This document summarizes the preparation, characterization, and antimicrobial activities of mixed ligand complexes of Fe(II), Co(II), Ni(II), Cu(II), and Zn(II) with a Schiff base ligand derived from cephalexin drug and 4(dimethylamino)benzaldehyde combined with nicotinamide. The ligand and complexes were characterized using various analytical techniques. The complexes were found to be non-electrolytes with octahedral geometry. Antimicrobial testing showed the complexes had antibacterial activity against Staphylococcus aureus and Escherichia coli.
Synthesis, structural characterization and biological activity of Cu(II), Co(...IJAEMSJORNAL
A novel series of metal complexes of 2-(thiazol-2-ylimino) thiazolidin-4-one ligand were prepared; the corresponding ligand was synthesized from reaction 2-Chloro-N-(thiazol-2-yl) acetamide with ammonium thiocyanate. The complexes are characterized by FTIR, UV-Vis, molar conductance and mass spectroscopy. The low molar conductance values indicate that the complexes are non-electrolytes.Spectroscopic studies confirmed that the ligand bonded to the metals through the sulphur atoms. Coordination number of copper and nickel complexes is four with square planar geometry, while the cobalt complex has octahedral geometry.In vitro antibacterial activity of ligand and its metal complexes was evaluated using well diffusion method and compared to the standard drug (tetracycline). The antibacterial activitywas examined against Escherichia coli, and pseudomonas aeruginosa, as gram negative bacteria and Staphylococcus aureus as gram positive bacteria. It was found that Nickel complex has the highest antibacterial activity among the synthesized compounds with Zone inhibition diameter in the range 25-29 mm.
Mixed Ligand, Palladium(II) and Platinum(II) Complexes of Tertiary Diphosphin...Karwan Omer
Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary
diphosphinesdppm. dppp and dppf with Thioester ligand S-1H benzo[d] imidazole-2-yl benzothioate
(HSBIBT) have been prepared by the reaction of PdCl2 and PtCl2 with one equiv of tertiary
diphosphines ligands to form [Pd(k2-dppf)Cl2], [Pd(k2-dppp)Cl2] and [Pt(k2-dppmCl)Cl2] complexes
and then add the ligand HSBIBT to these complexes to form mixed ligand complexes. The prepared
complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, magnetic
susceptibility, molar conductance, IR spectral data and UV-Visible. The results suggested that the
ligand HSBIBT bonded to the metal through N atom and square planner geometries were assigned
for the complexes.
SYNTHESIS AND CHARACTERIZATION OF SCHIFF BASE METAL COMPLEXES DERIVED FROM NA...chemsurya
New Schiff base metal complexes having general structural formulae ML2Cl2 where M= Co(II), Ni(II) and Cu(II), and MLCl2 where M=Zn(II), Cd(II) and Hg(II) were synthesized by the condensation of indoline-2,3-dione (Isatin) and naphtho[2,1-b]furan-2-carbohydrazide. Tentative structures for the synthesized compounds have been elucidated based on analytical, IR, 1HNMR, and Mass spectral studies. Further selected compounds were tested for their antimicrobial activity.
METALLO - BIOACTIVE COMPOUNDS AS POTENTIAL NOVEL ANTICANCER THERAPYijac123
Mono and bi-organometallic complexes of Cu(II), Ni(II), Mn(II), Zn(II) and Ag(I) complexes with
oxaloamide ligand has much potential as therapeutic and diagnostic agents. The ligand allows the
thermodynamic and kinetic reactivity of the metal ion to be controlled and also provide a scaffold for
functionalization. Specific examples involving the design of metal complexes as anticancer agents are
discussed. These complexes have been synthesized and characterized by (1H-NMR, mass, IR, UV-VIS,
ESR) spectra, magnetic moments and conductance measurements, elemental and thermal analyses. Molar
conductances in DMF solution indicates that, the complexes are non-electrolytes. The ESR spectra of solid
Cu(II) complexes (2-5) show an axial type indicating a d(X2-y2) ground state with a significant covalent
bond character. However, Mn(II) complex(9), shows an isotropic type indicating an octahedral geometry.
Cytotoxic evolution IC50 of the ligand and its complexes have been carried out. Cu(II) Complexes show
enhanced activity in comparison to the parent ligand or standard drug. Copper is enriched in various
human cancer tissues and is a co-factor essential for tumor angiogenesis processes. However, the use of
copper binding ligand to target tumor, copper could provide a novel strategy for cancer selective
treatment.
Synthesis, structural characterization and biological activity of Cu(II), Co(...IJAEMSJORNAL
A novel series of metal complexes of 2-(thiazol-2-ylimino) thiazolidin-4-one ligand were prepared; the corresponding ligand was synthesized from reaction 2-Chloro-N-(thiazol-2-yl) acetamide with ammonium thiocyanate. The complexes are characterized by FTIR, UV-Vis, molar conductance and mass spectroscopy. The low molar conductance values indicate that the complexes are non-electrolytes.Spectroscopic studies confirmed that the ligand bonded to the metals through the sulphur atoms. Coordination number of copper and nickel complexes is four with square planar geometry, while the cobalt complex has octahedral geometry.In vitro antibacterial activity of ligand and its metal complexes was evaluated using well diffusion method and compared to the standard drug (tetracycline). The antibacterial activitywas examined against Escherichia coli, and pseudomonas aeruginosa, as gram negative bacteria and Staphylococcus aureus as gram positive bacteria. It was found that Nickel complex has the highest antibacterial activity among the synthesized compounds with Zone inhibition diameter in the range 25-29 mm.
Mixed Ligand, Palladium(II) and Platinum(II) Complexes of Tertiary Diphosphin...Karwan Omer
Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary
diphosphinesdppm. dppp and dppf with Thioester ligand S-1H benzo[d] imidazole-2-yl benzothioate
(HSBIBT) have been prepared by the reaction of PdCl2 and PtCl2 with one equiv of tertiary
diphosphines ligands to form [Pd(k2-dppf)Cl2], [Pd(k2-dppp)Cl2] and [Pt(k2-dppmCl)Cl2] complexes
and then add the ligand HSBIBT to these complexes to form mixed ligand complexes. The prepared
complexes have been characterized by single-crystal X-ray diffraction, elemental analysis, magnetic
susceptibility, molar conductance, IR spectral data and UV-Visible. The results suggested that the
ligand HSBIBT bonded to the metal through N atom and square planner geometries were assigned
for the complexes.
SYNTHESIS AND CHARACTERIZATION OF SCHIFF BASE METAL COMPLEXES DERIVED FROM NA...chemsurya
New Schiff base metal complexes having general structural formulae ML2Cl2 where M= Co(II), Ni(II) and Cu(II), and MLCl2 where M=Zn(II), Cd(II) and Hg(II) were synthesized by the condensation of indoline-2,3-dione (Isatin) and naphtho[2,1-b]furan-2-carbohydrazide. Tentative structures for the synthesized compounds have been elucidated based on analytical, IR, 1HNMR, and Mass spectral studies. Further selected compounds were tested for their antimicrobial activity.
METALLO - BIOACTIVE COMPOUNDS AS POTENTIAL NOVEL ANTICANCER THERAPYijac123
Mono and bi-organometallic complexes of Cu(II), Ni(II), Mn(II), Zn(II) and Ag(I) complexes with
oxaloamide ligand has much potential as therapeutic and diagnostic agents. The ligand allows the
thermodynamic and kinetic reactivity of the metal ion to be controlled and also provide a scaffold for
functionalization. Specific examples involving the design of metal complexes as anticancer agents are
discussed. These complexes have been synthesized and characterized by (1H-NMR, mass, IR, UV-VIS,
ESR) spectra, magnetic moments and conductance measurements, elemental and thermal analyses. Molar
conductances in DMF solution indicates that, the complexes are non-electrolytes. The ESR spectra of solid
Cu(II) complexes (2-5) show an axial type indicating a d(X2-y2) ground state with a significant covalent
bond character. However, Mn(II) complex(9), shows an isotropic type indicating an octahedral geometry.
Cytotoxic evolution IC50 of the ligand and its complexes have been carried out. Cu(II) Complexes show
enhanced activity in comparison to the parent ligand or standard drug. Copper is enriched in various
human cancer tissues and is a co-factor essential for tumor angiogenesis processes. However, the use of
copper binding ligand to target tumor, copper could provide a novel strategy for cancer selective
treatment.
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
A new Schiff base 4-chlorophenyl)methanimine
(6R,7R)-3-methyl-8-oxo-7-(2-phenylpropanamido)-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylate= (HL)= C23H20
ClN3O4S) has been synthesized from β-lactam antibiotic
(cephalexin mono hydrate(CephH)=(C16H19N3O5S.H2O) and 4-
chlorobenzaldehyde . Figure(1) Metal mixed ligand complexes
of the Schiff base were prepared from chloride salt of
Fe(II),Co(II),Ni(II),Cu(II),Zn(II) and Cd (II), in 50% (v/v)
ethanol –water medium (SacH ) .in aqueous ethanol(1:1)
containing and Saccharin(C7H5NO3S) = sodium hydroxide.
Several physical tools in particular; IR, CHN, 1H NMR, 13C
NMR for ligand and melting point molar conductance, magnetic
moment. and determination the percentage of the metal in the
complexes by flame(AAS). The ligands and there metal
complexes were screened for their antimicrobial activity against
four bacteria (gram + ve) and (gram -ve) {Escherichia coli,
Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus}.
The proposed structure of the complexes using program, Chem
office 3D(2006). The general formula have been given for the
prepared mixed ligand complexes Na2[M(Sac)3(L)], M(II) = Fe
(II), Co(II) , Ni(II), Cu (II), Zn(II) , and Cd(II).
HL= C29H24 ClN3O4S, L= C29H23 ClN3O4S -.
Antibacterial Application of Novel Mixed-Ligand Dithiocarbamate Complexes of ...IOSR Journals
Nine stable mixed ligand dithiocarbamate complexes of Nickel (II) ion were prepared. The complexes were characterized with electronic spectroscopy, infrared spectroscopy, conductance measurement, melting point and percentage metal analysis. Resulting analytical data gave credence to the assignment of a tentative square planar geometry to all the complexes. The complexes were proposed to have a general formulae of [Ni(Sal)(Rdtc)], where Sal = salicylaldehyde; R = dibenzylamine(Bz2NH), methylphenylamine(MePhNH),pyrrolidineamine(pyrrolNH),piperidineamine(piperNH),morpholineamine(MorpNH), anilineamine(AnilNH), para-chloroanilineamine(p-ClAnilNH), toludineamine(TolNH) and anisidineamine(AnisNH); and dtc = dithiocarbamate anion. The metal complexes were screened against six different bacteria strain using Agar diffusion method. The antibacterial studies reveal that the metal complexes exhibit broad spectrum antibacterial activity against Escherichia coli, Staphylococcus aureus, Klebsiella oxytoca and Pseudomonas aureginosa with inhibitory range of 10.5.—20.0mm.
Synthesis, Characterization, Antibacterial and DNA Binding Studies of Mn (II)...IOSRJAC
Mn (II) complex of the Schiff base (L), 3-(2-(2-hydroxy-3-methoxybenzylidene) hydrazinyl) quinoxalin-2(1H)-one (VHQO) was prepared and characterized by IR, UV-VIS, Mass, Elemental analysis, TGDTA, magnetic susceptibility and conductivity measurements. VHQO behaved as monobasic, tridentate ligand and formed 1:2 complex (ML2) with the metal ion (M) coordinating through ring nitrogen, azomethine nitrogen and phenolic oxygen. Thermal analysis of the complex indicated the absence of lattice and coordinated water. Based on the spectral and analytical data, octahedral geometry was assigned to the complex. Antibacterial activity of the complex against gram positive bacteria, Bacillus subtillis, Staphylococcus aureus, and gram negative bacteria, Escherichia coli, Proteus vulgaris, Pseudomonas aeroginosa , and Klebsiella pneumonia was studied. The interaction of the complex with Calf Thymus DNA (CT-DNA) was studied by absorption spectroscopy and the intrinsic binding constant was calculated.
Synthesis and Characterization of Schiff Base from Aromatic Amine and Aromati...ijtsrd
The synthesis of Schiff base From Aromatic Amine And Aromatic P Nitro benzaldehyde was performed by a novel method of stirring followed by the addition of p nitro benzaldehydeandm nitro aniline 0.02M . Characterization of the synthesized compounds, determination of purity and identity of the compounds using following spectroscopic and chromatographic techniques Solubility, Thin Layer Chromatographic studies, Ultra Violet studied rotational and vibrational studies FT IR studies. The compounds were investigated for their Antimicrobial activity by cup plate method. Compound1 nitro 4 1 imino,4 nitrophenyl benzene was found to be the most active according to pharmacological evaluation exhibited antimicrobial. Ms. Chetana D. Patil | Mr. Digamber N. Bhosale | Ms. Smita P. Bedis "Synthesis and Characterization of Schiff Base from Aromatic Amine and Aromatic P-Nitro Benzaldehyde" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-5 , August 2019, URL: https://www.ijtsrd.com/papers/ijtsrd26401.pdfPaper URL: https://www.ijtsrd.com/pharmacy/medicinal-chemistry/26401/synthesis-and-characterization-of-schiff-base-from-aromatic-amine-and-aromatic-p-nitro-benzaldehyde/ms-chetana-d-patil
New Schiff base ligand (E)-6-(2-(4-
(dimethylamino)benzylideneamino)-2-phenylacetamido)-3,3-
dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic
acid = (HL) Figure(1) was prepared via condensation of
Ampicillin and 4(dimethylamino)benzaldehyde in methanol
.Polydentate mixed ligand complexes were obtained from 1:1:2
molar ratio reactions with metal ions and HL, 2NA on reaction
with MCl2 .nH2O salt yields complexes corresponding to the
formulas [M(L)(NA)2Cl] ,where M =
Fe(II),Co(II),Ni(II),Cu(II),and Zn(II) and NA=nicotinamide.
The 1H-NMR, FT-IR, UV-Vis and elemental analysis
were used for the characterization of the ligand. The complexes
were structurally studied through AAS, FT-IR, UV-Vis,
chloride contents, conductance, and magnetic susceptibility
measurements. All complexes are non-electrolytes in DMSO
solution. Octahedral geometries have been suggested for each
of the complexes. The Schiff base ligands function as
tridentates and the deprotonated enolic form is preferred for
coordination. In order to evaluate the effect of the bactericidal
activity, these synthesized complexes, in comparison to the un
complexed Schiff base has been screened against bacterial
species, Staphy
Role of mixed ligand Pd(II) and Pt(II)complexes in photooxygenation reactionIOSR Journals
Mixed ligand complexes of the formula [M (phen) bdt] where M= Pd (II) or Pt(II), phen =1,10-phenanthroline and bdt =1,2-benzenedithiolate have been synthesized and studied as photosensitizers of singlet molecular oxygen (1O2) production. It was observed that, Pt (II) complex shows a better photosensitizing ability as compared to its Pd (II) analogue. However, both Pd (II) and Pt (II) complexes act as chemical quenchers of 1O2, resulting in their photooxidation shown by decay of the respective complex. ThusPt (II) complex undergoes selfsensitizedphotooxidation by 1O2. The solvent dependence of this reaction is undertaken by performing the experiment using pure DMF(dimethyl formamide)and 10% H2O in DMF as solvent. The comparison of rate of decay of the Pt(II)and Pd(II) complexes show enhancement of the reaction in presence of water. The decay of the complex was monitored by recording the difference absorption spectra of the complex in the visible region after definite irradiation times. Involvement of 1O2 is further supported by quenching studies of this reaction using NaN3 as physical quencher of 1O2.
Synthesis and Crystal Structure of Anickel (II) and Zinc (II) Complex From 1,...IOSRJAC
:The title mononuclear nickel and zinc complexes, Ni(C11H9N4S3)2andZn(C11H9N4S3)2 .2(C3H7NO), were prepared by the reaction of Nickel(II) or Zinc(II)acetate with 1,5-bis[(2- thiophenyl)methylidene]thiocarbonohydrazide in a methanol solution. It features mono-deprotonated bisbidentate ligands, which coordinate to metal (II) ions by hydrazylN and thiocarbony lS atoms, yielding a tetracoordinated metal ions complexes. In Ni(II) complex the geometry around the metal ion is described as square planar. In the Zn(II) the metal atom shows severely tetrahedral distortion from anideal square-planar coordination geometry, as reflected by the dihedral angle between ZnN2and ZnS2 planes of 73.03(13)°. Two intramolecular hydrogen bonds are observed between the solvate dmf molecules and the coordinated ligands:N2—H2N…O1i and N6—H6N…O2 ii in this complex
Synthesis and characterization of mixed ligand complexes of some metals with ...Taghreed Al-Noor
This paper presents the synthesis and study of some new mixed-liagnd complexes containing nicotinamide(C6H7N2O) symbolized (NA) and phenylalanine (C9H11NO2)symbolized (pheH)] with some metal ions.
The resulting products were found to be solid crystalline complexes which have been characterized by :Melting points, Solubility, Molar conductivity.
determination the percentage of the metal in the complexes by flame(AAS), magnetic susceptipibility, Spectroscopic Method [FT-IR and UV-Vis].
The proposed structure of the complexes using program , chem office 3D(2006) .
The general formula have been given for the prepared complexes :[M(NA)2(phe)]cl
M(II): Mn(II) ,Co(II) , Ni(II) , Cu(II) , Zn(II) , Cd(II) & Hg(II) .
NA = Nicotinamide= C6H7N2O
Phe - = phenylalanine ion = C9H10NO2
Design, Synthesis and Structural Inspection of Some Novel Di- And Tri-Azometh...CrimsonPublishersACSR
In this study, NBA imine compound was synthesized via an easy one-pot condensation of 3-nitro-benzaldyhide with 2-amino benzoic acid in 1:1 ratio and DAPH imine compound derived from 2,6-diacetyl pyridine and phenyl hydrazine hydrochloride. Consequences of the newly synthesized compounds
hooked up with the aid of FT-IR, elemental analyses, 13C-NMR ,1H-NMR and digital spectral research.
Experiments had been consistent with their chemical structures. Theoretical DFT calculations had been
implemented to confirm the molecular geometry of the investigated chemo-sensors. The sensor property
of all organized imines had been tested upon addition of the metal ions, consisting of Cr(III) ,Fe(II) ,Co(II) ,
Ni(II) ,Cu(II) ,Zn(II) ,Mn(II), VO(II) and Pd(II) .The interactions among receptors and ions are effortlessly
monitored with the aid of UV-visible spectroscopy. DAPH receptor confirmed color modification from
blood red to excessive deep green color to Co(II) ,a yellow color to Cu(II) and different colors to different
ions. Where the NBA receptor showed color modification from light yellow to excessive deep orange color
to Fe(II), pale orange to Pd(II) and different colors for other ions.
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
A new Schiff base 4-chlorophenyl)methanimine
(6R,7R)-3-methyl-8-oxo-7-(2-phenylpropanamido)-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylate= (HL)= C23H20
ClN3O4S) has been synthesized from β-lactam antibiotic
(cephalexin mono hydrate(CephH)=(C16H19N3O5S.H2O) and 4-
chlorobenzaldehyde . Figure(1) Metal mixed ligand complexes
of the Schiff base were prepared from chloride salt of
Fe(II),Co(II),Ni(II),Cu(II),Zn(II) and Cd (II), in 50% (v/v)
ethanol –water medium (SacH ) .in aqueous ethanol(1:1)
containing and Saccharin(C7H5NO3S) = sodium hydroxide.
Several physical tools in particular; IR, CHN, 1H NMR, 13C
NMR for ligand and melting point molar conductance, magnetic
moment. and determination the percentage of the metal in the
complexes by flame(AAS). The ligands and there metal
complexes were screened for their antimicrobial activity against
four bacteria (gram + ve) and (gram -ve) {Escherichia coli,
Pseudomonas aeruginosa, Staphylococcus aureus and Bacillus}.
The proposed structure of the complexes using program, Chem
office 3D(2006). The general formula have been given for the
prepared mixed ligand complexes Na2[M(Sac)3(L)], M(II) = Fe
(II), Co(II) , Ni(II), Cu (II), Zn(II) , and Cd(II).
HL= C29H24 ClN3O4S, L= C29H23 ClN3O4S -.
Antibacterial Application of Novel Mixed-Ligand Dithiocarbamate Complexes of ...IOSR Journals
Nine stable mixed ligand dithiocarbamate complexes of Nickel (II) ion were prepared. The complexes were characterized with electronic spectroscopy, infrared spectroscopy, conductance measurement, melting point and percentage metal analysis. Resulting analytical data gave credence to the assignment of a tentative square planar geometry to all the complexes. The complexes were proposed to have a general formulae of [Ni(Sal)(Rdtc)], where Sal = salicylaldehyde; R = dibenzylamine(Bz2NH), methylphenylamine(MePhNH),pyrrolidineamine(pyrrolNH),piperidineamine(piperNH),morpholineamine(MorpNH), anilineamine(AnilNH), para-chloroanilineamine(p-ClAnilNH), toludineamine(TolNH) and anisidineamine(AnisNH); and dtc = dithiocarbamate anion. The metal complexes were screened against six different bacteria strain using Agar diffusion method. The antibacterial studies reveal that the metal complexes exhibit broad spectrum antibacterial activity against Escherichia coli, Staphylococcus aureus, Klebsiella oxytoca and Pseudomonas aureginosa with inhibitory range of 10.5.—20.0mm.
Synthesis, Characterization, Antibacterial and DNA Binding Studies of Mn (II)...IOSRJAC
Mn (II) complex of the Schiff base (L), 3-(2-(2-hydroxy-3-methoxybenzylidene) hydrazinyl) quinoxalin-2(1H)-one (VHQO) was prepared and characterized by IR, UV-VIS, Mass, Elemental analysis, TGDTA, magnetic susceptibility and conductivity measurements. VHQO behaved as monobasic, tridentate ligand and formed 1:2 complex (ML2) with the metal ion (M) coordinating through ring nitrogen, azomethine nitrogen and phenolic oxygen. Thermal analysis of the complex indicated the absence of lattice and coordinated water. Based on the spectral and analytical data, octahedral geometry was assigned to the complex. Antibacterial activity of the complex against gram positive bacteria, Bacillus subtillis, Staphylococcus aureus, and gram negative bacteria, Escherichia coli, Proteus vulgaris, Pseudomonas aeroginosa , and Klebsiella pneumonia was studied. The interaction of the complex with Calf Thymus DNA (CT-DNA) was studied by absorption spectroscopy and the intrinsic binding constant was calculated.
Synthesis and Characterization of Schiff Base from Aromatic Amine and Aromati...ijtsrd
The synthesis of Schiff base From Aromatic Amine And Aromatic P Nitro benzaldehyde was performed by a novel method of stirring followed by the addition of p nitro benzaldehydeandm nitro aniline 0.02M . Characterization of the synthesized compounds, determination of purity and identity of the compounds using following spectroscopic and chromatographic techniques Solubility, Thin Layer Chromatographic studies, Ultra Violet studied rotational and vibrational studies FT IR studies. The compounds were investigated for their Antimicrobial activity by cup plate method. Compound1 nitro 4 1 imino,4 nitrophenyl benzene was found to be the most active according to pharmacological evaluation exhibited antimicrobial. Ms. Chetana D. Patil | Mr. Digamber N. Bhosale | Ms. Smita P. Bedis "Synthesis and Characterization of Schiff Base from Aromatic Amine and Aromatic P-Nitro Benzaldehyde" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-5 , August 2019, URL: https://www.ijtsrd.com/papers/ijtsrd26401.pdfPaper URL: https://www.ijtsrd.com/pharmacy/medicinal-chemistry/26401/synthesis-and-characterization-of-schiff-base-from-aromatic-amine-and-aromatic-p-nitro-benzaldehyde/ms-chetana-d-patil
New Schiff base ligand (E)-6-(2-(4-
(dimethylamino)benzylideneamino)-2-phenylacetamido)-3,3-
dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic
acid = (HL) Figure(1) was prepared via condensation of
Ampicillin and 4(dimethylamino)benzaldehyde in methanol
.Polydentate mixed ligand complexes were obtained from 1:1:2
molar ratio reactions with metal ions and HL, 2NA on reaction
with MCl2 .nH2O salt yields complexes corresponding to the
formulas [M(L)(NA)2Cl] ,where M =
Fe(II),Co(II),Ni(II),Cu(II),and Zn(II) and NA=nicotinamide.
The 1H-NMR, FT-IR, UV-Vis and elemental analysis
were used for the characterization of the ligand. The complexes
were structurally studied through AAS, FT-IR, UV-Vis,
chloride contents, conductance, and magnetic susceptibility
measurements. All complexes are non-electrolytes in DMSO
solution. Octahedral geometries have been suggested for each
of the complexes. The Schiff base ligands function as
tridentates and the deprotonated enolic form is preferred for
coordination. In order to evaluate the effect of the bactericidal
activity, these synthesized complexes, in comparison to the un
complexed Schiff base has been screened against bacterial
species, Staphy
Role of mixed ligand Pd(II) and Pt(II)complexes in photooxygenation reactionIOSR Journals
Mixed ligand complexes of the formula [M (phen) bdt] where M= Pd (II) or Pt(II), phen =1,10-phenanthroline and bdt =1,2-benzenedithiolate have been synthesized and studied as photosensitizers of singlet molecular oxygen (1O2) production. It was observed that, Pt (II) complex shows a better photosensitizing ability as compared to its Pd (II) analogue. However, both Pd (II) and Pt (II) complexes act as chemical quenchers of 1O2, resulting in their photooxidation shown by decay of the respective complex. ThusPt (II) complex undergoes selfsensitizedphotooxidation by 1O2. The solvent dependence of this reaction is undertaken by performing the experiment using pure DMF(dimethyl formamide)and 10% H2O in DMF as solvent. The comparison of rate of decay of the Pt(II)and Pd(II) complexes show enhancement of the reaction in presence of water. The decay of the complex was monitored by recording the difference absorption spectra of the complex in the visible region after definite irradiation times. Involvement of 1O2 is further supported by quenching studies of this reaction using NaN3 as physical quencher of 1O2.
Synthesis and Crystal Structure of Anickel (II) and Zinc (II) Complex From 1,...IOSRJAC
:The title mononuclear nickel and zinc complexes, Ni(C11H9N4S3)2andZn(C11H9N4S3)2 .2(C3H7NO), were prepared by the reaction of Nickel(II) or Zinc(II)acetate with 1,5-bis[(2- thiophenyl)methylidene]thiocarbonohydrazide in a methanol solution. It features mono-deprotonated bisbidentate ligands, which coordinate to metal (II) ions by hydrazylN and thiocarbony lS atoms, yielding a tetracoordinated metal ions complexes. In Ni(II) complex the geometry around the metal ion is described as square planar. In the Zn(II) the metal atom shows severely tetrahedral distortion from anideal square-planar coordination geometry, as reflected by the dihedral angle between ZnN2and ZnS2 planes of 73.03(13)°. Two intramolecular hydrogen bonds are observed between the solvate dmf molecules and the coordinated ligands:N2—H2N…O1i and N6—H6N…O2 ii in this complex
Synthesis and characterization of mixed ligand complexes of some metals with ...Taghreed Al-Noor
This paper presents the synthesis and study of some new mixed-liagnd complexes containing nicotinamide(C6H7N2O) symbolized (NA) and phenylalanine (C9H11NO2)symbolized (pheH)] with some metal ions.
The resulting products were found to be solid crystalline complexes which have been characterized by :Melting points, Solubility, Molar conductivity.
determination the percentage of the metal in the complexes by flame(AAS), magnetic susceptipibility, Spectroscopic Method [FT-IR and UV-Vis].
The proposed structure of the complexes using program , chem office 3D(2006) .
The general formula have been given for the prepared complexes :[M(NA)2(phe)]cl
M(II): Mn(II) ,Co(II) , Ni(II) , Cu(II) , Zn(II) , Cd(II) & Hg(II) .
NA = Nicotinamide= C6H7N2O
Phe - = phenylalanine ion = C9H10NO2
Design, Synthesis and Structural Inspection of Some Novel Di- And Tri-Azometh...CrimsonPublishersACSR
In this study, NBA imine compound was synthesized via an easy one-pot condensation of 3-nitro-benzaldyhide with 2-amino benzoic acid in 1:1 ratio and DAPH imine compound derived from 2,6-diacetyl pyridine and phenyl hydrazine hydrochloride. Consequences of the newly synthesized compounds
hooked up with the aid of FT-IR, elemental analyses, 13C-NMR ,1H-NMR and digital spectral research.
Experiments had been consistent with their chemical structures. Theoretical DFT calculations had been
implemented to confirm the molecular geometry of the investigated chemo-sensors. The sensor property
of all organized imines had been tested upon addition of the metal ions, consisting of Cr(III) ,Fe(II) ,Co(II) ,
Ni(II) ,Cu(II) ,Zn(II) ,Mn(II), VO(II) and Pd(II) .The interactions among receptors and ions are effortlessly
monitored with the aid of UV-visible spectroscopy. DAPH receptor confirmed color modification from
blood red to excessive deep green color to Co(II) ,a yellow color to Cu(II) and different colors to different
ions. Where the NBA receptor showed color modification from light yellow to excessive deep orange color
to Fe(II), pale orange to Pd(II) and different colors for other ions.
International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis and Characterization of Thermal Analysis of La (Ii) Macrocyclic Com...inventionjournals
The macrocyclic complex compounds of La(II) containing a ligand having tetraoxotetrahydrazin moity are synthesized by template condensation of malonodihydrazide (C3H8N4O2) with different aldehydes. The complexes are characterized on the basis of elemental analysis, UV-visible & IR spectroscopy, magnetic moment and conductance measurement and other physical properties.Antibacterial activity of the derived complex compounds, as well as already used standard compound kanamycin, was tested on fourteen pathogenic bacteria. Given results were then compared to the efficacy of the Antibacterial activity of standard compound kanamycin used for control of these pathogenic bacteria.
Synthesis, Characterization and antimicrobial activity of some novel sulfacet...iosrjce
IOSR Journal of Applied Chemistry (IOSR-JAC) is a double blind peer reviewed International Journal that provides rapid publication (within a month) of articles in all areas of applied chemistry and its applications. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Chemical Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
Chelation Trends and Antibacterial Activity of Some Mixed Ligand ChelatesTaghreed Al-Noor
Synthesis and investigation of new Co(II), Ni(II), Cu(II), Zn(II) and Cr(III)chelates of mixed ligands including
aSchiff base [(E)-2-(4-(dimethylamino)benzylideneamino)phenol] (C15H16N2O) derived from the condensation of 4-
dimethylaminobenzaldehyde with 2-aminophenol as main ligand (L1) and an amino acid; L-Histidine as co-ligand (L2)
were studied. The obtained Schiff base and the mixed ligand chelates were subjected to several physiochemical
techniques, in terms of CHN elemental analyses, molar conductivity, magnetic moment measurements, infrared,
electronic and mass spectroscopies. The CHN analytical data showed the formation of the Schiff base compound and the
mixed ligand chelates in 1:1:1[M:L1:L2] ratio. All the prepared mixed ligand chelates were non-electrolyte in nature.
The infrared spectral data exhibited that the used ligands behaving as bidentate ligands towards the metal ions. The
1HNMR spectra of the ligands and their Zn(II) mixed ligand chelate exhibited the effect of the activated groups of the
ligands by the metal ion. The electronic spectral results showed the existence of π→π* (phenyl ring) and n→π*(HC=N)
and suggested the geometrical structures of the chelates. Meanwhile, the mass spectral data revealed the fragmentations
of the Schiff base, Histidine and their Cu(II) mixed ligand chelate. The studies made on these chelates proposed a six
coordinated octahedral geometry for all these chelates. The antibacterial activities of the Schiff base, Histidine, metal
salts and mixed ligand chelates were screened. It is found that the mixed ligand chelates have the most biological activity
in comparison to the free ligands and salts.
Keywords: Schiff base; 4-dimethylaminobenzaldehyde; 2-aminophenol; Histidine; mixed ligand chelates;
Physiochemical techniques; Antibacterial activity.
Synthesis, spectroscopic, electrochemical, magnetic properties and super oxid...IOSR Journals
Five new mixed-ligand nickel (II) complexes; viz; [Ni (BHM)(PMDT)]1; [Ni(BHM)(dien)] 2; [Ni(BHM)(L1)]3; [Ni(BHM)(L2)] 4, [Ni(BHM)(L3)] 5; where H2BHM= N’-(1E)-(5-bromo-2-hydroxyphenyl) methylidene] benzoylhydrazide, PMDT= N,N,N’,N,”N”-Pentamethyldiethylenetriamine; dien= diethylenetriamine; L1 = N,N- dimethyl-N’ (Pyrid-2-yl-methyl) ethylenediamine; L2= N-methyl-N’-(pyrid-2-ylmethyl)ethylenediamine; L3 = N,N-dimethyl-N’-(6-methyl)pyrid-2-ylmethyl) ethylenediamine, have been synthesized and characterized by using elemental analyses, FAB (fast atomic bombardment), magnetic measurements, electronic absorption , conductivity measurements, cyclic voltammetry (CV) and IR- spectroscopy . All the complexes yielded an irreversible couple that can be assigned to a NiII→ NiI redox process. Infrared spectra, ligand field spectra and magnetic susceptibility measurements agree with the observed octahedral environment. H2BHM is a diprotic tridentate Schiff base ligand (ONO donor atom) whereas L1-L3 possessing N3 coordination sites. The SOD activities have been measured using alkaline DMSO as a source of superoxide radical (O2–) and nitro blue tetrazolium (NBT) as O2– scavenger.
International Journal of Engineering and Science Invention (IJESI)inventionjournals
International Journal of Engineering and Science Invention (IJESI) is an international journal intended for professionals and researchers in all fields of computer science and electronics. IJESI publishes research articles and reviews within the whole field Engineering Science and Technology, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis, Physicochemical Characterization and Structure Determination of So...IOSR Journals
Some novel nickel(II) complexes with the ligand (z)-4-((2-hydroxy-3-
methoxyphenyl)diazenyl)-1,5-dimethyl-2-phenyl-1H-pyrazol-3-(2H)-one,GAAP,guiacolazoantipyrine, L
having molecular formulae [Ni(L)2X2] and [Ni(L)2(NCS)Cl] where X = Cl-, Br-, NO3
- were synthesized and
characterized. The elemental analysis, Spectral (IR, UV-Visible, EPR, FAB – mass) studies and thermo
gravimetric analysis reveals that the Ni(II) is six coordinated in its complexes. A rhombic symmetry can be
tentatively proposed for the complexes. The magnetic susceptibility measurements show that the complexes are
paramagnetic in nature. The powder XRD study shows its anisotropic nature
Shanghai ranking's global ranking of academic subjects 2020 chemistry convertedTaghreed Al-Noor
Shanghai Ranking's Global Ranking of Academic Subjects 2020 – Chemistry
http://www.shanghairanking.com/Shanghairanking-Subject-Rankings/chemistry.html
2020 تصنيف شنغهاي للجامعات حسب الموضوع – الكيمياء
Shanghai Ranking's Global Ranking of Academic Subjects 2020 Chemistry
prof .Taghreed H Al-Noor أ. د تغريد هاشم النور
جامعة بغداد University of Baghdad
that causes COVID-19 is called SARS-CoV
2020 - www.compoundchem.com @
prof .Taghreed H Al-Noor أ.د تغريد هاشم النور
University of Baghdad,Chair ACS Iraq chapter
Virtual International Scientific Conference Curriculum The Role Of Higher Education And Scientific Research Formations And National Institutions In Confronting The Corona Pandemic Forensic DNA Center for Research and Training / Al-Nahrain University .American Chemical Society ACS and its role in confronting Corona pandemic )
Prof. Taghreed Hashim Al.Noor Chairman chapter Iraq of the American Chemical Society
Asian Journal of Biochemistry is an International peer-reviewed journal dedicated to publish the results of original research in form of original articles, reviews and short communications. Scope of the journal includes: Structure, function and regulation of biologically active molecules; gene structure and expression; biochemical mechanisms; protein biosynthesis; protein folding; membrane structure-function relationships; bioenergetics and immunochemistry. Asian Journal of Biochemistry now accepting new submissions. Submit your next paper via online submission system.
ACS Iraq chapter
Supported
45Mins5th International Turkic World
Conference on Chemical Sciences and
Technologies (ITWCCST 2019)” which will take place in Sakarya,
Turkey between 25-29 October 2019.
1SecondScientific Committee
Taghreed H AL-NOOR
University of Baghdad, Iraq chair ACS IRAQ member in
http://2019.itwccst.org/?page_id=149
Catalysis, chemical engineering 2019 taghreed al noorTaghreed Al-Noor
Synthesis, spectroscopic characterization, biological Activity and dye on
cotton fabric of mixed ligand metal complexes derived From curcumin and Lphenyl alanine, schiff Base and anthranilic acid
DFT, cytotoxicity and molecular docking studies of (E)-2((2- hydroxybenzylide...Taghreed Al-Noor
Kathmandu Symposia on Advanced Materials (KaSAM)-2018; October 26-29, 2018, Kathmandu, Nepal
DFT, cytotoxicity and molecular docking studies of (E)-2((2-
hydroxybenzylidene) amino-3-mercaptopropanoic acid and its Co(II),
Ni(II) and Cu(II) complexes
M.M. El-ajaily1*, S.S. Mahmoud2, R.N. El-daghare1, A.K. Sarangi3, R.K. Mohapatra3* and T.H.
Al-Noor4
1Chemistry Department, Faculty of Science, Benghazi University, Benghazi, Libya
2Chemistry department, Faculty of Science, Cairo University, Giza, Egypt
3Department of Chemistry, Government College of Engineering, Keonjhar, Odisha, India
4Chemistry Department, Ibn-Al-Haithem College of Education for Pure Science, Baghdad University,
Baghdad, Iraq
*E-mail: ranjank_mohapatra@yahoo.com
The cytotoxicity studies of a Schiff base; (E)-2((2-hydroxybenzylidene)amino-3-mercaptopropanoic acid
(HL) derived from the condensation of 2-hydroxybenzaldehyde and L-cysteine and its Co(II), Ni(II)
and Cu(II) complexes have been reported against four cancer cell lines. The evaluation of the growth
inhibitory on human cancer cells is studied for the chelates against HCT-116, MCF-7, HFB-4,
HepG-2 cell lines. The obtained results (Fig. 1) revealed that the compounds are active against human
hepatocellular carcinoma cell line (HepG-2).
Scimago journal & country rank taghreed al noorTaghreed Al-Noor
Scimago Journal & Country Rank
ترتيب الدول من ناحية نشر الباحثين في المجلات العالمية المصنفة و
H index جودة البحوث من خلال عدد الاقتباسات
حسب موقع
)SJR (Scimago Journal Rank الترتيب خاص بسنة 201
ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society ACS GCCE Chemical Society Capacity Building Workshop Capacity Building Workshop Capacity Building Workshop Capacity Building Workshop Capacity Building Workshop Capacity Building Workshop Capacity Building Workshop 14 -18 October, 2018 October, 2018October, 2018 October, 2018
•
Anthranillic acid and tributylphosphine4652 6725-1-pbTaghreed Al-Noor
Mixed ligand complexes of bivalent metal ions, viz; Co(II), Ni(II), Cu(II) and Zn(II) of the
composition [M(A)2((PBu3)2]in(1:2:2)(M:A:(PBu3). molar ratio, (where A- Anthranilate ion
,(PBu3)= tributylphosphine. M= Co(II),Ni(II),Cu(II) and Zn(II).
The prepared complexes were characterized using flame atomic absorption, by FT-IR,
UV/visible spectra methods as well as magnetic susceptibility and conductivity measurements. The
metal complexes were tested in vitro against three types of pathogenic bacteria microorganisms:
(Staphylococcus, Klebsiella SPP .and Bacillas)to assess their antimicrobial properties. Results. The
study shows that all complexes have octahedral geometry; in addition, it has high activity against
tested bacteria. Based on the reported results, it may be concluded that.The results showed that the
deprotonated ligand(nthranilc acid ) to anthranilate ion (A-) by using (KOH) coordinated to metal
ions as bidentate ligand through the oxygen atom of the carboxylate group (−COO−), and the
nitrogen atom of the amine group (-NH2), where the Tributylphosphine coordinated as a
3rd Internatioanl Medical Congress, will be hold in Kerbala, Iraq in 14-15 De...Taghreed Al-Noor
3rd Internatioanl Medical Congress, will be hold in Kerbala, Iraq in 14-15 December 2018 by Nab'a Al-Hayat Foundation for Medical Sciences and Health Care, and in collaboration with (University of Kerbala, University of Kufa, Directory of Research -Ministry of Health Oman, University of Sussex, University of Komar, University of Diyala, University of Qaddisya, University of Al-Anbar, University of Al-Mustansariya and Helal Iran Pharmaceutical Complex.
Facial Acne Therapy by Using Pumpkin Seed Oil with Its Physicochemical Proper...Taghreed Al-Noor
The herbal remedy individually or in combination with standard medicines has been used in diverse medical treatises for the cure of different diseases. Pumpkin seed oil is one of the recognized edible oil and has substantial medicinal properties due to the presence of unique natural edible substances. Inflammation is an adaptive response that is triggered by noxious stimuli and conditions, which involves interactions amongst many cell types and mediators, and underlies many pathological processes. Unsaturated fatty acids (UFAs) can influence inflammation through a variety of mechanisms, and have been indicated as alternative anti-inflammatory agents to treat several inflammatory skin disorders. Pumpkin seed oil is rich in (UFAs), that its topical anti-inflammatory properties have been investigated. For that reason, the goal of this article was to evaluate the effects of pumpkin seed oil on acute and chronic cutaneous inflammation experimental models. The extracted pumpkin seed oil had an acceptable initial quality, when it was extracted using soxhlet extraction method and was characterized using standard methods .The physicochemical parameters of purified oil were determined. The boiling point of pumpkin seed oil was (158.90 oC) that equal to the values obtained in literature for some oil seeds, but lower than the boiling point of the oils studied, plus the melting point of pumpkin seed oil was (15.39 oC) that lead to a characteristic in cold cream manufacture. The iodine value was (104 ± 0.03 mg of KOH/g) of oil, indicated a high degree of unsaturation. The saponification value was (181± 3.2 mg KOH/g), this value indicated the pumpkin seed oil had fatty acids with higher number of carbon atoms. As a final point, the acid value was
1. Advances in Physics Theories and Applications www.iiste.org
ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)
Vol.18, 2013
1
Preparation , Characterization and Antimicrobial activities of
{Fe(II),Co(II),Ni(II),Cu(II),and Zn(II)}Mixed Ligand Complexes
Schiff base derived from Cephalexin drug and
4(dimethylamino)benzaldehyde with Nicotinamide
Taghreed . H. Al-Noor , Ahmed .T.AL- Jeboori , Manhel Reemon Aziz
Department of Chemistry.Ibn -Al-Haithem College of Education for pure science
Baghdad University-Iraq
Corresponding author: e-mail- taghreedalnoor@yahoo,com
Abstract
New Schiff base ligand (Z)-7-(2-(4-(dimethylamino)benzylideneamino)-2-phenylacetamido)-3-methyl-8-
oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid = (HL)was prepared via condensation of Cephalexin
and 4(dimethylamino)benzaldehyde in methanol . Polydentate mixed ligand complexes were obtained from
1:1:2 molar ratio reactions with metal ions and HL, 2NA on reaction with MCl2 .nH2O salt yields complexes
corresponding to the formulas [M(L)(NA)2Cl] ,where M = Fe(II),Co(II),Ni(II),Cu(II),and Zn(II) and
NA=nicotinamide .
The 1H-NMR, FT-IR, UV-Vis and elemental analysis were used for the characterization of the ligand. The
complexes were structurally studied through AAS, FT-IR, UV-Vis, chloride contents, conductance, and
magnetic susceptibility measurements. All complexes are non-electrolytes in DMSO solution. Octahedral
geometries have been suggested for each of the complexes.
the Schiff base ligands function as tridentates and the deprotonated enolic form is
preferred for coordination. In order to evaluate the effect ofthe bactericidal activity, these synthesized complexes,
in comparison to the uncomplexed Schiff base has been screened against bacterial species., Staphylococcus
aureus,Escherichia coil and the results are reported.
Key words:(Cephalexin drug, Nicotinamide ,mixed ligand) Complexes, Antibacterial activities, and spectral
studies
1-Introduction
Transition metal complexes containing heterocyclic compounds have been of considerable interest in terms of
structural chemistry, catalysis and biological functions. The field has undergone spectacular growth due to the
synthesis of multidentate ligands from heterocyclic compounds and the complexes of such ligands form with
metal ions [1]. There are a number of multidentate ligands that play important roles in coordination chemistry and
catalyst designing. A large number of multidentate ligands have been synthesized and investigated for their metal
binding character. Several such ligands possessing C=N (azomethine) group are known as Schiff bases [2].The IR
and 1
HNMR spectra of the complexes suggest that cephalexin behaves as a monoanionic tridentate ligand. In
vitro antibacterial activities of cephalexin and the complexes were tested .Icbudak and co-workers [3], are
reported 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. When a metal ion combines with a ligand (Drug), the resulting substance
is said to be a complex.If the ligand (Drug) which combine with the metal forms one or more rings with the metal,
the resulting structure is said to be a metal chelate and the process is known as chelation[4].Beta lactam
antibiotics form a bulky family of zwitterionic drugs that are potent inhibitors of bacterial wall
biosynthesis,which account for approximately 60% of commercial antibiotics formulations. [5].Cephalexin
(structure given in Scheme (1) is one of the most used first generation cephalosporin based antibiotics to treat
infections due to its broad antibacterial activity. Its crystalline structure was published by Kennedy et al. [6].In
2006 Jian-ning and co-workers [7],synthesized 4-(Benzeneazo)salicylaldehyde which was synthesized with
aniline, sodium nitrite and salicylaldehyde. Two tetradentate ligands, N,N-bis[4-(benzeneazo) salicylaldehyde]-o-
phenylenediamine (H2L) and N,N-bis[4-(benzeneazo) salicylaldehyde]ethylenediamine (H2L) were formed by the
2:1 molar condensation of 4-(benzeneazo) salicylaldehyde with o-phenylenediamine or ethylenediamine. Their
Cu(II), Ni(II), Zn(II),Co(II), Mn(II) and Cd(II) complexes were synthesized and characterized by elemental
analysis, molar conductivity measurements, and infrared and electronic spectral data.In 2007 Dursun and co-
worker [8],Synthesized Nicotinamide-acetylsalicylato complexes of Co(II), Ni(II), Cu(II), and Zn(II) were
2. Advances in Physics Theories and Applications www.iiste.org
ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)
Vol.18, 2013
2
synthesised and their structural properties were investigated by employing elemental analysis, magnetic
susceptibilitiy, solid state UV-vis, direct injection probe mass, FTIR and thermoanalytic TG-DTG methods. It
was found that ratio of metal:ligand:ligand is 1:2:2 and the decomposition of each complex starts with
dehydration and follows by decomposition of the nicotinamide and acetylsalicylato, respectively.In 2009 El-Said
and co-workers [9], Synthesized Mixed ligand complexes of Zn(II) and Cd(II) containing ceftriaxone (Naceftria)
or cephradine (Hcefphr) antibiotics and other ligands have been prepared and characterized by elemental analysis,
spectral, biological and thermal studies.
The complexes have the general formulas [Cd2(cephr)(diamine)Cl3(H2O)].xH2O,
[ Cd3(cephr)(µHL)Cl5(H2O)].2H2O where diamine= 2,2'-bipyridyl or o-phenanthroline; M= Cd(II) or Zn(II), L=
glycine, proline or methionine and x=0-6. In 2010 Suresh and co-worker [10], synthesized A
novel .aminoantipyrene) and vanillin and forms stable complexes with transition metal ions such as Cr (III), Mn
(II), Co (II), Ni (II), Cu (II), Zn (II) and Cd (II). Their structures were investigated by elemental analysis, infrared
spectroscopy, electronic spectroscopy, NMR spectroscopy; thermo gravimetric analysis and electron spin
resonance spectroscopy. On the basis of the studies the coordination sites were proven to be through oxygen of
the ring C = O and Nitrogen of the azomethine (-CH = N-)group. The microbiological studies revealed the anti
bacterial nature of the complexes. In (2011) Sunil Joshi, and co-workers [11], synthesized the present study,
Schiff bases have been synthesized by the condensation of cephalexin with p-chlorobenzldehyde and
cinnamaldehyde respectively in methanol. Further metal salts of Mn (II), Co (II), Ni (II) and Zn (II) have
synthesized their metal complexes.
The work presented in this paper concerns the Preparation , Characterization and Antimicrobial activities of
{Fe(II),Co(II),Ni(II),Cu(II),and Zn(II)}Mixed Ligand Complexes Schiff base derived from Cephalexin drug and
4(dimethylamino)benzaldehyde with Nicotinamide in 1:1:2(M:L:2NA) ratio.
2. Experimental
2.1- Chemical
All chemicals used were of reagent grade (supplied by either Merck or Fluka , and used as received., ethanol,
methanol and dimethylforamaide , and KBr, from (B.D.H). Cephalexin mono hydrate powder) and
4(dimethylamino)benzaldehyde from Riedial-Dehaen DSM (Spain).
2.2- Instrumentation
UV-Vis spectra were recorded on a (Shimadzu UV- 160A) Ultra Violet-Visible Spectrophotometer. IR- spectra
were taken on a (Shimadzu, FTI R- 8400S) Fourier Transform Infrared Spectrophotometer (4000- 400) cm-1
with
samples prepared as KBr discs. Elemental micro analysis for the ligand was performed on a (C.H.N.S.O) Perkin
Elemar 2400. While metal contents of the complexes were determined by atomic absorption (A.A) technique
using a Shimadzu AA 620G atomic absorption spectrophotometer. The Chloride contents of complexes were
determined by potentiometric titration method using (686-Titro processor-665. Dosimat Metrohn Swiss).
Molecular weight determined by Rast Camphor method, confirming the monomeric nature of the compounds.
Conductivities were measured for 10-3
M of complexes in DMSO at 25о
C using (conductivity meter, Jewnwary,
model 4070). Magnetic measurements were recorded on a Bruker BM6 instrument at 298°K following the
Farady’s method .Nuclear magnetic resonance spectrum 1H NMR for ligand was recorded in DMSO-d6 using a
Bruker 300 MHz instrument with a tetra methyl silane (TMS) as an internal standard. The samples were recorded
at Queen Mary, university of Al-Albeit, Jordon, Amman. In addition melting points were obtained using (Stuart
Melting Point Apparatus). The proposed molecular structure of the complexes were drawing by using chem.
office prog, 3DX (2006).
2.3- preparation of ligand (HL): [11]
A solution of (Ceph) (0.365 gm, mmole) in methanol (20 ml) was added to a solution of (4DMAB) (0.149 gm,
m mole) in methanol (10 ml). The mixture was refluxed for (5 hours) with stirring. The resulting was an orange
solution allowed to cool and dried at room temperature, then re-crystallization to the precipitate with ethanol,
orange solid was obtained by evaporation of ethanol during (24 hours) Scheme (1), m. p (76-80º). yield 78% .
Anal. Calcd for ligand( HL) C = 62.74%, H = 5.48%, N = 11.71 %. = Found:
C = 61.71%, H = 6.11%, N = 11.90%.
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3
CH
N
H3C
H3C
NH2
O
N
H
H
N
S
H
CH3
O
O
OH
. H2O
N
NH
H
N
S
H
CH3
O
O
OH
(Z)-7-(2-(4-(dimethylamino)benzylideneamino)-2-phenylacetamido)-3-methyl-8-oxo-5-
thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid
Cephalexin
O
+
MeOH Reflux 5 hours
C
O
H
N
H3C CH3
4-(dimethylamino)benzaldehyde
( HL )
Scheme (1) : Schematic representation of synthesis of the ligand(HL)
2.4 -Synthesis of [Cu(L)(NA)2Cl] complex : [11]
A solution of (HL) (0.478 gm, mmole) in methanol (10 ml) and a solution of (NA) (0.244 gm, m mole) in
methanol (10ml), were added to a stirred solution of Cu (II) chloride dihydrate (0.09 gm, m mole) in methanol
(5 ml).The resulting mixture was heated under reflux for (5 hours). Then the mixture was filtered and the
precipitation was washed with an excess of ethanol and dried at room temperature during (24 hours).A green
solid was obtained, m.p (272-276) º C.
2.5- Synthesis of [Fe(L)(NA)2Cl], [Co(L)(NA)2Cl], [Ni(L)(NA)2Cl], and [Zn(L)(NA)2Cl] complexes :
The method used to prepare these complexes was similar method to that mentioned in preparation of
[Cu(L)(NA)2Cl] complex in paragraph above.
2.6 - Preparation of Microorganism suspension
A) The micro- organism suspension was prepared by taking 2–4 colonies from all the studied micro-
organism. Then it was inserted in the physiological solution in 0.85% concentration and was compared with
Macferr land tube number 0.5 which is equal to 1.5×108 cell/mm. It is used for Petri dish preparation for the
examination of biological activity against the under studied chemical compound.
B) Inhibition Activity Selection for the complexes in studied Microorganism
The agar well diffusion method was used to see the effect of under studied chemical complexes on the
microorganism growth. This is done by using 20–25 ml from Nutrient agar medium for each Petri dish. The dish
was incubated in incubator for 24 hours at (37°C) to make sure that no contamination would occur in the dish.
Bore was made on the cultured medium surface by using cork borer. The chemical complexes were made as 100
m ml per bore and left the central bore containing only DMF. The biological activity for the complexes was
defined by measuring the diameter of the inhibition area surrounding each bore in millimeters. [12]
3. Results and Discussion
Physical Properties
Ligand (L) is soluble in( N,N-dimetylformamide (DMF), dimetylsulphoxide (DMSO), methanol (MeOH),
ethanol (EtOH), acetone (C3H6O), 2-propanol (C3H8O) and completely insoluble in water (H2O), carbon tetra
chloride (CCl4), benzene(C6H6), Petroleum ether and chloroform (CHCl3).
Characterization of Metal Complexes:
Generally, the complexes were prepared by reacting the respective metal salts with the ligands using 1:1:2 mole
ratio, i.e. one mole of metal salt : one mole of HL and two moles of nicotinamide. The formula weights and
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4
melting points are given in(Table I based on the physicochemical characteristics, it was found that all the
complexes were non-hygroscopic, stable at room temperature and appears as powders with high melting points.
The solubility of the complexes of ligands was studied in various solvents. They are not soluble in water .All
complexes are soluble in (DMF) and (DMSO) solvent. The complexes were analyzed for their metal by atomic
absorption measurements and chloride contents were determined by standard methods. (Table-1) for all
complexes gave approximated values for theoretical values.
Molar conductance values of the soluble complexes in DMSO show values (5.3-5.8 Ω-1
cm2
mol-1
) indicating
that they are all non-electrolytic in nature . [ 13]
FT-IR spectrum of the ligand (L ):
The (FT-IR) spectrum for the starting material cephalexin exhibits band at (3275) cm-1
due to υ(N–H) primary
amine stretching vibration[14].The bands at (3219, 3049) cm-1
are due to the υ(N–H) secondary amine
stretching vibration .The carboxylic acid group of cephalexin free ligand shows strong absorptions at 1759 cm-1
)
for υ (C=O) and 3406 cm-1
for υ (O- H) stretchings and 1595, 1398 cm-1) due to the asym., sym. stretchings of
(COO) group respectively [6]. Where ∆ υ =[ υ asym (COO) , υ sym (COO)] is 197 cm-1
.These values are quite
agreeable with the values reported earlier [14]. The band at (1689) cm-1
stretching vibration is due to υ (C=O)
for β-Lactum group [14].The carbonyl stretching frequencies for amide, acid and β-lactum groups in cephalexin
free ligand have been assigned at 1595 cm-I [109], 1759 cm-1 and 1760 cm-1 [5], respectively .The bands at
(1595),and (1398) cm-1
were assigned to stretching vibration υ (COO-
) asymmetric and symmetric stretching
vibration, respectively, ∆ υ (COO-
)asym- υ (COO-
)sym =197 [14].. The bands at (1577), (3010), (1163), and (2388)
were assigned to υ(C=C) aromatic, υ(C–H) aromatic, υ(C–C) aliphatic, and υ(C–C) aliphatic stretching
vibration respectively. The band at (1280) cm-1
is due to υ(C–N) stretching vibration. The band at (1247) cm-1
was assigned to υ(C–O) stretching vibration. The band at (580) cm-1
was assigned to υ(C–S) ring stretching
vibration.
[14 - 15].the spectrum for the starting material 4(dimethylamino)benzaldehyde (DMBA) exhibits a
band due to υ (C–N) were observed in the (1371) cm–1
. The bands at (1165) cm–1
and (2796) cm–1
were assigned
to the υ(C–C) and υ(C–H) aliphatic stretching vibration[ 16-17 ].The very strong bands due to carbonyl group
υ(C=O) stretchings of (DMBA) were observed in the (1662 -1600) cm-1
regions [15 ], while the bands at (1548)
cm–1
and (2819) cm–1
were assigned to the υ(C=C) aromatic and υ(C–H) aromatic stretching vibration
respectively [18]. The (FT-IR) spectrum for the ligand (L), the band at (3228) cm-1
due to υ(N–H) secondary
amine stretching vibration , and disappeared The band for the υ(N–H) primary amine stretching vibration. The
spectrum displays a new band at (1678) cm-1
is due υ (HC=N-) group of the azomethine stretching vibrations of
the ligand[15] .The band at (1678) cm-1
is due to υ(C=O) cm-1
stretching vibration for (COOH) overlapping with
azomethine group υ(-HC=N-) .The band at (1678) cm-1
stretching vibration is due to υ (C=O) for β-Lactum
group overlapping with υ(-HC=N-) and υ(C=O) stretching vibrations. The bands at (1597) and (1373) cm-1
were
assigned to stretching vibration (COOH) asymmetric and symmetric stretching vibration, respectively. The bands
at (1531), (3062), (1168)and (2924) were assigned to υ(C=C) aromatic, υ(C–H) aromatic, υ(C–C) aliphatic. and
υ(C–C) stretching vibration respectively. The band at (1315) cm-1
is due to υ(C–N) cm-1
stretching vibration. The
band at (1230) cm-1
was assigned to υ(C–O) stretching vibration [14-16].The band at (584) cm-1
was assigned to
υ(C–S) stretching vibration [13 -15-19-].The assignment of the characteristic bands for the starting materials,
intermediate compounds and the ligand are summarized in Table (2).
FT-IR of spectral data for the Schiff base mixed ligands complexes
[Fe(L)(NA)2Cl](1),[Co(L)(NA)2Cl](2),[Ni(L)(NA)2Cl](3),[Cu(L)(NA)2Cl](4),[Zn(L)(NA)2Cl](5):
The characteristic bands in Schiff base are used to determine the binding modes found in the system are υ
(HC=N-) group of the azomethine, υ (N-H), υ (M-O), υ (M-N).The assignments of the characteristic bands are
summarized in Table (2).on complexation these band has been shifted to lower frequencies (1597), (1624),
(1624), (1660), and (1593) cm-1
for complexes (1), (2), (3), (4), and (5), (6) This band gets shifted to lower
frequency in the complexes, indicating the coordination through azomethine nitrogen to metal atom. [14-15],.
The bands at (1597), and (1373) cm-1
were assigned to stretching vibration (COOH) asymmetric and symmetric
stretching vibration, respectively. on complexation these bands have been shifted to lower and higher
frequencies [(1681), (1600), (1624), (1678), and (1539) cm-1
for υ(-COO)asy], and [(1377), (1396), (1396),
(1375), and (1377) cm-1
,for υ(-COO) sy] for the compounds (1) , (2) , (3) , (4) , and (5), that the coordination
with metal was occurred through the oxygen atom of carboxylate ion.
and the band at (1678w) cm-1
stretching vibration is due to υ (C=O) for β-Lactum group, but these band has
been shifted to higher frequency at 1681 for complex showing that the coordination is through the Oxygen
atom of β-Lactum group. The bands at (439), (482), (459) , (478), and (489) cm-1
were assigned to υ(M–O) for
5. Advances in Physics Theories and Applications www.iiste.org
ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)
Vol.18, 2013
5
compounds (1), (2), (3), (4),and (5), indicating that to the carbocylic oxygen, and oxygen of β-Lactum group of
the ligand are involved in coordination with metal ions.
The bands at (540), (582), (528), (505) and (551) cm-1
were assigned to υ(M–N) for compounds (1), (2), (3), (4),
and (5), respectively , indicating that the amine nitrogen is involved in coordination with metal ions.
(U.V-Vis) Spectrum for the Schiff base ligand:
The electronic spectrum of the ligand has been measured in DMSO solution between 200- 1100 nm at room
temperature .In the spectrum of the Schiff base ligand(L) ) , the absorption band observed at 212 nm (47169 cm-
1
), 242 nm(41322 cm-1
) (267 nm) (59880 cm-1
) which are assigned to benzene (π-π*) transition, and the band at
(336 nm) (29761cm-1
) is assigned due to( n-π*) transition associated with the azomethine chromosphere (-C=N)
[14-15,20].
(U.V-Vis) Spectral data for the Shiff base mixed ligands complexes:
The absorption data for complexes are given in Table (3).
[Fe(L)(NA)2Cl]: The (U.V- Vis) spectrum, exhibits four peaks, the first middle peak at 269 nm (37174 cm-1
), is
due to the ligand field, while the second high peak at342 nm (29239 cm-1
) (is due to the (C.T), the third and
fourth weak peaks at 803 nm (12453 cm-1
), and 977 nm (10235 cm-1
), which assigned to
(5
E → 5
T2) (d–d), and (5
E → 5
T2) (d–d) transition respectively in an octahedral geometry.
[Co(L)(NA)2Cl]: The (U.V- Vis) spectrum, exhibits three peaks ,the first high peak shoulder with at 269 nm
(37174 cm-1
) is due to the ligand field and (C.T), while the second and third weak peaks at (897 nm)(11148 cm-
1
), and (992 nm)(10080 cm-1
) which assigned to (5
E → 5
T2) (d–d), and (5
E → 5
T2) (d–d) transition respectively in
an octahedral geometry.
[Ni(L)(NA)2Cl]: The (U.V- Vis) spectrum, exhibits two peaks, the first high intense peak at (268 nm)(37313 cm-
1
) is due to the ligand field and (C.T) , while the second weak peaks at (992 nm)(10080 cm-1
), which assigned to
(5
E → 5
T2) (d–d), transition in an octahedral geometry .
[Cu(L)(NA)2Cl]: The (U.V- Vis) spectrum, exhibits two peaks , the first high broad peak at (272 nm)(36764 cm-
1
is due to the ligand field and (C.T) , while the second weak broad peak at (924 nm)(10822 cm-1
), which
assigned to (5
E → 5
T2) (d–d), transition in an octahedral geometry.
[Zn(L)(NA)2Cl]: The (U.V- Vis) spectrum, exhibits two high peaks, the first middle peak at 271 nm (36900 cm-
1
) is due to the ligand field and, the second high peak at (339 nm)(29498 cm-1
) is due to the (C.T) in an
octahedral geometry.
Also, the values of the magnetic moment Table (3).may be taken as additional evidence3’32 for their octahedral
structure.
Molecular weight determined by Rast Camphor method and were found in accordance with calculated value the
range of metal complexes (1060-1092), [11].
Antimicrobial activity:
The in vitro antimicrobial screening results are given in Table 4, Chart (1). On the basis of observed zones of
inhibition, all the metal-mixed ligand complexes are active against all six tested organisms
which in fact is in agreement with the literature [24]. The antibacterial results evidently show that the activity of
the Schiff base became more upon coordination to the metal atoms.
Chart (1) Chart of biological effects of some of the studied complexes
6. Advances in Physics Theories and Applications www.iiste.org
ISSN 2224-719X (Paper) ISSN 2225-0638 (Online)
Vol.18, 2013
6
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Vol.18, 2013
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[22] Chaudhary Rakhi and Shelly, (2011) Synthesis, Spectral and Pharmacological Study of Cu(II), Ni(II) and
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Table(1):The physical properties of the compounds
Cl%
Metal%Λm
s.cm2
.mol-
1
)
M .p° c
(de) °c
theory
(exp)
Yield %ColorM. wt
Rats
method.
M. wt
Calc.
Compounds
--
-76-8078orange498.17
478.17
L
C25H26N4O4S
4.36
(4.50)
6.875.3172 Dec.87Grey
green
823.0
813.10
[Fe(L)(NA)2 Cl]
C37H37ClFeN8O6S
4.34
(4.50)
7.225.3280 Dec.77Violet843.5
815.16
[Co(L) (NA)2Cl]
C37H37Cl Co N8O6S
4.34
(4.50)7.19
5.8280 Dec.82Yellow833.10
815.95
[Ni(L)(NA)2Cl]
C37H37Cl Ni N8O6S
4.32
(4.33)
7.74
5.4272-27684Green829.50
820.80
[Cu(L)(NA)2 Cl]
C37H37Cl Cu N8O6S
4.31
(4.50)
7.95
8.6102-11687Brown843.80
822.67
[Zn(L)(NA)2Cl]
C37H37Cl Zn N8O6S
M. wt = Molecular Weight ,Λm = Molar Conductivity , dec. = decomposition , Calc.=calculation
Table(2):Data from the Infrared Spectra for the Free Lingands and there Metal Complexes (cm-1
).
Compound
(N-H)
primary
amine
υ(N-H)
Secondary
amide
υ(C=O)
for
COOH
υ(C=O)
β-lactam
υ(C=O)
amide
υ(C=N)
υas
COO
υs
COO
υ(C=C)
arom.
υ(C-
C)
aliph.
υ(C-
N)
υ(C-
O)
υ(C-
S)
υ
(C-
H)
arom.
υ(C-
H)
aliph.
υ(M-
N)
υ
(M-
O)
L -------
3228
overlap
1678
overlap
1678
overlap
------
1678
overlap
1597 1373 1531 1168 1315 1230 594 3062 2924 ----- -----
Nicotine amide
3367,
3159
-------- -------- ------- 1679vs ------ ----- ------ 1593 1124 1201 ----- ------ 3061 2787 ------ -----
[Fe(L)(NA)2Cl] 3441
3441
overlap
1681
overlap
1681
overlap
------- 1597
1597
overlap
1377 1539 1168 1288 1248 597 3070 2970 540 439
Co(L)(NA)2
Cl]
3402
3306 ,
3267
1666
overlap
1666
overlap
------ 1624 1600 1396 1581 1199 1296 1238 3078 2940 582 482
Ni(L)(NA)2 Cl] 3406
3321 ,
3267
1666
overlap
1666
overlap
------ 1624
1624
overlap
1396 1581 1195 1292 1234 3078 2950 528 459
Cu(L)(NA)2
Cl]
3406 3236
1678
overlap
1678
overlap
------
1660
overlap
1678
overlap
1435 1531 1134 1284 1249 2966 2924 505 478
Zn(L)(NA)2 Cl] 3410
3363 ,
3232
1678
overlap
1678
overlap
----- 1593
1593
overlap
1377 1535 1166 1288 1230 3066 2850 551 489
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