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American Society for Testing and Materials

Thiosemicarbazone complexes of copper(II): structural and biological studies

The nature of metal complexes of heterocyclic thiosemicarbazones reported in the literature through 1989 have been reviewed with an emphasis on variations in stoichiometry and stereochemistry. A brief introduction is followed by a survey of the biological activity of the uncomplexed thiosemicarbazones. Next is a section on the chemical nature of thiosemicarbazones including a discussion of preparative methods, modes of coordination and isomerism. This is followed by a discussion of structural information and biological activity of the iron(III), iron(II), copper(II), cobalt(III), cobalt(II) and nickel(II) complexes of heterocyclic thiosemicarbazones. Short sections on the biological activity of other chelating thiosemicarbazones and metal complexes are also included.

Structural and physical correlations in the biological properties of transition metal heterocyclic thiosemicarbazone and S -alkyldithiocarbazate complexes

This paper is concerned with the cross-linking of poly(vinyl alcohol) (PVA) using maleic acid as the cross-linker. The curative (maleic acid) dose and the curing temperature and time were varied between 2.5 and 60% (w/w), 120 and 160 °C and 30 and 120 min, respectively. From a thorough swelling study in both hot and cold water (percentage swelling, gel content, swelling ratio, etc-) the optimum curative dose and curing conditions have been evaluated. The molecular weight between the cross-links exhibited a sharp fall up to a maleic acid dose of 20% (w/w). A comparative evaluation of maleic acid cross-linked and heat-treated PVA films has been done. Better heat stability for maleic acid cross-linked PVA was observed from thermogravimetric analysis. A shift in glass transition temperature was observed for both heat-treated and maleic acid treated PVA compared with the virgin one. IR spectroscopic study indicated the presence of an ester linkage and an olefinic double bond in maleic acid treated and heat-treated PVA films, respectively. Maleic acid cross-linked PVA is quite stable in different polar and nonpolar solvents. A definite structural pattern has been observed in maleic acid cross-linked PVA films through scanning electron microscopy.

Studies On The Crosslinking Of Poly (Vinyl Alcohol)

The synthesis and characterization of metal complexes of some dipositive metal ions with 1-valeroyl-4-phenyl-3-thiosemicarbazide (VTSC) is reported. The data of elemental analysis, molar conductivities, magnetic measurments and spectral (i.r., visible) studies have been used to elucidate the structure of the complexes. I.r spectra show that VTSC acts as a bidentate ligand and coordinates via 2NH and the enolic carbonyl oxygen (=C-OH) of the hydrazide moiety with the displacement of a hydrogen atom from the latter group. The values of molar conductivities in DMF indicate the non-electrolytic nature of all metal chelates. A tetrahedral structure is proposed for [Co (VTSC-H) Ac], square-planar for [Ni (VTSC-H) Ac] and [Cu (VTSC-H) Ac]H2O complexes, and octahedral for [Ni (VTSC-H)2. 2H2O]2H2O and [Co (VTSC-H)2.2H2O]2H2O complexes according to the data of magnetic and electronic spectral measurments.

Synthesis of Some Transition Metal Complexes Derived from 1-Valeroyl-4-phenyl-3-thiosemicarbazide

(0.087 g, 0.5 mmol) in H2O (1 ml) was added to H2papts (0.143 g, 0.5 mmol) or H2pxapts (0.151 g, 0.5 mmol) in EtOH (10 ml) to give yellow (H2papts) or orange-brown (H2pxapts) solids. These were left in the dark for 3 h, filtered off, washed with little H2O, EtOH, Et2O and dried in the dark in vacuo. Trans-[UO2(HL)(bipy)(AcO)(H2O)2 ]· nH2O (HL5Hpapts, n53; HL5 Hpxapts, n50; bipy52,29-bipyridyl): Hydrated uranyl acetate (0.21 g, 0.5 mmol) in MeOH (10 ml) was added to a MeOH solution of 2,29-bipyridyl (0.078 g, 0.5 mmol) and H2papts (0.143 g, 0.5 mmol) or H2pxapts (0.151 g, 0.5 mmol). The resulting solution was boiled under reflux for 3 h in a steam bath. The red-orange (H2papts) or yellow (H2pxapts) solutions were reduced in volume until the precipitates separated out. These were filtered off, washed with little MeOH and dried in a desicator over silica gel. [Ag(H2papts)(bipy)]BPh4: AgNO3 (0.087 g, 0.5 mmol) in H2O (0.5 ml) was added to 2,29-bipyridyl (0.078 g, 0.5 mmol) in MeOH (25 ml) to form a colorless solution, to which H2papts (0.143 g, 0.5 mmol) in MeOH (10 ml) was added to produce a red-brown solution. NaBPh4 (0.17 g, 0.5 mmol) in MeOH (5 ml) was added and the precipitate was separated out. This was filtered off, washed with a little H2O, MeOH, Et2O and dried in the dark in vacuo. [Pd(Hpapts)(bipy)]BPh4: The complex [Pd(bipy)Cl2] was prepared by the literature method. 12) To a stirred suspension of [Pd(bipy)Cl2] (0.17 g, 0.5 mmol) in acetone (10 ml), H2papts (0.143 g, 0.5 mmol) and KOH (0.056 g, 1 mmol) in MeOH (10 ml) was added. The mixture was stirred overnight. NaBPh4 (0.17 g, 0.5 mmol) in MeOH (5 ml) was added to the resulting brown solution. The complex was filtered off, washed with MeOH, Et2O and dried in vacuo. Catalytic Oxidation For the catalytic oxidation by [Ru(HL)2(H2O)2] (HL5Hpapts, Hpxapts) complexes, the organic substrate (1.0 mmol) was added to NaIO4 (2.5 mmol) in CCl4‐CH3CN‐H2 O (1 :1:2 ; 20ml) and the catalyst (0.02 mmol). The reaction mixture was stirred under reflux at 70 °C, then cooled and extracted with diethyl ether (3320 ml). The etheral layer was then dried with anhydrous Na2SO4 and the aldehyde or ketone content quantified as its 2,4-dinitrophenylhydrazone derivatives. The aqueous layer 266

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Synthesis and structure studies of complexes of some second row transition metals with 1-(phenylacetyl and phenoxyacetyl)-4-phenyl-3-thiosemicarbazide.

The synthesis and characterization of MnII, CoII, NiII, CuII, ZnII, CdII UO
 2
 2+
 , CrIII and FeIII complexes of biacetylmonoxime nicotinoyl hydrazone (H2BMNH) are reported. Elemental analysis, molar conductance, magnetic moment and spectral (i.r., visible and n.m.r.) measurements have been used to characterize the complexes. I.r. spectral data show that the ligand behaves in a bidentate and/or tridentate manner. An octahedral structure is proposed for the MnII, NiII, CrIII and FeIII complexes, while a square-planar structure is proposed for both CoII and CuII complexes on the basis of magnetic and spectral measurements.

Ligational behaviour of biacetylmonoxime nicotinoyl hydrazone (H2BMNH) towards transition metal ions

The synthesis and characterization of cobalt(II), nickel(II), copper(II), zinc(II) and cadmium(II) chelates containing 1-anthranyl-4-phenyl-3-semicarbazide (APSC) and/or 1-anthranyl-4-phenyl-3-thiosemicarbazide (APTSC) are reported. The chelates have been characterized on the basis of elemental analyses, spectra (NMR, IR, visible), magnetic moments, conductivities and molecular weight measurements. The values of molar conductivities in DMP or DMSO indicate the non-ionic nature of all metal chelates. A tetrahedral structure is proposed for the Ni(II) chelates, square-planar for the Cu(II) chelates and tetrahedral or octahedral for the Co(II) chelates according to the data of magnetic measurements and electronic spectra. The ligands (APSC, APTSC) behave in a bidentate manner toward the metal ions, but with different coordination sites. 1HNMR spectra of the ligands and the diamagnetic chelates are discussed. The chelates have a monomeric or a polymeric nature.

M. M. Bekheit

Papers

Synthesis of Some Transition Metal Complexes Derived from 1-Valeroyl-4-phenyl-3-thiosemicarbazide

Synthesis and structure studies of complexes of some second row transition metals with 1-(phenylacetyl and phenoxyacetyl)-4-phenyl-3-thiosemicarbazide.

Ligational behaviour of biacetylmonoxime nicotinoyl hydrazone (H2BMNH) towards transition metal ions

Synthesis and Structural Studies of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) Chelates Derived From Semicarbazide and Thiosemicarbazide Derivatives

Complexes of Cu(II), Co(II), Ni(II), Cd(II) and Hg(II) halides with hydrazones derived from girard T and chromone