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2015

Number: 5

18721.
STRUCTURE, OPTICAL AND ELECTROCHEMICAL PROPERTIES OF BINUCLEAR COMPLEXES WITH PLATINATED 2-PHENYLBENZOTHIAZOL AND BRIDGING 2-MERCAPTO-DERIVATIVES OF PYRIDINE, PYRIMIDINE, BENZOTHIAZOLE, AND BENZOXAZOLE

E. A. Katlenok1, A. A. Zolotarev2, A. Yu. Ivanov2, S. N. Smirnov2, K. P. Balashev1
1Gertsen Russian State Pedagogical University, St. Petersburg, Russia
2St. Petersburg State University, St. Petersburg, Russia
Keywords: биядерные циклометаллированные комплексы Pt(II), РСА, ЯМР Н, Pt спектроскопия , электронная спектроскопия поглощения и испускания, вольтамперометрия окисления и восстановления, binuclear cyclometalated complexes of Pt(II), X-ray crystallography, Н , Pt NMR spectroscopy , electronic absorption and emission spectroscopy, redox voltammetry

Abstract >>
Binuclear [Pt(bt)m-(N^S)] 2 complexes (bt - is the deprotonated form of 2-phenylbenzothiazole, (N^S) - = 2-mercaptopyridineate, 2-mercaptopyrimidineate, 2-mercaptobenzothiazoleate, 2-mercaptobenzoxazoleate ions) are characterized by the following methods: X-ray crystallography, 1Н and 195Pt NMR spectroscopy, electronic absorption and emission spectroscopy, cyclic voltammetry. The occurrence of the Pt-Pt chemical bond and complexes in both crystalline state and solution in the form of cis -N (bt),S-binding isomers with the asymmetrical arrangement of two cyclometalated and two bridging ligands is shown. Long-wavе absorption bands and luminescence of the complexes in the red spectral range are due to spin-allowed and spin-forbidden optical charge transfer transitions from the metal-metal bond to the metalated ligand. In cyclic voltammetry, two-electron redox waves of the complexes are attributed to metal- and ligand-centered processes involving s* HOMO and p*(bt) LUMO of the complexes.



Number: 5

18722.
GAS-PHASE DEPOSITION OF COMPLEX HIGH-MELTING COATINGS ON CARBON FIBER MATERIAL

V. V. Lozanov1, N. I. Baklanova1, N. B. Morozova2
1Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
Keywords: осаждение из газовой фазы, карбид гафния, иридий, покрытия, углеродный волокнистый материал, vapor deposition, hafnium carbide, iridium, coatings, carbon fiber material

Abstract >>
The possibility of modifying carbon materials by RCVD and MOCVD of complex high-melting coatings consisting of the inner hafnium carbide layer and the outer iridium layer is studied. The morphological features, microstructure, and phase composition of the carbide and complex HfC-Ir coating on a carbon material are examined by scanning electron microscopy and powder X-ray diffraction analysis. The HfC coating is uniform, continuous, repeating the geometry of a carbon substrate. A scheme of chemical reactions describing the processes of hafnium transfer on carbon in the form of gaseous hafnium fluorides with a lower valence is proposed. The iridium coating consists of slightly elongated crystallites and has a good adhesion to the carbide layer.



Number: 5

18723.
CRYSTAL STRUCTURE OF TWO IONIC SPARFLOXACIN COMPOUNDS

A. D. Vasiliev1,2, N. N. Golovnev1
1Siberian Federal University, Krasnoyarsk, Russia
2Kirensky Institute of Physics, Siberian Branch, Russian Academy of Sciences, Krasnoyarsk, Russia
Keywords: кристаллическая структура, катион спарфлоксациниума, π-π-взаимодействие, тетрагалогенид-анионы цинка и кадмия, crystal structure, sparfloxacindi-ium cation, zinc and cadmium tetrahalide anions, hydrogen bonds, π-π interaction

Abstract >>
The structure of two new ionic compounds of sparfloxacin (C 19H 22F 2N 4O 3, SfH), SfH 3[ZnCl 4]×1.5H 2O (I) and SfH 3[CdBr 4]×H 2O (II), is determined. Crystallographic data are as follows: for I a = 14.505(3) Å, b = 12.615(3) Å, c = 29.118(7) Å, V = 5254(4)Å 3, space group Pbca , Z = 8; for II a = 13.2822(5) Å, b = 10.2564(4) Å, c = 21.3250(8) Å, b = 100.7248(4)°, V = 2854.3(3) Å 3, space group P 2 1/ n , Z = 4. The structures of the compounds are stabilized by intra- and intermolecular hydrogen bonds and the structure of I is additionally stabilized by the p-p interaction between the SfH ions.



Number: 5

18724.
TWO ISOMERIC STRUCTURES OF OXOVANADIUM(V) COMPLEXES WITH HYDRAZONE AND 8-HYDROXYQUINOLINE LIGANDS

G.-H. Sheng1, X.-S. Cheng2, Z.-L. You2, H.-L. Zhu1
1Shandong University of Technology, Zibo, P. R. China
2Liaoning Normal University, Dalian, P. R. China
Keywords: hydrazone ligand, 8-hydroxyquinoline, oxovanadium complex, crystal structure, thermal property

Abstract >>
Two new oxovanadium(V) complexes [VOL 1(HQ)] (1) and [VOL 2(HQ)] (2) are prepared by the reaction of [VO(acac) 2] (where acac = acetylacetonate), 8-hydroxyquinoline (HHQ) with 4-bromo- N'-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide (H 2L 1) and 2-bromo- N'-(3-ethoxy-2-hydroxybenzylidene)benzohydrazide (H 2L 2), respectively, in methanol. Crystal and molecular structures of the complexes are determined by elemental analysis, infrared spectroscopy, and single crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P 2 1/ c , with unit cell dimensions a = 12.5236(13) Å, b = 22.5260(15) Å, c = 16.7029(13) Å, b = 90.054(2)°, V = 4712.0(7) Å 3, Z = 8, GOOF = 1.024, R 1 = 0.0586 and wR 2 = 0.0835. Complex 2 crystallizes in the triclinic space group P -1, with unit cell dimensions a = 7.4344(12) Å, b = 10.8677(16) Å, c = 14.687(2) Å, α = 85.327(5)°, β = 77.357(5)°, γ = 84.896(5)°, V = 1150.9(3) Å 3, Z = 2, GOOF = 1.153, R 1 = 0.0917 and wR 2 = 0.3014. The V atoms are in the octahedral coordination. Thermal stability of the complexes is also studied.



Number: 5

18725.
X-RAY STRUCTURE OF AN AMIDE-APPENDED CHLOROMERCURATED DERIVATIVE OF 2-PHENYLQUINOLINE

C.-Y. Lin, W. Henderson, B.K. Nicholson
University of Waikato, Hamilton, New Zealand
Keywords: synthesis, mercury complexes, orthometallation reactions, crystal structure

Abstract >>
Reaction of the morpholine amide derivative of 2-phenyl-4-quinolinecarboxylic acid with mercury(II) acetate and lithium chloride results in chloromercuration at the ortho position on the phenyl ring; the complex was characterised by ESI mass spectrometry and an X-ray structure determination.



Number: 5

18726.
MOLECULAR STRUCTURE OF 3-OXO-URS-12-EN-28-OIC ACID ANHYDRIDE

N. I. Medvedeva1, K. Yu. Suponitskii2, T. V. Lopatina1, A. N. Lobov1, A. I. Poptsov1, O. B. Kazakova1
1Institute of Organic Chemistry, Ufa Scientific Centre, Russian Academy of Sciences, Ufa, Russia
2Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow, Russia
Keywords: ангидрид 3-оксо-урс-12-ен-28-овой кислоты, синтез, рентгеноструктурный анализ, 3-oxo-urs-12-en-28-oic acid anhydride, synthesis, single crystal X-ray diffraction analysis

Abstract >>
The molecular structure of 3-oxo-urs-12-en-28-oic acid anhydride is determined. Crystals of C 60H 90O 5 compound (III) are monoclinic, space group С2, at 100 K a = 15.1308(13) Å, b = 23.5150(19) Å, c = 15.1275(12) Å, β = 108.276(2)°. Molecules in the crystal are located in a special position on axis 2.



Number: 5

18727.
CRYSTAL HYDRATES OF ORGANIC COMPOUNDS

A. M. Banaru, Yu. L. Slovokhotov
Lomonosov Moscow State University, Moscow, Russia
Keywords: кристаллогидрат, водный ассоциат, планарный граф, протоноизбыточность, crystal hydrate, water associate, planar graph, proton excess

Abstract >>
Structures of different classes of organic crystal hydrates are considered and their structural classification is presented based on the dimensionality and planarity of the included (Н 2О) n motif (water associate). The structural data are generalized with respect to the proton excess of the water associate.



Number: 5

18728.
CRYSTALLOGRAPHIC ANALYSIS OF THE STRUCTURE OF SCANDIUM BOROCARBOSILICIDE. HIERARCHY IN THE HIGHLY SYMMETRICAL ORDERING OF ATOMIC GROUPS AND ATOMS

S. V. Borisov, S. A. Magarill, N. V. Pervukhina
Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
Keywords: кристаллографический анализ, катионные и анионные подрешетки, борокарбосилицид скандия, иерархия упорядочения, crystallographic analysis, cation and anion sublattices, scandium borocarbosilicide, ordering hierarchy

Abstract >>
A crystallographic analysis of the highly symmetrical cubic structure of Sc 0,8B 9,64C 0,53Si 0,057 is conducted of both centers of the [B 12] and [B 10] cluster groups with Sc and Si atoms and separately all individual atoms. In the first case, the analysis reveals an ordering with an I cub sublattice ( а ≈ 5.1 Å) and a competing ordering with an F cub sublattice ( а ≈ 6.8 Å). In the second case (for individual atoms), the analysis reveals orderings with analogous sublattices with twice as small parameters.



Number: 5

18729.
STRUCTURE OF THE PRODUCT OF 1,8-DIAZABICYCLO[5.4.0]UNDECANE-7-ENE SUBSTITUTION FOR CHLORINE ATOMS IN DICHLORINE SUBSTITUTED Fe(II) CLATHROCHELATE

M. A. Vershinin1, A. B. Burdukov1, N. V. Pervukhina1, I. V. Eltsov2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: клатрохелаты, нуклеофильное замещение, РСА, ЯМР, clathrochelates, nucleophilic substitution, single crystal X-ray diffraction, NMR spectroscopy

Abstract >>
Methods of X-ray diffraction analysis and nuclear magnetic resonance are used to determine the molecular structure of macrobicyclic boron-capped tris -dioxymate iron(II) clathrochelate containing an annellated 5-membered heterocycle.



Number: 5

18730.
CRYSTAL STRUCTURE OF THE INCLUSION COMPOUND OF A POROUS METAL-ORGANIC POLYMER WITH 2-CYCLOPENTENE-1-ONE

I. S. Khan1,2, D. G. Samsonenko1,2, V. P. Fedin1,2
1Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2Novosibirsk National Research State University, Novosibirsk, Russia
Keywords: кристаллическая структура, пористые координационные полимеры, соединение включения, цинк, crystal structure, porous coordination polymers, inclusion compounds, zinc

Abstract >>
The inclusion compound of the composition [Zn 2(dmf)(bdc)(lac)]×C 5H 6O is obtained by keeping a porous homochiral metal-organic polymer of the composition [Zn 2(dmf)(bdc)(lac)]·DMF (DMF = N,N-dimethylformamide, H 2bdc = terephthalic acid, H 2lac = S -lactic acid) in liquid 2-cyclopentene-1-one, and the crystal structure of the compound is determined.




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