Ukrainian Chemistry Journal

Contents of Volume 81 № 11 (2015)

Inorganic and Physical Chemistry

MIRNAYA T.A., ASAULA V.N., YAREMCHUK G.G., VOLKOV S.V.
Synthesis of zinc and lead sulfide, selenide nanoparticles into mesogenic metal caprylate melts
  • Summary: Results for obtaining, optical and fluorescence properties of nanocomposites based on zinc and lead sulfide and selenide nanoparticles into caprylate matrix have been represented. Nanoparticle morphology has been investigated by transmission electron microscopy. The matrix nature was shown to affect the spectral properties of nanocomposites synthesized.
  • Keywords: liquid crystals, semiconductor chalcogenides nanoparticles, optical properties, nanocomposites, alcanoates of metals, fluorescence.
  • pp.: 6 - 10.

SHARANDA L.F., OGENKO V.M., LYSYUK L.S., VOLKOV S.V.
Features of the synthesis of nanosized heterogeneous Pd-carbon-containing catalytic systems and their using in the crosscoupling reactions
  • Summary: A novel approaches for the stabilization carbon nanostructures and metallic nanoparticles Pd(0) within oxide-containing composite materials were developed and the nanosized carbon-containing palladium catalytic systems with nonporous, mesoporous or biporous (micro- and mesoporous) structure at their base were synthesized. The synthesized heterogeneous carboncontaining palladium nanocatalysts show excellent catalytic activity in the cross-coupling reactions (yield is 91 —100 %), allow carrying out the reaction in water — an environmentally safe solvent, easily regenerate and do not lose their activity if reused.
  • Keywords: composite nanomaterials, palladium, heterogeneous catalysis, carbon films, carbon nanotubes, alumina, silica, titanium oxides, cross-coupling reactions.
  • pp.: 11 - 23

VARZATSKII О.А., KATS S.V., VOLKOV S.V.
Synthesis pathway and molecular design of macrobicyclic tris-diiminates of d-metals (clathrochelates)
  • Summary: Synthesis of pseudomacrobicyclic complexes based on oximehydrazones and pyrazoloximes. There are also provided themethods of stepwise template assembly for the synthesis of unsymmetrical frame macrobicyclic compounds with non-equivalent apical and rib groups by remetallation apical groups, stepwise framework assembly and application of surface metaloxide matrices as topochemical protective group. The composition and structure of molecules were determined by elemental analysis, by the complex of spectral methods (NMR-, UV-Viz, infrared and mass-spectrometry). In the described reactions the high yields were reached and the selectivity of these reactions made possible to purificate the target products without the use of chromatography in most cases.
  • Keywords: macrocyclic tris-diiminates of d-metals, clathrochelates, template synthesis, "forced" synthesis of solvatocomplexes, aimed template synthesis, psevdoсlatroсhelates complexes, dinuclear clathrochelates, phtalotsianine clathrochelates, transmetallation reaction apical groups.
  • pp.: 24 - 33

CHERNII V.Ya., TRETYAKOVA I.N., DOVBII Y.M., VOLKOV S.V.
Synthesis of phthalocyanine complexes of d- and f-metals
  • Summary: Methods for the synthesis of macrocyclic complexes of phthalocyanines and their analogues with d- and f-metals have been considered. The characteristic features of their structure; patterns of influence of the nature of the central atom, the peripheral and outof- plane substituents on the physico-chemical properties were discussed. Possibility of their modification by introduction of substituents at the periphery of the macrocycle and to the central metal atom was shown. Methods for the synthesis of bis (8-hydroxyquinolatо)phthalocyanines zirconium and hafnium are given.
  • Keywords: phthalocyanine complexes, d-metals, f-metals, synthesis, NMR, UV-vis spectroscopy.
  • pp.: 34 - 38

TRUNOVA Ye.K., ZHELEZNOVA L.I., GERASIMCHUK A.I., BEREZHNYTSKAYA A.S.
Metal complexes of β-diketone as basic components of nanocomposite systems
  • Summary: Methods of synthesis of Ge(IV), 3d-metal and lanthanide coordination compounds with saturated and unsaturated β-diketones are designed, their composition, structure and thermal properties were determined. The correlation between the properties of complexes and the nature of the ligand and the electronic structure of metal was established. The possibility of using the β-diketonates as precursors for obtaining germanium nano- and submicron particles of different morphology, lanthanum, copper, manganese complex oxide coatings and cobalt metallic and oxide structures on carbon nanotubes by CVD-technology (PEMOSVD, spraypyrolysis, plasma-chemical methods) was shown. Metallopolymers based on lanthanide complexes with unsaturated β-diketones were obtained. The influence of the nature of metal and ligand on the polymerization rate was established. On the basis of the metallopolymers nanoscale films (~10—30 nm thickness) on silicon substrates were obtained and planar sandwich-type ITO/ PEDOT : PSS/[Ln(mphpd)3]n/PVC/Al heterostructures showing electroluminescence were designed. The lanthanide- containing metallopolymers can be used as emissive layers in organic electroluminescent devices.
  • Keywords: complexes, 3d-metals, lanthanides, β-diketones, synthesis, nanoparticles, luminescence, polymers.
  • pp.: 39 -52

PEKHNYO V.I., KOZACHKOVA A.N., TSARYK N.V., KUTSENKO I.P., SHTOKVISH O.A., TRACHEVSKII V.V.
Structure and stability of complexes of palladium (II) with 1-aminobutylidene-1,1-bisphosphonic acid
  • Summary: It has been found by pH potentiometry, electron spectroscopy and 31P NMR spectroscopy that when K2[PdCl4] interacts with 1-aminobutylidene-1, 1-bisphosphonic acid (ABBPA, H4L), complexes of equimolar and bisligand composition, in which one or two ligand molecules are coordinated to palladium (II) by a nitrogen atom of amine group and an oxygen atom of phosphonic group with closure of one or two five-membered chelate rings, are formed in aqueous solutions at the physiologic concentration of chloride ions (0.15 mol/L KCl) depending on the metal: ligand ratio and pH. Formation constants of complexes of the composition [PdH2LCl2]2– (lgβ=36.87(6)), [Pd(H2L)2]2– (lgβ=60.68(9)) and [Pd(H2L)-(HL)]3– (lgβ=57.19(4)) have been calculated. A bisligand complex of Pd(II) with ABBPA (A) and a heterometallic complex of Pd(II)—Cu(II) with ABBPA (B) have been synthesized. Single crystals of the compound (B) have been obtained, for which an X-ray diffraction study has been carried out.
  • Keywords: heterometallic complexes, palladium (II) complexes, aminobisphosphonic acids, formation constants of complexes, X-ray diffraction analysis.
  • pp.:

YANKO O.G., KHARKOVA L.B., BARANETS S.A., FOKINA Z.A., ALEKSANDROVA N.G., MASHKOVA E.M., SUBBOTIN V.V.
Synthesis and structure of chalcohalides of platinum and rare metals
  • Summary: Novel chalcogen halide complex compounds of Ru, Rh, Ir, Os and Re have been obtained. It has been shown that in contrast to solid-phase synthesis, the use of liquid chalcogen halide media makes it possible to control the composition and structure of complexes depending on reaction medium and temperature. In media with excess chalcogen, osmium, ruthenium, rhodium and iridium form binuclear complex compounds with different ligands: molecules of chalcogen dihalides, polychalcogenide chains, ring-crown Se9. In osmium and ruthenium complexes there are metal–metal bonds. Rhenium forms under these conditions mononuclear octahedral complexes and is able to form at 200 oC tri- and tetranuclear complexes with coordination number 9, and osmium is able to form binuclear octahedral cluster polymers.
  • Keywords: chalcohalides, rhodium, ruthenium, iridium, rhenium, osmium, selenium, sulfur, chlorine, bromine, ring-crown, rare metals, liquid media, trinuclear, tetranuclear complexes.
  • pp.: 61 - 67

KOLESNICHENKO V.L., GOLOVERDA G.Z.
Synthesis of colloidal nanoparticles of iron oxide in coordinated non-aqueous solvents
  • Summary: Complexing polar solvents were used as a medium for the synthesis of nanoparticles of metal oxides in the colloidal state without any surfactants. By coordinating and chelating, diethylene glycol and Nmethyldiethanolamine inhibit hydrolysis reaction of iron alkoxide, and reaction solutions containing stoichiometric amounts of all reagents can be stored indefinitely at ambient temperature. Variation of temperature (150— 220 °C) allows to adjust the reaction rate and thus affect the kinetics of nucleation and crystal growth of iron oxide. The monodisperse nanoparticles of magnetite (Fe3O4) synthesized in the size range 3.2—7.5 nm among diethylene glycol and 16.8nm in the medium of N-methyldiethanolamine. These colloids oxygenation results in the formation of stable colloids of maghemite (γ-Fe2O3). Highly dispersed oxide samples synthesized have shown superparamagnetic properties with high saturation of magnetization thus indicating spin ordering. The active surface of the nanoparticles may easily be chemically modified in accordance with the proposed technical implementation.
  • Keywords: synthesis, superparamagnetic nanoparticles, iron oxides, colloids.
  • pp.: 68 - 73

BURYAK N.I.
Titanium coatings electrodeposited on metals from a carbamide-chloride melt
  • Summary: It has been found spectroscopic data that in the case of anodic (j = 30-50 мА/сm2) dissolution of titanium in carbamide-chloride melt (120-140 oС), quasi-octahedral complexes [Ti(CO(NH2)2)6]3+ of D4h symmetry with coordination by carbamide molecules through the nitrogen atom are formed. Electrodeposition of titanium up to 1 μm coating thickness with good adhesion to Fe, Cu, Mo substrates has been performed from a carbamide-cloride melt containing complex Ti(III) compounds and a soluble titanium anode.
  • Keywords: titanium, melt, coatings, X-ray, UV- Vis- spectroscopic.
  • pp.: 74 - 76

   

   

   

   

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