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AbstractAbstract
[en] Complex [Ce(Piv)3(HPiv)3]2 was prepared by precipitation of cerium(III) nitrate aqueous solution with salt NH4(Piv) (HPiv = pivalic acid) and subsequent recrystallization from 5% HPiv solution in hexane. According to data of X-ray diffraction analysis and IR spectroscopy crystal structure of the complex is built of centrally symmetric dimers, in which cerium atoms are bound by four bridge pivalate ligands. Thermal analysis suggests that heating of the complex in nitrogen atmosphere results first in splitting off six HPiv molecules in the range of 90-190 deg C and then in thermolysis of Ce(Piv)3 formed at 290-450 deg C. Sublimation of Ce(Piv)3 occurs in the range of 290-350 deg C along with thermolysis during heating in vacuum (0.01 mm Hg), which permits preparing CeO2 films by the method of chemical precipitation from gaseous phase
[ru]
Комплекс [Ce(Piv)3(HPiv)3]2 получен осаждением водного раствора нитрата церия(III) солью NH4(Piv) (HPiv = пивалевая кислота) и последующей перекристаллизацией из 5% раствора HPiv в гексане. По данным рентгеноструктурного анализа и ИК спектроскопии кристаллическая структура комплекса построена из центросимметричных димеров, в которых атомы церия связаны четырьмя мостиковыми пивалатными лигандами. Термический анализ показал, что нагревание комплекса в атмосфере азота приводит сначала к отщеплению шести молекул HPiv в интервале 90-190 град С, а затем к термолизу образовавшегося Ce(Piv)3 при 290-450 град С. При нагревании в вакууме (0.01 мм рт.ст.) в интервале 290-350 град С наряду с термолизом происходит сублимация Ce(Piv)3, что позволяет получать пленки CeO2 методом химического осаждения из газовой фазыOriginal Title
Sintez, kristallicheskaya struktura i termicheskaya ustojchivost' pivalata tseriya(III) sostava [Ce(Piv)3(HPiv)3]2 (HPiv - pivalevaya kislota)
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6 refs.; 2 tabs.; 2 figs.
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CARBOXYLIC ACIDS, CERIUM COMPOUNDS, CHALCOGENIDES, CHEMICAL COATING, CHEMICAL REACTIONS, COMPLEXES, CRYSTAL LATTICES, CRYSTAL STRUCTURE, DECOMPOSITION, DEPOSITION, EVAPORATION, MONOCARBOXYLIC ACIDS, ORGANIC ACIDS, ORGANIC COMPOUNDS, OXIDES, OXYGEN COMPOUNDS, PHASE TRANSFORMATIONS, RARE EARTH COMPLEXES, RARE EARTH COMPOUNDS, SPECTRA, SURFACE COATING, SYNTHESIS, THERMOCHEMICAL PROCESSES, YIELDS
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AbstractAbstract
[en] La(Acac)3Phen complex is synthetized, its X-tray structure analysis is carried out. Crystals are monoclinic ones, sp.gr. P21/n, a=17.11 (12), b=18.16 (3), c=17.86 (2) A, β=91.32 (2) deg, V=5548 (13) A3, Z=8. Structure contains two crystallographically non-equivalent types of molecules differing in interatomic distances and valent angles, as well as, in angles between ligand planes. Behaviour of La(Acac)3Phen at heating in vacuum (0.1-0.01 mm Hg) is studied. It is shown that under those conditions processes of Phen splitting, of sublimation and polymerization of La(Acac)3 lanthanum acetylacetonate formed following Phen splitting and that under 220 deg C during 30 min quantitative transition of La(Acac)3Phen into gas phase is reached. 10 refs., 2 figs., 3 tabs
Original Title
Letuchij raznoligandnyj kompleks lantana(3) s atsetilatsetonom i 1,10-fenantrolinom
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[en] Existence of previously disputed dihydrate of ytterbium tris-acetylacetonate YbAs-2H2O is proved by the methods of preparative chemistry, chemical, X-ray diffraction, X-ray phase and thermal analyses. The structure YbA3central dot2H2O contains monomer molecules unified in layers by hydrogen bonds. Coordination polyhedron of Yb atom is a slightly distorted square antiprism. Yb-O distances in dihydrate are much longer than in YbA3central dotH2O monohydrate. The absence of a correlation in bond lengths Yb-O, O-C and C-C in chelate cycles is pointed out, which proves mainly ionic type of metal-ligand bond in the given compounds. A scheme of muturl transitions of ytterbium tris-acetylacetonate hydrated is suggested, their thermodynamic stability being discussed. 9 refs., 3 figs., 3 tabs
Original Title
Gidraty tis-atsetilatsetonata itterbiya
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[en] Synthesis and X-ray diffraction analysis of praseodymium tris-pivalate adduct with α,α'-dipyridyl of PrPiv3Dipy composition were conducted. Coordination number of praseodymium atom equals 9 in central-symmetrical dimeric molecule. Praseodymium atoms are connected by two bidentate-bridge and two tridentate-bridge-cyclic carboxylic groups. Molecules of α.α'-Dipy form five-membered chelate cycles. 5 refs., 1 scheme, 1 tab
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Kristallicheskaya i molekulyarnaya struktura addukta pivalata prazeodima s α,α'-dipiridilom
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[en] The paper deals with the synthesis and X-ray diffraction investigation of praseodymium nitrate dipivalate adduct with o-phenanthroline of PrPiv2(NO3)Phen2 composition. The crystals are triclinic: a = 9.738(4), b = 11.860(5), c = 15.451(6) A, α = 91.80(2), β = 99.41(2), γ = 103.69(2) deg, sp. gr. P1, dcald = 1.490 g/cm3. The coordination number of praseodymium atom in a monomeric molecule equals 10, both carboxylate groups and nitrate ion are coordinated by the bidentate-cyclic method. Phenanthroline molecules are formed by five-membered chelate cycles in the process of coordination. 5 refs., 1 fig., 2 tab
Original Title
Kristallicheskaya i molekulyarnaya struktura addukta nitratodipivalata prazeodima s o-fenantrolinom
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[en] Solid mixed-ligand complexes (MLC) formed as a result of pivalic acid (HPiv) action on dipivaloylmethanates of holmium, erbium and ytterbium (MDpm3) in hexane, have been isolated. By the methods of IR spectroscopy and element analysis it has been ascertained that MLC of erbium and ytterbium have the composition MDpm3xHPiv, and in case of holmium a mixture of the complexes is formed. For HoDpm3xHPiv X-ray diffraction analysis has been carried out and its crystal structure has been refined. 7 refs.; 1 fig.; 4 tabs
Original Title
Sintez, stroenie i svojstva smeshanoligandnykh kompleksov RZEh, soderzhashchikh dipivaloilmetanatnyj i pivalatnyj ligand. Smeshanoligandnye kompleksy gol'miya, ehrbiya i itterbiya
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[en] Solid mixed-ligand complexes (MLC) formed under the action of pivalic acid (HPiv) on dipivaloylmethanates of Nd, Eu, Gd, Dy, Tb (MDpm3) in hexane have been isolated. On the basis of data of IR spectroscopic analysis it is ascertained that derivatives of neodymium, europium and gadolinium have the following composition MDpm2Piv · xHDpm (0 < x < 0.5), and in case of Dy and Tb a mixture of complexes of the composition MDpm3xHPiv and MDpm2PivxHDpm is formed X-ray diffraction analysis of [GdDpm2PivxH2O] and [Nd8Dpm8Piv6x(OH)6(CO3)(H2O)]x4H2O monocrystals prepared in the course of initial MLC recrystallization, has been performed. 3 refs.; 2 figs.; 5 tabs
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Sintez, stroenie i svojstva smeshanoligandnykh kompleksov RZEh, soderzhashchikh dipivaloilmetanatnyj i pivalatnyj ligandy. Smeshanoligandnye kompleksy neodima, evropiya, gadoliniya, doisproziya i terbiya
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[en] The structure of Ba(ReO4)2·4H2O crystals of monoclinic modification (a=7.371, b=12.572, c=12.156 A, β=90.09 deg, Z=4, sp.gr. P21/n) prepared at room temperature from aqueous solution was studied by the method of X-ray diffraction analysis
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Kristallicheskaya struktura i termicheskaya ustojchivost' tetragidrata perrenata bariya Ba(ReO4)2·4H2O
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[en] LaCl3x3ROH(1) compounds is prepared at interaction of metallic lanthanum or ''La(i-PrO3'' with HCl solution in ROH(Ri-Pr) dehydrated alcohol. Non-controlled hydration results in formation of LaCl3x2ROHxH2O (2) compound. Presence of [La2(ROH)6Cl4(μ-Cl)2 dymer molecules where CN equals to 7, is determined in 1 compound structure using X-ray structure analysis. [La(ROH)2(H2O)Cl(μ-Cl)2]n more stable polymer structure of 2 compound with LaCN equal to 8 results from slight substitution of water molecule for ROH one molecule. Structures of 1 and 2 compounds are compared with LaCl3x7H2O structure. 18 refs., 2 figs., 5 tabs
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O strukturakh sol'vatov khlorida lantana s izopropilovym spirtom
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[en] Anodic oxidation of Ta in isopropyl alcohol or prolonged reflux of the solution of Ta(OPri)5 in isopropyl alcohol yield binulear crystalline oxoisopropoxide Ta2O(OPri)8·PriOH (1). Its molecule providing the first example of oxoisopropoxide with only two metal atoms involves tantalum coordination octahedra fused alone a common edge. Complex 1 is stable in solution; on transition to the gas phase it is desolvated, thus forming rather stable Ta2O(OPri)8 species. Analogous molecules according to the mass spectral data exist in vapour phase over Ta(OAlk)5 (Alk = Me, Et, Pri and Bun). On heating of 1 in vacuo Ta(OPri) is sublimated. Heptanuclear complex Ta7O9(OPri)17 (2) is precipitated from the solution of 1 in isopropyl alcohol after prolonged storage. Its metal core is built of two tetrahedra [Ta4] sharing a common vertex. 20 refs., 3 figs., 6 tabs
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Oksoalkogolyaty tantala(5). Sintez i struktura
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