Nagwa Nawar

Preparation and characterization of chelating fibers based on natural wool for removal of Hg(II), Cu(II) and Co(II) metal ions from aqueous solutions.

The graft copolymerization of acrylonitrile (AN) onto natural wool fibers initiated by KMnO(4) and oxalic acid combined redox initiator system in limited aqueous medium was carried out in heterogeneous media. Moreover, modification of the grafted wool fibers was done by changing the nitrile group (-CN) into cyano-acetic acid α-amino-acrylic-hydrazide through the reaction with hydrazine hydrate followed by ethylcyanoacetate which eventually produce wool-grafted-poly(cyano-acetic acid α-amino-acrylic-hydrazide) (wool-g-PCAH) chelating fibers. The application of the modified fibers for metal ion uptake was studied using Hg(2+), Cu(2+) and Co(2+). The modified chelating fibers were characterized using FTIR spectroscopy, SEM and X-ray diffraction.

Synthesis, spectral and antimicrobial activity studies of o-aminoacetophenone o-hydroxybenzoylhydrazone complexes

Coordination compounds of MnII, CoII, NiII, CuII, ZnII, CdII and HgII ions with o-aminoacetophenone o-hydroxybenzoylhydrazone (AAOHBH) were synthesized and characterized by elemental analyses, molar conductivity, magnetic moments (at ca. 25 °C) and spectral (i.r., u.v., n.m.r. and m.s.) studies. The i.r. spectra show that the ligand acts in a monovalent bidentate, neutral bidentate and/or neutral tridentate fashion, depending on the metal salt used and the reaction medium. Tetrahedral structures are proposed for both CoII and NiII complexes and square planar for CuII complexes on the basis of magnetic and spectral evidence. The complex formation in solution was investigated potentiometrically and spectrophotometrically. Spectral studies in solution show that the ligand can be used for the microdetermination of CoII ion within a metal concentration up to 46.3 p.p.m. The electrical conductivity of AAOHBH and its metal complexes was determined. The tendency of AAOHBH to form complexes with CoII, NiII, CuII, CdII and HgII ions in 50% aqueous-dioxane was studied by pH measurements.The antimicrobiol activity of AAOHBH and its complexes derived from CoII, NiII and CuII illustrates that the NiII complex seems to be inert towards Escherichia coli and Bacillus subtilis. The antimicrobial activity of the CuII complex was higher against E. coli and lower against B. subtilis than the corresponding organic ligand. The CoII complex has the same activity as the organic ligand against E. coli.

Mono- and binuclear Schiff base complexes derived from glycine, 3-acetylpyridine and transition metal ions

Binuclear Schiff base complexes derived from glycine (Gly) and 3-acetylpyridine (3-APy) in the presence of M(OAc)2 [M = CoII, NiII, CuII, ZnII and CdII] have been synthesized. The role of pH in promoting the condensation of glycine and 3-acetylpyridine, as well as the substitution of acetates by hydroxide ion, has been discussed. Also, the reaction of glycine with 3-acetylpyridine in the presence of MCl2 [M = CoII and NiII] and MCl3 [M = FeIII and CrIII] yields mono- and/or binuclear complexes containing both of glycine and 3-acetylpyridine without condensation. Both types of complex were isolated and characterized by chemical analysis, conductance, spectral (u.v.–vis., i.r., and 1H-n.m.r.), magnetic and thermal measurements.

Synthesis, spectral characterization and DNA binding of Schiff-base metal complexes derived from 2-amino-3-hydroxyprobanoic acid and acetylacetone

Four new metal complexes derived from the reaction of Cu(II), Co(II), Ni(II) and Zn(II) acetates with the Schiff-base ligand (H3L) resulted from the condensation of the amino acid 2-amino-3-hydroxyprobanoic acid (serine) and acetylacetone have been synthesized and characterized by, elemental analyses, ES-MS, IR, UV-Vis., 1H NMR, 13C NMR, ESR, thermal analyses (TGA and DTG) and magnetic measurements. The results showed that the Schiff-base ligand acts as bi-negative tridentate through the azomethine nitrogen, the deprotonated carboxylate oxygen and the enolic carbonyl oxygen. The optical band gaps measurements indicated the semi-conducting nature of these complexes. Molecular docking was used to predict the binding between the Schiff base ligand with the receptor of prostate cancer mutant H874Y. The interactions between the Cu(II) complex and calf thymus DNA (CT-DNA) have been studied by UV spectra. The results confirm that the Cu(II) complex binds to CT-DNA in an intercalative mode.

SYNTHESES OF RUTHENIUM-CONTAINING HETEROMETALLIC COMPLEXES BY USE OF TRIDENTATE PHOSPHINE LIGANDS

Abstract Treatment of [RuCl(dppee)(η-C 5 H 5 )] [dppee = 1,1-bis(diphenylphosphino)ethene] with HPPh 2 gives the addition product [RuCl{(PPh 2 ) 2 CHCH 2 PPh 2 }(C 5 H 5 )], 1 . The uncoordinated phosphine group of complex 1 reacts with [IrCl(CO) 2 ( p -toluidine)] to give the heterobimetallic complex [RuCl(C 5 H 5 )}(PPh 2 ) 2 CHCH 2 PPh 2 }IrCl(CO) 2 ], 2 . Complex 1 reacts with [Fe(CO) 5 ] to yield [RuCl(C 5 H 5 ){(PPh 2 ) 2 CHCH 2 PPh 2 }Fe(CO) 4 ], 3 , and with [Mo(CO) 6 ] to give the heterometallic complex [RuCl(C 5 H 5 ){(PPh 2 ) 2 CHCH 2 PPh 2 }Mo(CO) 5 ], 4 . Complex 1 also reacts with [RuCl 2 ( p -cymene)] 2 , [Ru 3 (CO) 12 ] and [Ru 3 (CO) 10 (dppee)] to give the homometallic complexes [RuCl(C 5 H 5 ){(PPh 2 ) 2 CHCH 2 PPh 2 }RuCl 2 ( p -cymene)], 5 , [RuCl(C 5 H 5 ){(PPh 2 ) 2 CHCH 2 PPh 2 }Ru 3 (CO) 11 ], 6 , and [RuCl(C 5 H 5 ){(PPh 2 ) 2 CHCH 2 PPh 2 }Ru 3 (CO) 9 (dppee)], 7 , respectively.

Iron-rhodium complexes with a single bridging diphosphine ligand: the crystal structure of [CpFe(μ-CO)2(μ-dppm)RhI2]

The mononuclear complexes [FeCpl(CO) 2 ] 1 , FeCp(CO) 2 (η 1 -dppm)]I 2 , [FeCp(CO)(η 2 -dppm)]I 3 , [FeCp(CO) 2 ( η 1 -dppen)]I 5 and [FeCp(CO)( η 2 -dppen)]I 6 [dppen = Ph 2 PC(= CH 2 )PPh 2 ] have been synthesise and reacetd with [Rh 2 Cl 2 (CO) 4 ] to produce heterobimetallic complexes of the type [CpFe(μ-CO) 2 (μ-PP)RhX 2 (X = Cl or I). The structure of [CpFe(μ-CO) 2 {μ-Ph 2 PCH 2 PPh 2 }RhI 2 ] 4 has been determined by X-ray crystallography.

Iridium carbonyl cluster complexes with bidentate phosphine ligands; the X-ray crystal structure of [Ir4(CO)8(dppa)2]·3(THF)

Abstract Reactions of [Ir4(CO)12] with 1,1-bis(diphenylphosphino)ethene, Ph2PC( CH2)PPh2 (dppen) and 1,1-bis(diphenylphosphino)amine, Ph2PN(H)PPh2(dppa) gave [Ir4(CO)12−n(L)n−2)] (L=dppen or dppa and n=2 or 4) depending upon the reaction conditions. The structures of the cluster complexes are discussed on the basis of IR, 31P-NMR spectroscopic data and FAB mass spectra. The structure of the disubstituted species [Ir4(CO)8(dppa)2]·3(THF) (THF=tetrahydrofuran, C4H8O) has been determined by X-ray crystallography.

New rhodiumruthenium heterobimetallic complexes with bridging bi- or tri-dentate phosphine ligands

Abstract The mononuclear chelated complex [RuCl(Cp)(η 2 -dppa)] has been synthesised and reacted with [Rh 2 Cl 2 (CO) 4 ] to form the heterobimetallic complex [(Cp)Ru(μ-CO) 2 {(μ-Ph 2 PN(H)PPh 2 }RhCl 2 ]. Complexes of [RuCl(Cp){(PPh 2 ) 2 CHCH 2 PPh 2 }] have been reacted with [Rh 2 Cl 2 (CO) 4 ] or [RhCl(CO) 2 ( p -toluidene)]. Characterisation of these new ruthenium complexes was carried out using 31 P-NMR, FAB mass spectroscopy, elemental analysis and IR spectrophotometry.

Synthesis of new rutheniumiridium heterobimetallic complexes via ring-opening reactions of bidentate phosphine ligands and tridentate phosphine ligand: crystal structure of [(C5H5)Ru(μ-CO)2{μ-Ph2PN(H)PPh2}IrCl2]

Abstract Treatment of [Ru(C5H5)Cl(dppm)] (1) [dppm=1,1-bis(diphenylphosphino)methane], [Ru(C5H5)Cl(dppen)] (2) [dppen=1,1-bis(diphenylphosphino)ethene] or [Ru(C5H5)Cl(dppa)] (3) [dppa=1,1-bis(diphenylphosphino)amine] with [IrCl(CO)2(p-toluidine)] leads to the formation of the heterobimetallic complexes [(C5H5)Ru(μ-CO)2{μ-L}IrCl2] (L=dppm 4, dppen 5 or dppa 6) in high yield. The structure of [(C5H5)Ru(μ-CO)2{μ-Ph2PN(H)PPh2}IrCl2] (6) has been determined by X-ray diffraction. The uncoordinated phosphine group of [Ru(C5H5)Cl{(PPh2)2CHCH2PPh2}] (7) reacts with [IrCl(CO)2(p-toluidine)] to give [(C5H5)RuCl{(PPh2)2CHCH2PPh2}Ir(CO)2Cl] (8). Treatment of the heterobimetallic complex 8 with Me3NO·2H2O affords [(C5H5)R u(μ-CO){(PPh 2 ) 2 CHCH 2 PPh 2 }I rCl2] (9).

Synthesis and Spectral Characterization of Some Complexes Derived From N-Benzoyl-N′-Carboxylmethylthiopropylidine Thiourea (Bcmt)

Abstract New metal complexes derived from the reaction of N-benzoyl-N′-carboxyl methylthiopropylidine thiourea (BCMT) with Cu(II), Co(II), Ni(II), and Fe(III) chloride and/or acetate salts have been synthesized and characterized using elemental analyses, molar conductance, spectral (IR, UV-Vis., mass, 1H NMR), thermal (TGA, DTG), and magnetic measurements. The IR results showed the modes of coordination in case of mononuclear and binuclear metal complexes. Different types of geometries are suggested on the basis of the spectral and the magnetic data. Also, the ligand field parameters for the metal complexes were calculated. The amounts of the solvents as well as the mechanism of decomposition were proposed using thermal measurements. The results of biological activity of the ligand give us the promise to be effective in tumors treatment. GRAPHICAL ABSTRACT