax and Bcl-2. Moreover, molecular docking was carried out to find the potentiality of Cu(II) complex as an inhibitor of Adenosine Deaminase (ADA). ADA, Superoxide Dismutase (SOD) and reduced Glutathione (GSH) levels were measured in the most affected cancer cell line. Results: The obtained results demonstrated that H2L and its Cu(II) complex exhibited a strong cytotoxic activity compared to other complexes against HepG2 cells (IC50 = 4.14±0.036μM/ml and 3.2±0.02μM/ml), respectively. Both H2L and its Cu(II) complex induced G2/M phase cell cycle arrest in HepG2 cells. Additionally, they induced apoptosis in HepG2 cells via upregulation of Bax and downregulation of Bcl-2. Interestingly, the activity of ADA was decreased by 2.8 fold in HepG2 cells treated with Cu(II) complex compared to untreated cells. An increase of SOD activity and GSH level in HepG2 cells compared to control was observed. Conclusion: The results concluded that Cu(II) complex of H2L induced apoptosis in HepG2 cells. Further studies are needed to confirm its anti-cancer effect in vivo.


1967 ◽  
Vol 13 (3) ◽  
pp. 215-219 ◽  
Author(s):  
Karel P M Heirwegh ◽  
Johan Fevery

Abstract A sensitive and accurate method is described for the determination of N-acetyl-p-aminophenol (NAPA) and its metabolites in urine and serum. In strongly acidic medium, p-aminophenol (PAP) resulting from differential extraction and acid hydrolysis of total NAPA and unconjugated NAPA, is diazotized and the diazonium salt coupled with N-(1-naphthyl)ethylenediamine (NED) in the presence of ethanol. The blue azo dye formed is determined spectrophotometrically. Application to liver disease is briefly reported.


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