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Sample records for title compound c22h18os

  1. Triosmium cluster compounds containing isocyanide and hydride ligands. Crystal and molecular structure of (μ-H)(μ-eta1-C==N(H)(t-C4H9))Os3(CO)10

    International Nuclear Information System (INIS)

    Adams, R.D.; Golembeski, N.M.

    1979-01-01

    The crystal and molecular structure of the compound (μ-H)(μ-eta 1 -C==N(H)(t-C 4 H 9 ))Os 3 (CO) 10 has been determined by X-ray crystallographic methods. The compound crystallizes in the centrosymmetric monoclinic space group P2 1 /n[C/sub 2h/ 5 ]:a = 13.651 (4) A, b = 9.156 (4) A, c = 18.275 (5) A, β = 111.42 (2) 0 , V = 2126.3 (25) A 3 , Z = 4, rho/sub calcd/ = 2.92 g cm -3 . A uniform triangular cluster of three osmium atoms contains ten linear carbonyl groups and a μ-eta 1 -C==N(H)(t-C 4 H 9 ) iminyl ligand. The carbon atom of the iminyl ligand symmetrically bridges one osmium-osmium bond, as is shown by the internuclear separations Os(2)-C(11) = 2.066 (8) A and Os(3)-C(11) = 2.043 (8) A. The iminyl bond, C(11)-N, is double with the C-N distance being 1.298 (10) A

  2. Triosmium cluster compounds containing isocyanide and hydride ligands. Crystal and molecular structures of (μ-H)(H)Os3(CO)10(CN-t-C4H9) and (μ-H)2Os3(CO)9(CN-t-C4H9)

    International Nuclear Information System (INIS)

    Adams, R.D.; Golembski, N.M.

    1979-01-01

    The structures of the compounds (μ-H)(H)Os 3 (CO) 10 (CN-t-C 4 H 9 ) and (μ-H) 2 Os 3 (CO) 9 (CN-t-C 4 H 9 ) have been revealed by x-ray crystallographic techniques. For (μ-H)(H)Os 3 (CO) 10 (CN-t-C 4 H 9 ): a = 9.064 (3), b = 12.225 (3), c = 20.364 (4) A; β = 98.73 (3) 0 ; space group P2 1 /c[C/sub 2h/ 5 ], No. 14; Z = 4; d/sub calcd/ = 2.79 g cm -3 . This compound contains a triangular cluster of three osmium atoms; Os(1)--Os(2) = 2.930 (1) A, Os(1)--Os(3) = 2.876 (1) A, and Os(2)--Os(3) = 3.000 (1) A. There are ten linear terminal carbonyl groups and one linear terminal isocyanide ligand which occupies an axial coordination site. The hydrogen atoms were not observed crystallographically, but their positions are strongly inferred from considerations of molecular geometry. For (μ-H) 2 Os 3 (CO) 9 (CN-t-C 4 H 9 ): a = 15.220 (8), b = 12.093 (6), c = 23.454 (5) A; space group Pbcn [D/sub 2h/ 14 ], No. 60; Z = 8; d/sub calcd/ = 2.79 g cm -3 . The compound is analogous to the parent carbonyl (μ-H) 2 Os 3 (CO) 10 and has two normal and one short osmium--osmium bonds: Os(1)--Os(2) = 2.827 (1) A, Os(1)--Os(3) = 2.828 (1) A, Os(2)--Os(3) = 2.691 (1) A. The isocyanide ligand resides in an equatorial coordination site on osmium Os(2). The hydrogen atoms were not observed but are believed to occupy bridging positions as in the parent carbonyl complex. 2 figures, 7 tables

  3. The synthesis of the 2H, 3H, and 14C-isotopomers of 2'-deoxy-2',2'-difluorocytidine hydrochloride, an anti-tumor compound

    International Nuclear Information System (INIS)

    Wheeler, W.J.; Mabry, T.E.; Jones, C.D.

    1991-01-01

    The 2 H, 3 H, and 14 C-isotopomers of 2'-deoxy-2', 2'-difluorocytidine hydrochloride (gemcitabine hydrochloride) have been synthesized in two radiochemical steps from the reaction of bis-trimethylsilylcytosine-[2- 14 C] and 3,5-O-bis-benzoyl-1-O-methanesulfonyl-2-deoxy-2,2-difluororibose. A mixture of anomers of 3',5'-dibenzoyl-2'-deoxy-2',2'-difluorocytidine or its 14 C-isotopomer were obtained which were readily separated by crystallization from ethyl acetate. Deprotection using methanolic ammonia yielded the target compound. The 2 H and 3 H-isotopomers were prepared by deuterium (or tritium) gas hydrogenolysis of 5-iodo-2'-deoxy-2',2'-difluorocytidine. (author)

  4. Structure elucidation of 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C23H18Cl2N4OS from synchrotron X-ray powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül

    2017-12-01

    The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C23H18Cl2N4OS compound was synthesized, as a member of the family of novel potential anticancer agents. The structure of the title compound was characterized by IR,1H-NMR, mass spectroscopy, and elemental analysis, previously. In this study, the crystal structure of this compound has been determined from synchrotron X-ray powder diffraction data. The crystal structure was solved by simulated annealing and the final structure was achieved by Rietveld refinement method using soft restrains on all interatomic bond lengths and angles. This compound crystallizes in space groupP21,Z= 2, with the unit-cell parametersa= 15.55645(11) Å,b= 8.61693(6) Å,c= 8.56702(6) Å,β= 104.3270(4)°, andV= 1112.68(1) Å3. In the crystal structure, strong C-H∙∙∙πand weak intermolecular hydrogen-bonding interactions link the molecules into a three-dimensional network. The molecules are in a head-to-head arrangement in the unit cell.

  5. Diaqua{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolato-κ2O,N,N′,O′}manganese(III perchlorate 18-crown-6 hemisolvate monohydrate

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    Ming-Ming Yu

    2009-02-01

    Full Text Available In the cation of the title compound, [Mn(C18H18N2O4(H2O2]ClO4·0.5C12H24O6·H2O, the MnIII ion is coordinated by two water O atoms, and two O atoms and two N atoms from the tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolate ligand, completing a distorted octahedral geometry. One O atom of the 18-crown-6-ether is disordered over two positions with occupancies of 0.70 (2 and 0.30 (2.

  6. Synthesis and X-ray crystal structure of (OsO(3)F(2))(2)2XeOF(4) and the Raman spectra of (OsO(3)F(2))(infinity), (OsO(3)F(2))(2), and (OsO(3)F(2))(2)2XeOF(4).

    Science.gov (United States)

    Hughes, Michael J; Mercier, Hélène P A; Schrobilgen, Gary J

    2009-05-18

    The adduct, (OsO(3)F(2))(2)2XeOF(4), was synthesized by dissolution of the infinite chain polymer, (OsO(3)F(2))(infinity), in XeOF(4) solvent at room temperature followed by removal of excess XeOF(4) under dynamic vacuum at 0 degrees C. Continued pumping at 0 degrees C resulted in removal of associated XeOF(4), yielding (OsO(3)F(2))(2), a new low-temperature phase of OsO(3)F(2). Upon standing at 25 degrees C for 1(1)/(2) h, (OsO(3)F(2))(2) underwent a phase transition to the known monoclinic phase, (OsO(3)F(2))(infinity). The title compounds, (OsO(3)F(2))(infinity), (OsO(3)F(2))(2), and (OsO(3)F(2))(2)2XeOF(4) have been characterized by low-temperature (-150 degrees C) Raman spectroscopy. Crystallization of (OsO(3)F(2))(2)2XeOF(4) from XeOF(4) solution at 0 degrees C yielded crystals suitable for X-ray structure determination. The structural unit contains the (OsO(3)F(2))(2) dimer in which the OsO(3)F(3) units are joined by two Os---F---Os bridges having fluorine bridge atoms that are equidistant from the osmium centers (2.117(5) and 2.107(4) A). The dimer coordinates to two XeOF(4) molecules through Os-F...Xe bridges in which the Xe...F distances (2.757(5) A) are significantly less than the sum of the Xe and F van der Waals radii (3.63 A). The (OsO(3)F(2))(2) dimer has C(i) symmetry in which each pseudo-octahedral OsO(3)F(3) unit has a facial arrangement of oxygen ligands with XeOF(4) molecules that are only slightly distorted from their gas-phase C(4v) symmetry. Quantum-chemical calculations using SVWN and B3LYP methods were employed to calculate the gas-phase geometries, natural bond orbital analyses, and vibrational frequencies of (OsO(3)F(2))(2), (OsO(3)F(2))(2)2XeOF(4), XeOF(4), OsO(2)F(4), and (mu-FOsO(3)F(2))(2)OsO(3)F(-) to aid in the assignment of the experimental vibrational frequencies of (OsO(3)F(2))(2), (OsO(3)F(2))(2)2XeOF(4), and (OsO(3)F(2))(infinity). The vibrational modes of the low-temperature polymeric phase, (OsO(3)F(2))(infinity), have been

  7. 1-Methoxy-3-o-tolylbicyclo[2.2.2]oct-5-ene-2,2-dicarbonitrile

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    Orhan Büyükgüngör

    2009-09-01

    Full Text Available In the title compound, C18H18N2O, the cyclohexene and cyclohexane rings of the bicyclo[2.2.2]oct-5-ene unit adopt distorted boat conformations. In the crystal, molecules exist as C—H...N hydrogen-bonded centrosymmetric R22(14 dimers, which are further linked by C—H...π interactions.

  8. (Z-3-Benzyl-2-[(2-phenylcyclohex-2-enylimino]-1,3-thiazolidin-4-one

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    Chin Wei Ooi

    2012-08-01

    Full Text Available The title compound, C22H22N2OS, exists in a Z configuration with respect to the N=C bond. The cyclohexene ring adopts a distorted sofa conformation. The thiazolidine ring is essentially planar, with a maximum deviation of 0.030 (2 Å, and forms dihedral angles of 76.66 (6 and 74.55 (6° with the terminal phenyl rings. The dihedral angle between the phenyl rings is 71.55 (7°. In the crystal, a C—H...π interaction is observed.

  9. Synthesis, characterization, electrochemical investigation and antioxidant activities of a new hybrid cyclohexaphosphate: Cu1.5Li(C2H10N2)P6O18·7H2O

    Science.gov (United States)

    Sleymi, Samira; Lahbib, Karima; Rahmouni, Nihed; Rzaigui, Mohamed; Besbes-Hentati, Salma; Abid, Sonia

    2017-09-01

    A new organic-inorganic hybrid transition metal phosphate, Cu1.5Li(C2H10N2)P6O18·7H2O, has been prepared and characterized by X-ray diffraction, spectroscopy (infrared, Raman, diffuse reflectance and UV-Vis) and thermal analysis (TG). In addition, its electrochemical behaviors, as well as its antioxidant and antibacterial activities, have been investigated. Its structure is built up by the alternate linkages between copper and phosphate polyhedra, forming puckered layers with intersecting 12-membered rings, in which the ethylenediammonium cations reside. This compound is the first framework structure constructed from cyclohexaphosphates and three distinct copper cations. Cyclic voltammetry study in an acetonitrile solution reveals the facile anodic oxidation of its organic part on a platinum disk and a progressive growing of a thin film, though the repetitive cycling of potential. The title compound was tested for its in vitro antioxidant activities by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2‧-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), Ferrous chelating ability (FIC) and Ferric Reducing Power (FRP) methods. The antioxidant activity of Cu1.5Li(C2H10N2)P6O18·7H2O was analyzed simultaneously with its antibacterial capacity against Escherichia coli, Salmonella typhimurium, Staphylococus aureus, Enterococcus feacium, Streptococcus agalactiae and Candida albicans. The tested compound showed significant antioxidant activities with low antibacterial properties.

  10. The nido-osmaboranes [2,2,2-(CO)(PPh(3))(2)-nido-2-OsB(5)H(9)] and [6,6,6-(CO)(PPh(3))(2)-nido-6-OsB(9)H(13)].

    Science.gov (United States)

    Bould, J; Kennedy, J D; Thomas, R L; Rath, N P; Barton, L

    2001-11-01

    The structural characterization of the osmahexaborane 2-carbonyl-2,2-bis(triphenylphosphine)-nido-2-osmahexaborane(9), [Os(B(5)H(9))(C(18)H(15)P)(2)(CO)], (I), a metallaborane analogue of B(6)H(10), confirms the structure proposed from NMR spectroscopy. The structure of the osmadecaborane 6-carbonyl-6,6-bis(triphenylphosphine)-nido-6-osmadecaborane(13), [Os(B(9)H(13))(C(18)H(15)P)(2)(CO)], (IV), is similarly confirmed. The short basal B-B distance of 1.652 (8) A in (I), not bridged by an H atom, mirrors that in the parent hexaborane(10) [1.626 (4) A].

  11. Vibrational spectrum of solid picene (C22H14)

    International Nuclear Information System (INIS)

    Joseph, B; Capitani, F; Boeri, L; Malavasi, L; Artioli, G A; Protti, S; Fagnoni, M; Albini, A; Marini, C; Baldassarre, L; Perucchi, A; Lupi, S; Postorino, P; Dore, P

    2012-01-01

    Recently, Mitsuhashi et al observed superconductivity with a transition temperature up to 18 K in potassium doped picene (C 22 H 14 ), a polycyclic aromatic hydrocarbon compound (Mitsuhashi et al 2010 Nature 464 76). Theoretical analysis indicates the importance of electron-phonon coupling in the superconducting mechanisms of these systems, with different emphasis on inter- and intra-molecular vibrations, depending on the approximations used. Here we present a combined experimental and ab initio study of the Raman and infrared spectrum of undoped solid picene, which allows us to unambiguously assign the vibrational modes. This combined study enables the identification of the modes which couple strongly to electrons and hence can play an important role in the superconducting properties of the doped samples. (fast track communication)

  12. Photochemically activated antiviral halogenated 1,8-naphthalimides: synthesis of N,N'-bis-{2-[(5-bromo-2-[1-14C]hexyl-1H-benz[de]isoquinolin-1,3(2H)-dion-6-yl)amino]ethyl}hexanediamide

    International Nuclear Information System (INIS)

    Hayes, B.A.; Gupta, Surendra; Shaochieh Chang; Utecht, R.E.; Lewis, D.E.

    1996-01-01

    The synthesis of N,N'-bis-{2-[(5-bromo-2-[1- 14 C]hexyl-1H-benz[de]isoquinolin-1, 3(2H)-dion-6-yl)amino]ethyl}hexanediamide from 1-[1- 14 C]-hexylamine and 4-chloro-1,8-naphthalic anhydride is described. The anhydride is first converted to the 4-chloro-n-[1- 14 C]hexyl-1,8-naphthalimide by condensation with 1-[1- 14 C]-hexylamine, and the chlorine is then displaced with ethylenediamine to give the 4-(2-aminoethylamino-N-[1- 14 C]hexyl-1,8-naphthalimide. Coupling of this monomeric naphthalimide with adipoyl chloride affords the dimeric naphthalimide which is brominated regiospecifically with elemental bromine in carbon tetrachloride to afford the title compound. (author)

  13. Triaquabis(1H-imidazolebis[μ2-2-(oxaloaminobenzoato(3−]dicopper(IIcalcium(II heptahydrate

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    Peng Zhang

    2008-02-01

    Full Text Available In the title heterotrinuclear coordination compound, [CaCu2(C9H4NO52(C3H4N22(H2O3]·7H2O, the Ca2+ cation is in a pentagonal–bipyramidal geometry and bridges two (1H-imidazole[2-(oxaloaminobenzoato(3−]copper(II units in its equatorial plane. Each CuII atom has a normal square-planar geometry. The molecule has approximate local (non-crystallographic mirror symmetry and 23 classical hydrogen bonds are found in the crystal structure.

  14. Bis{1,2-bis[bis(3-methoxypropylphosphanyl]ethane-κ2P,P′}dichloridoosmium(II

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    Nathaniel K. Szymczak

    2011-12-01

    Full Text Available In the centrosymmetric title compound, [OsCl2(C18H40O4P22], the OsII atom adopts a trans-OsCl2P4 geometry, arising from its coordination by two chelating diphosphane ligands and two chloride ions. One of the methoxy side chains of the ligand is disordered over two orientations in a 0.700 (6:0.300 (6 ratio.

  15. Study of complex formation between C18H36N2O6 and UO22+ cation in some binary mixed non-aqueous solutions

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    G.H. Rounaghi

    2017-02-01

    Full Text Available The complexation reaction between UO22+ cation and the macrobicyclic ligand C18H36N2O6 was studied in acetonitrile–dimethylformamide (AN–DMF, acetonitrile–tetrahydrofuran (AN–THF, acetonitrile–dichloromethane (AN–DCM binary solvent solutions at different temperatures using the coductometric method. In most cases, C18H36N2O6 forms a 1:1 [M:L] complex with the UO22+ cation. But in some of the studied solvent systems, in addition to formation of a 1:1 complex, a 1:2 [M:L2] complex is formed in solution. A non-linear behavior was observed for changes of logKf of the (C18H36N2O6·UO22+ complex versus the composition of the binary mixed solvents. The sequence of the stability of the (C18H36N2O6·UO22+ complex in pure solvent systems at 25 °C decreases in the order: AN > THF > DMF. In the case of binary solvent solutions, the stability constant of the complex at 25 °C was found to be: AN–DCM > AN–THF > AN–DMF. The values of thermodynamic quantities (ΔSc°,ΔHc°, for the formation of the complex were obtained from temperature dependence of the stability constant of the complex using the van't Hoff plots. The results show that in all cases, the complex is both entropy and enthalpy stabilized and both of these parameters are affected by the nature and composition of the mixed solvent systems.

  16. Bis{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(iminomethylene]diphenolato(1.5−-κ4O,N,N′,O′}praeseodymium(III

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    Da-Qi Wang

    2009-02-01

    Full Text Available The title compound, [Pr(C18H22.5N2O42], is isotypic with its Er and Tb analogues. All interatomic distances, angles and the hydrogen bond geometry are very similar for the three structures..

  17. 1,5-Dimethyl-2-phenyl-1H-pyrazol-3(2H-one–4,4′-(propane-2,2-diylbis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one] (1/1

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    Krzysztof Lyczko

    2013-01-01

    Full Text Available The asymmetric unit of the title compound, C11H12N2O·C25H28N4O2, contains two different molecules. The smaller is known as antipyrine [systematic name: 1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one] and the larger is built up from two antypirine molecules which are connected through a C atom of the pyrazolone ring to a central propanyl part [systematic name: 4,4′-(propane-2,2-diylbis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one]. Intramolecular C—H...O hydrogen bonds occur in the latter molecule. In the crystal, C—H...O hydrogen bonds link the molecules into a two-dimensional network parallel to (001.

  18. (E-2-(5-Chloro-2-hydroxybenzylidene-N-cyclohexylhydrazine-1-carbothioamide

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    Md. Azharul Arafath

    2017-01-01

    Full Text Available In the title compound, C14H18ClN3OS, the phenol ring is almost coplanar with the hydrazinecarbothioamide moiety, making a dihedral angle of 6.92 (8°. The cyclohexane ring has a chair conformation and the conformation about the C=N bond is E. In the crystal, molecules are linked by N—H...O and O—H...S hydrogen bonds, forming inversion dimers with an R22(14 ring motif flanked by two R22(6 ring motifs. The dimers are linked by short Cl...Cl interactions, forming layers parallel to the ab plane.

  19. 2-[3-(4-Methoxyphenyl-1-phenyl-1H-pyrazol-5-yl]phenol

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    2009-03-01

    Full Text Available The title compound, C22H18N2O2, was derived from 1-(2-hydroxyphenyl-3-(4-methoxyphenylpropane-1,3-dione. The central pyrazole ring forms dihedral angles of 16.83 (5, 48.97 (4 and 51.68 (4°, respectively, with the methoxyphenyl, phenyl and hydroxyphenyl rings. The crystal packing is stabilized by O—H...N hydrogen bonding.

  20. Fragmentations and rearrangements of metastable [C2H5OS]+ ions

    NARCIS (Netherlands)

    de Vries, Marcel; Oudman, D; Weringa, WD

    1992-01-01

    Several [C2H5OS]+ ions with different structures were generated from the appropriate precursors and their metastable ion spectra were determined. Deuterium labelled analogues of some of the [C2H5OS]+ ions were used to elucidate the nature of the observed fragmentations and their mechanisms.

  1. Aquachlorido{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolato-κ2O1,N,N′,O1′}cobalt(III dimethylformamide monosolvate

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    Yun Wei

    2012-04-01

    Full Text Available In the title compound, [Co(C18H18N2O4Cl(H2O]·C3H7NO, the CoIII ion is six-coordinated by a tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolate ligand, with a chloride ion and an aqua ligand in the apical positions. The compound crystallized as a dimethylformamide (DMF monosolvate. In the crystal, complex molecules are linked via O—Hwater...O hydrogen bonds to form a dimer-like arrangement. These dimers are linked via a C—H...Cl interaction, and the DMF molecule is linked to the complex molecule by C—H...O interactions.

  2. (4Z-4-[1-(2-Aminoanilinoethylidene]-3-methyl-1-phenyl-4,5-dihydro-1H-pyrazol-5-one

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    Mohamed Samba

    2017-02-01

    Full Text Available The conformation of the title compound, C18H18N4O, is partly determined by an intramolecular N—H...O hydrogen bond that imposes planarity on the central aminoethylidene-3-methylpyrazol-5-one segment of the molecule. In the crystal, N—H...O hydrogen and N—H...N hydrogen bonds both form centrosymmetric dimers that enclose R22(18 rings. These, together with C—H...N and π–π stacking interactions between centrosymmetrically related pyrazalone rings, stack the molecules along the b-axis direction.

  3. 4-(2,4-Dichlorophenyl-2-(1H-indol-3-yl-6-methoxypyridine-3,5-dicarbonitrile

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    M. N. Ponnuswamy

    2008-10-01

    Full Text Available In the title compound, C22H12Cl2N4O, the indole ring system and the benzene ring form dihedral angles of 21.18 (7° and 68.43 (8°, respectively, with the pyridine ring. The methoxy group is coplanar with the pyridine ring. In the crystal structure N—H...N intermolecular hydrogen bonds link the molecules into C(10 chains running along [011]. Intramolecular C—H...N hydrogen bonds are also observed.

  4. Radical C-H functionalization to construct heterocyclic compounds.

    Science.gov (United States)

    Yu, Jin-Tao; Pan, Changduo

    2016-02-07

    Heterocyclic compounds are widely present in natural products, pharmaceuticals and bioactive molecules. Thus, organic and pharmaceutical chemists have been making extensive efforts to construct those heterocyclic frameworks through developing versatile and efficient synthetic strategies. The direct C-H functionalization via the radical pathway has emerged as a promising and dramatic approach towards heterocycles with high atom- and step-economy. Heterocyclic compounds such as coumarins, furans, benzofurans, xanthones, benzothiazoles, indoles, indolines, oxindoles, quinolines, isoquinolines, quinoxaline, and phenanthridines have been successfully synthesized by C-H functionalization through the radical pathway. In this review, recent advances on radical C-H functionalization to construct heterocyclic compounds are highlighted with discussions.

  5. Bis{μ-2,2′-[1,1′-(ethane-1,2-diyldinitrilodiethylidyne]diphenolato-κ5O,N,N′,O′:O}bis[chloridomanganese(III

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    Robert D. Pike

    2008-02-01

    Full Text Available The title compound, [Mn2(C18H18N2O22Cl2], was synthesized by the reaction between manganese(II o-chlorobenzoate and the Schiff base generated in situ by the condensation of ethane-1,2-diamine and o-hydroxyacetophenone. The centrosymmetric dimer contains two Jahn–Teller-distorted manganese(III ions, each in an octahedral geometry, connected through two phenoxy bridges from two ligands.

  6. 1,4-Dimethyl-3-phenyl-3H-pyrazolo[3,4-c]isoquinolin-5(4H-one

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    Giuseppe Daidone

    2008-05-01

    Full Text Available The title compound, C18H15N3O, is the product of the thermal decomposition of the diazonium salt derived from 2-amino-N-methyl-N-(3-methyl-1-phenyl-1H-pyrazol-5-ylbenzamide. It is characterized by a trans orientation of the methyl groups with respect to the tricyclic ring system. The molecule has a nearly planar phenylpyrazolo[3,4-c]isoquinolin-5-one system, the largest deviation from the mean plane being 0.066 (2 Å for the O atom. The dihedral angle between the phenyl substituent and the heterotricycle is 67 (1°. The packing is stabilized by C—H...N hydrogen-bond interactions, with the formation of molecular chains along the c axis.

  7. Homoleptic Diphosphacyclobutadiene Complexes [M(η4-P2C2R2)2]x- (M=Fe, Co; x=0, 1)

    NARCIS (Netherlands)

    Wolf, Robert; Ehlers, A.W.; Khusniyarov, M.M.; Hartl, F.; de Bruin, B.; Long, G.J.; Grandjean, F.; Schappacher, F.M.; Pöttgen, R.; Slootweg, J.C.; Lutz, M.; Spek, A.L.; Lammertsma, K.

    2011-01-01

    The preparation and comprehensive characterization of a series of homoleptic sandwich complexes containing diphosphacyclobutadiene ligands are reported. Compounds [K([18]crown-6)ACHTUNGTRENUNG(thf)2][Fe(η4- P2C2tBu2)2] (K1), [K([18]crown-6)- ACHTUNGTRENUNG(thf)2][Co(h4-P2C2tBu2)2] (K2), and

  8. Aquachlorido{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolato-κ2O1,N,N′,O1′}cobalt(III monohydrate

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    Jianxin Xing

    2009-04-01

    Full Text Available The title compound, [Co(C18H18N2O4Cl(H2O]·H2O, contains a distorted octahedral cobalt(III complex with a 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolate ligand, a chloride and an aqua ligand, and also a disordered water solvent molecule (half-occupancy. The CoIII ion is coordinated in an N2O3Cl manner. Weak O—H...O hydrogen bonds may help to stabilize the crystal packing.

  9. 3-Isobutyl-4-phenylsulfanyl-1H-pyrazol-5-ol

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    Tara Shahani

    2011-02-01

    Full Text Available The asymmetric unit of the title compound, C13H16N2OS, contains two independent molecules (A and B. The pyrazole ring [maximum deviations = 0.0049 (17 Å in molecule A and 0.0112 (19 Å in molecule B] makes a dihedral angle of 70.23 (11 and 73.18 (12° with the phenyl ring in molecules A and B, respectively. The isobutyl group in molecule B is disordered over two sets of sites with a ratio of refined occupancies of 0.858 (5:0.142 (5. In the crystal, molecules A and B are linked via a pair of intermolecular N—H...O hydrogen bonds, generating an R22(8 ring motif. These ring motifs are further linked into two-dimensional arrays parallel to the bc plane by intermolecular N—H...O and weak C—H...S hydrogen bonds. The crystal is further stablized by weak π–π interactions [centroid–centroid distances = 3.5698 (13 and 3.5287 (12 Å].

  10. Crystal structure of 2-methylamino-4-(6-methyl-4-oxo-4H-chromen-3-yl-3-nitropyrano[3,2-c]chromen-5(4H-one with an unknown solvate

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    Rajamani Raja

    2015-09-01

    Full Text Available In the title compound, C23H16N2O7, the mean planes of the two chromene units (r.m.s. deviations = 0.031 and 0.064 Å are almost normal to one another with a dihedral angle of 85.59 (6°. The central six-membered pyran ring has a distorted envelope conformation, with the methine C atom at the flap. There is an intramolecular N—H...O hydrogen bond, which generates an S(6 ring motif. In the crystal, molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R22(12 ring motif. The dimers are linked by pairs of C—H...O hydrogen bonds, enclosing R22(6 ring motifs, forming zigzag chains along [001]. The chains are linked by a second pair of C—H...O hydrogen bonds, forming slabs parallel to (110. Within the slabs there are C—H...π interactions present. A region of disordered electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s.

  11. Aqua(dicyanamido{μ-6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolato}copper(IIsodium(I

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    Yong-Miao Shen

    2009-04-01

    Full Text Available The molecule of the title compound, [CuNa(C18H18N2O4(C2N3(H2O], is almost planar, the maximum deviation from the molecular plane being 0.48 (4 Å. The coordination environment of the Cu2+ ion is distorted square-planar and it is N2O2-chelated by the Schiff base ligand. The Na+ cation has a distorted octahedral environment defined by the four O atoms of the 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolate ligand, a water ligand and a dicyanamide anion.

  12. (3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione

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    Garima Sharma

    2012-09-01

    Full Text Available In the title compound, C26H18N2O3, the maximum deviations from planarity for the tetrahydro-1H-naphtho[2,3-c]pyrrole and indoline rings systems are 0.091 (1 and 0.012 (2 Å, respectively. These ring systems make a dihedral angle of 89.95 (6° with each other and they make dihedral angles of 73.42 (8 and 71.28 (9°, respectively, with the benzene ring. In the crystal, inversion dimers linked by pairs of N—H...O hydrogen bonds generate R22(8 loops and C—H...O interactions connect the dimers into corrugated sheets lying parallel to the bc plane.

  13. 5-(4-Ethoxyphenyl-3-(pyridin-2-yl-4,5-dihydro-1H-pyrazole-1-carbothioamide

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    Hoong-Kun Fun

    2012-03-01

    Full Text Available In the title compound, C17H18N4OS, a pyrazoline derivative, the pyrazoline ring adopts an envelope conformation with the C atom bonded to the benzene ring as the flap atom. The dihedral angle between the pyridine and benzene rings is 80.50 (6°. The ethoxyphenyl group is approximately planar, with an r.m.s. deviation of 0.0238 (1 Å for the nine non-H atoms. In the crystal, molecules are linked by N—H...O and N—H...S hydrogen bonds into a tape along the b axis. Weak C—H...N and C—H...π interactions are also observed.

  14. Bis(μ-biphenyl-2,2′-dicarboxylatobis[(2,2′-bipyridinecopper(II

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    Zhe An

    2009-04-01

    Full Text Available The title compound, [Cu2(C14H8O42(C10H8N22], was obtained by solvothermal synthesis. The CuII atom is coordinated by one chelating 2,2′-bipyridine ligand and two carboxyl groups from different biphenyl-2,2′-dicarboxylate ligands, leading to a distorted octahedral environment. Each carboxylate group makes one short Cu—O bond [1.9608 (14 and 1.9701 (14 Å] and one longer Cu—O contact [2.4338 (17 and 2.5541 (17 Å] to each CuII atom. The biphenyl-2,2′-dicarboxylate ligands bridge between CuII atoms, forming a dinuclear complex around a crystallographic inversion centre.

  15. Neutron diffraction analysis of HRh[P(C6H5)3]4

    International Nuclear Information System (INIS)

    Bau, R.; Stevens, R.C.; McLean, M.; Koetzle, T.F.

    1987-01-01

    We have collected neutron diffraction data on a large single crystal of the title compound. The most surprising result is an extremely short Rh-H distance of 1.31(8) A, presumably caused by steric interactions involving the bulky triphenyl phosphine ligands. Crystallographic details: HRh[P(C 6 H 5 ) 3 ] 4 . 1 / 2 C 6 H 6 crystallizes in the space group Pa3, with a = b = c = 22.776(3) A, Z = 8. Data were collected at the Brookhaven High Flux Beam reactor at a temperature of -23 0 C, λ = 1.15882(7) A -1 . Least-squares refinement (in which the phenyl rings were treated as rigid groups) resulted in an R factor [based on data with f > 4σ(F)] of 0.12 for 914 reflections and 95 parameters. 10 refs

  16. Synthesis, characterization, and thermochemistry of the solid state coordination compound Zn(Nic){sub 2} . H{sub 2}O(s) (Nic = nicotinic acid)

    Energy Technology Data Exchange (ETDEWEB)

    Di Youying [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China)], E-mail: yydi@lcu.edu.cn; Hong Yuanping; Kong Yuxia; Yang Weiwei [College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong (China); Tan Zhicheng [Thermochemistry Laboratory, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China)

    2009-01-15

    A novel compound, viz. zinc nicotinate monohydrate, was synthesized by the method of room temperature solid phase synthesis. The techniques of FT-IR chemical and elemental analyses and X-ray powder diffraction were applied to characterise the structure and composition of the complex. In accordance with Hess' law, a thermochemical cycle was designed and the enthalpy change of the solid phase reaction of nicotinic acid with hydrated zinc acetate was determined to be {delta}{sub r}H{sub m}{sup 0}=(46.71{+-}0.21)kJ.mol{sup -1} by use of an isoperibol solution-reaction calorimeter. The standard molar enthalpy of formation of the title complex Zn(Nic){sub 2} . H{sub 2}O(s) was calculated as -(1062.3 {+-} 2.0) kJ . mol{sup -1} by use of the enthalpies of dissolution and other auxiliary thermodynamic data.

  17. 4-Bromoanilinium perchlorate 18-crown-6 clathrate

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    Min Guo

    2010-11-01

    Full Text Available The reaction of 4-bromoaniline, 18-crown-6, and perchloric acid in methanol yields the title compound, C6H7BrN+·ClO4−·C12H24O6, in which the protonated –NH3+ group forms three bifurcated N—H...O hydrogen bonds to the O atoms of the crown ether.

  18. (Acetylacetonato-κ2O,O′bis[5-methoxy-2-(naphth[1,2-d][1,3]oxazol-2-ylphenyl-κ2C1,N]iridium(III

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    Yuan-Yuan Zhou

    2011-10-01

    Full Text Available In the title compound, [Ir(C18H12NO22(C5H7O2], the Ir atom is O,O′-chelated by the acetylacetonate group and C,N-chelated by the 2-arylnaphth[1,2-d]oxazole groups. The six-coordinate metal atom displays a distorted octahedral geometry. Intramolecular C—H...O hydrogen bonds occur. In the crystal, intermolecular C—H...O hydrogen bonds link the molecules into columns parallel to the b axis.

  19. 2-Ethyl-6-(2-pyridyl-5,6,6a,11b-tetrahydro-7H-indeno[2,1-c]quinoline

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    Alexander Briceño

    2010-03-01

    Full Text Available The title compound, C23H22N2, was obtained using the three-component imino Diels–Alder reaction via a one-pot condensation between anilines, α-pyridinecarboxyaldehyde and indene using BF3·OEt2 as the catalyst. The molecular structure reveals the cis-form as the unique diastereoisomer. The crystal structure comprises one-dimensional zigzag ribbons connected via N—H...N hydrogen bonds. C—H...π interactions also occur.

  20. 12,12′-[2,2′-Oxybis(ethane-2,1-diylbis(oxy]bis[(Rp-4-bromo[2.2]paracyclophane

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    Bing Hong

    2011-04-01

    Full Text Available The title compound, C36H36Br2O3, was synthesized from (Rp-4-bromo-12-hydroxy[2.2]paracyclophane and oxydiethane-2,1-diyl bis(4-methylbenzenesulfonate. The crystal packing exhibits a short O...Br interaction [Br...O = 3.185 (3 Å] and a weak intermolecular C—H...O contact.

  1. 2-[2-Benzoyl-3,3-bis(methylsulfanylprop-2-enylidene]malononitrile

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    Joseph Nirmala

    2009-08-01

    Full Text Available The title compound, C15H12N2OS2, is an example of a push–pull butadiene in which the electron-releasing methylsulfanyl groups and electron-withdrawing nitrile groups on either end of the butadiene chain enhance the conjugation in the system. Short intramolecular C—H...S interactions are observed. In the crystal structure, an O...C short contact of 2.917 (3 Å is observed.

  2. cis-Bis(2,2′-bipyridine-κ2N,N′bis(dimethyl sulfoxide-κOzinc bis(tetraphenylborate dimethyl sulfoxide monosolvate

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    Stefania Tomyn

    2011-12-01

    Full Text Available In the mononuclear title complex, [Zn(C10H8N22(C2H6OS2](C24H20B2·C2H6OS, the ZnII ion is coordinated by four N atoms of two bidentate 2,2′-bipyridine molecules and by the O atoms of two cis-disposed dimethyl sulfoxide molecules in a distorted octahedral geometry. The S atom and the methyl groups of one of the coordinated dimethyl sulfoxide molecules are disordered in a 0.509 (2:0.491 (2 ratio. The crystal packing is stabilized by C—H...O hydrogen bonds between the dimethyl sulfoxide solvent molecules and tetraphenylborate anions.

  3. Ethyl 2-[(2-hydroxybenzylideneamino]-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate

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    Naki Çolak

    2013-07-01

    Full Text Available The title compound, C18H20N2O3S, exists as the phenol–imine form in the crystal and there are bifurcated intramolecular O—H...(N/O hydrogen bonds present. The conformation about the C=N bond is anti (1E; the C=N imine bond length is 1.287 (4 Å and the C=N—C angle is 122.5 (3°. In the tetrahydrothienopyridine moiety, the six-membered ring has a flattened-boat conformation. In the crystal, molecules are stacked nearly parallel to (110 and a weak C—H...π interaction is observed. The carbonyl O atom is disordered over two positions and was refined with a fixed occupancy ratio of 0.7:0.3.

  4. Low-temperature heat capacities and thermodynamic properties of ethylenediammonium tetrachlorozincate chloride (C2H10N2)2(ZnCl4)Cl2

    International Nuclear Information System (INIS)

    He, Dong-Hua; Di, You-Ying; Wang, Bin; Dan, Wen-Yan; Tan, Zhi-Cheng

    2010-01-01

    The ethylenediammonium tetrachlorozincate chloride (C 2 H 10 N 2 ) 2 (ZnCl 4 )Cl 2 was synthesized. Chemical analysis, elemental analysis, and X-ray crystallography were applied to characterize the composition and crystal structure of the complex. Low-temperature heat capacities of the compound were measured by a precision automatic adiabatic calorimeter over the temperature range from T = 77-377 K. A polynomial equation of heat capacities as a function of the reduced temperature was fitted by a least square method. Based on the polynomial equation, the smoothed heat capacities and thermodynamic functions of the title compound relative to the standard reference temperature 298.15 K were calculated at intervals of 5 K. A thermochemical cycle was designed and the enthalpy change of the solid phase reaction of ethylenediamine dihydrochloride with zinc chloride was determined to be Δ r H m o =-(17.9±0.6)kJmol -1 by an isoperibol solution-reaction calorimeter. Finally, the standard molar enthalpy of formation of the title compound was derived to be Δ f H m o [(C 2 H 10 N 2 ) 2 (ZnCl 4 )Cl 2 ,s]=-(1514.4±2.7)kJmol -1 in accordance with Hess law.

  5. 2,2′-(Ethane-1,2-diylbis(1H-benzimidazole

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    Guo-Liang Zhao

    2012-05-01

    Full Text Available The complete molecule of the title compound, C16H14N4, is generated by crystallographic inversion symmetry. In the crystal, molecules are linked by N—H...N hydrogen bonds, generating (001 sheets. Weak aromatic π–π stacking interactions [centroid–centroid distances = 3.7383 (13 and 3.7935 (14 Å] are also observed.

  6. 4-(2,4-Dichlorophenyl-6-(1H-indol-3-yl-2,2′-bipyridine-5-carbonitrile

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    M. N. Ponnuswamy

    2009-05-01

    Full Text Available The title compound, C25H14Cl2N4, crystallizes with two independent molecules in the asymmetric unit. The two pyridine rings are almost coplanar, making dihedral angles of 3.2 (1 and 8.6 (1° in the two independent molecules. The dichlorophenyl and indole rings are twisted away from the bipyridine ring by 64.32 (5 and 18.46 (4°, respectively in the first molecule and by 51.0 (1 and 27.99 (5°, respectively in the second molecule. The crystal packing is stabilized by C—H...N, C—H...Cl, N—H...N and C—H...π interactions.

  7. 2-(2-Chlorophenyl-2,3-dihydroquinazolin-4(1H-one

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    Ming-Jian Li

    2009-09-01

    Full Text Available The title compound, C14H11ClN2O, was synthesized by the reaction of 2-chlorobenzaldehyde and 2-aminobenzamide in an ionic liquid. The pyrimidine ring adopts a skew-boat conformation and the two benzene rings make a dihedral angle of 87.1 (1°. In the crystal, N—H...O and C—H...N hydrogen bonding links the molecules along b.

  8. 3-(1H-Indol-3-yl-2-(2-nitrobenzenesulfonamidopropanoic acid including an unknown solvate

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    Islam Ullah Khan

    2012-07-01

    Full Text Available In the title compound, C17H15N3O6S, which crystallized with highly disordered methanol and/or water solvent molecules, the dihedral angle between the the indole and benzene ring systems is 5.3 (2°, which allows for the formation of intramolecular π–π stacking interactions [centroid–centroid separations = 3.641 (3 and 3.694 (3 Å] and an approximate overall U-shape for the molecule. In the crystal, dimers linked by pairs of Ns—H...Oc (s = sulfonamide and c = carboxylate hydrogen bonds generate R22(10 loops, whereas Ni—H...π (i = indole interactions lead to chains propagating in [100] or [010]. Together, these lead to a three-dimensional network in which the solvent voids are present as intersecting (two-dimensional systems of [100] and [010] channels. The title compound was found to contain a heavily disordered solvent molecule, which could be methanol or water or a mixture of the two. Due to its uncertain nature and the unresolvable disorder, the data were processed with the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155], which revealed 877.8 Å3 of solvent-accessible volume per unit cell and 126 electron-units of scattering density or 109.7 Å3 (16 electron units per organic molecule.. This was not included in the calculations of overall formula weight, density and absorption coefficient.

  9. Volume properties and refraction of aqueous solutions of bisadducts of light fullerene C60 and essential amino acids lysine, threonine, and oxyproline (C60(C6H13N2O2)2, C60(C4H8NO3)2, and C60(C5H9NO2)2) at 25°C

    Science.gov (United States)

    Semenov, K. N.; Ivanova, N. M.; Charykov, N. A.; Keskinov, V. A.; Kalacheva, S. S.; Duryagina, N. N.; Garamova, P. V.; Kulenova, N. A.; Nabieva, A.

    2017-02-01

    Concentration dependences of the density of aqueous solutions of bisadducts of light fullerene C60 and essential amino acids are studied by pycnometry. Concentration dependences of the average molar volumes and partial volumes of components (H2O and corresponding bisadducts) are calculated for C60(C6H13N2O2)2-H2O, C60(C4H8NO3)2-H2O, and C60(C5H9NO2)2-H2O binary systems at 25°C. Concentration dependences of the indices of refraction of C60(C6H13N2O2)2-H2O, C60(C4H8NO3)2-H2O, and C60(C5H9NO2)2-H2O binary systems are determined at 25°C. The concentration dependences of specific refraction and molar refraction of bisadducts and aqueous solutions of them are calculated.

  10. Investigations on the synthesis and pharmacological properties of 4-alkoxy-2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl]-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones.

    Science.gov (United States)

    Sladowska, Helena; Filipek, Barbara; Szkatuła, Dominika; Sabiniarz, Aleksandra; Kardasz, Małgorzata; Potoczek, Joanna; Sieklucka-Dziuba, Maria; Rajtar, Grazyna; Kleinrok, Zdzisław; Lis, Tadeusz

    2002-11-01

    Synthesis of 2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl] derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (8-12) is described. The chlorides used in the above synthesis can exist in two isomeric forms: chain (18-20) and cyclic (19a, 20a). The compounds 8-12 exhibited potent analgesic activity which was superior than that of acetylsalicylic acid in two different tests. Most of the investigated imides suppressed significantly spontaneous locomotor activity in mice.

  11. 5-Pentyl-4-phenylsulfonyl-1H-pyrazol-3-ol

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    Tara Shahani

    2010-06-01

    Full Text Available In the title compound, C14H18N2O3S, the 1H-pyrazole ring is approximately planar, with a maximum deviation of 0.005 (1 Å. The dihedral angle formed between the 1H-pyrazole and phenyl rings is 79.09 (5°. Pairs of intermolecular N—H...O and O...H...N hydrogen bonds form dimers between neighboring molecules, generating R22(10 ring motifs. These dimers are further linked byintermolecular N—H...O and O—H...N hydrogen bonds into a two-dimensional array parallel to the ac plane. The crystal structure is also stabilized by C—H...π interactions.

  12. Liquid state sup1H and sup13C-NMR studies on polymerisation reaction of 2,2'-difurfuryloxy-2- silapropane

    International Nuclear Information System (INIS)

    Rusli bin Omar

    1994-01-01

    The purpose of this study was to prepare the copolymer of 2,2'-difurfuryloxy-2-silapropane (DFS) and 1,1'-(methylenedi-4, 1-phenylene) bismaleimide (BM). DFS was prepared at 0 degC through the reaction of 2 moles of furfuryl alcohol (FA) with 1 mole of dichlorodimethylsilane (DCMS) in the presence of pyridine and chloroform as a solvent. The formation of this compound was characterized by the sup1H and sup13C-NMR spectroscopy and mass spectrometry. DFS has the ability to undergo the Diels-Alder reaction. The furan end groups of DFS could react with dienophile groups of other materials. The adduct of DFS-BM was prepared by the reaction of DFS with BM at room temperature (18degC) in chloroform (CDClsub3). Characterization of the adduct was carried out through a study of the sup1H and sup13C-NMR spectra of the adduct

  13. 2-(2-Pyridylpyridinium (2,2′-bipyridine-κ2N,N′tetrakis(nitrato-κ2O,O′bismuthate(III

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    Shu-Shen Zhang

    2011-10-01

    Full Text Available The structure of the title compound, (C10H9N2[Bi(NO34(C10H8N2], consists of 2-(2-pyridylpyridinium cations and anions [Bi(NO34(C10H8N2]−. The Bi3+ ion lies on the twofold axis. It is coordinated by two nitrogen atoms from one 2,2′-bipyridine ligand and eight oxygen atoms from four NO3− anions. The disordered cation is positioned at the inversion centre. The [Bi(NO34(C10H8N2]− anions and 2-(2-pyridylpyridinium cations are connected via N—H...O hydrogen bonds into chains. Moreover, these chains are further linked into a two-dimensional layered structure through π–π stacking interactions between bipyridine ligands along the c axis [centroid–centroid distance = 2.868 (4 Å].

  14. Bis{(E-3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropan-1-aminium} bis[μ-(E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamido(2−]bis{[(E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide]copper(II} bis((E-{3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropyl}carbamate acetonitrile disolvate

    Directory of Open Access Journals (Sweden)

    Andrii I. Buvailo

    2012-12-01

    Full Text Available The reaction between copper(II nitrate and (E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide led to the formation of the dinuclear centrosymmetric copper(II title complex, (C8H18N3O22[Cu2(C8H15N3O22(C8H17N3O22](C9H16N3O42·2CH3CN, in which an inversion center is located at the midpoint of the Cu2 unit in the center of the neutral [Cu2(C8H15N3O22(C8H17N3O22] complex fragment. The Cu2+ ions are connected by two N—O bridging groups [Cu...Cu separation = 4.0608 (5 Å] while the CuII ions are five-coordinated in a square-pyramidal N4O coordination environment. The complex molecule co-crystallizes with two molecules of acetonitrile, two molecules of the protonated ligand (E-3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropan-1-aminium and two negatively charged (E-{3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropyl}carbamate anions, which were probably formed as a result of condensation between (E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide and hydrogencarbonate anions. In the crystal, the complex fragment [Cu2(C8H15N3O22(C8H17N3O22] and the ion pair C8H18N3O2+.C9H16N3O4− are connected via an extended system of hydrogen bonds.

  15. Hydrothermal synthesis, structural elucidation, spectroscopic studies, thermal behavior and luminescence properties of a new 3-d compound: FeAlF2(C10H8N2)(HPO4)2(H2O)

    Science.gov (United States)

    Bouzidia, Nabaa; Salah, Najet; Hamdi, Besma; Ben Salah, Abdelhamid

    2017-04-01

    The study of metal phosphate has been a proactive field of research thanks to its applied and scientific importance, especially in terms of the development of optical devices such as solid state lasers as well as optical fibers. The present paper seeks to investigate the synthesis, crystal structure, elemental analysis and properties of FeAlF2(C10H8N2)(HPO4)2(H2O) compound investigated by spectroscopic studies (FT-IR and FT-Raman), thermal behavior and luminescence. The Hirshfeld surface analysis and 2-D fingerprint plot have been performed to explore the behavior of these weak interactions and crystal cohesion. This investigation shows that the molecules are connected by hydrogen bonds of the type Osbnd H⋯O and Osbnd H⋯F. In addition, the 2,2'‒bipyridine ligand plays a significant role in the construction of 3-D supramolecular framework via π‒π stacking. FT‒IR and FT‒Raman spectra were used so as to ease the responsibilities of the vibration modes of the title compound. The thermal analysis (TGA) study shows a mass loss evolution as a temperature function. Finally, the optical properties were evaluated by photoluminescence spectroscopy.

  16. 2-(2-Methyl-1,3-dioxolan-2-yl-1,1-diphenylethanol

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    Dennis P. Arnold

    2010-01-01

    Full Text Available The molecules of the title compound, C18H20O3, display an intramolecular O—H...O hydrogen bond between the hydroxy donor and a ketal O-atom acceptor. In the crystal, intermolecular C—H...π interactions connect adjacent molecules into chains parallel to the b axis.

  17. 1,4-Dihydroxyquinoxaline-2,3(1H,4H-dione

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    Wolfgang Frey

    2008-03-01

    Full Text Available The asymmetric unit of the title compound, C8H6N2O4, contains one half-molecule; a twofold rotation axis bisects the molecule. The quinoxaline ring is planar, which can be attributed to electron delocalization. In the crystal structure, intermolecular O—H...O hydrogen bonds link the molecules into R22(10 motifs, leading to layers, which interact via phenyl–phenyl interactions (C...C distances in the range 3.238–3.521 Å.

  18. (Acetato-κO{2-[(2-aminoethyl-κNdisulfanyl]ethanaminium}dichloridozinc(II

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    Naoto Kuwamura

    2016-01-01

    Full Text Available In the title compound, [Zn(C4H13N2S2(CH3COOCl2], the ZnII ion is in a tetrahedral coordination geometry, coordinated by one acetate, two chloride and one 2-[(2-aminoethyldisulfanyl]ethanaminium ligand, with a Zn—O distance of 1.977 (3 Å, a Zn—N distance of 2.015 (3 Å and Zn—Cl distances of 2.2673 (18 and 2.2688 (15 Å. In the crystal, molecules are self-assembled by N—H...Cl hydrogen bonds, leading to a one-dimensional chain structure. The chains interact with each other through N—H...O, N—H...S, C—H...Cl and C—H...S hydrogen bonding, completing a three-dimensional hydrogen-bonding network structure.

  19. Crystal Structure and Hydrogen Bonding Study of (10E-2,2-Dimethyl-3,4-dihydro-2H-benzo[g]chromene-5,10-dione 10-Oxime Derived From a-Lapachone

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    Lorenzo C. Visentin

    2011-01-01

    Full Text Available The compound (10E-2,2-dimethyl-3,4-dihydro-2H-benzo[g]chromene-5,10-dione-10-oxime (1 was synthesized from a-lapachone and hydroxylamine chloride in alkaline medium. Single-crystals suitable for X-ray diffraction measurements were grown from an ethanol solution, and the crystal structure of the title molecule is reported for the first time. The title molecule was also characterized by 1H- and 13C-NMR in CDCl3 solution, FTIR and MS. The crystal structure of 1 shows an E stereochemistry and dimers formed through classical hydrogen bonds.

  20. A novel organic–inorganic hybrid with Anderson type polyanions as building blocks: (C{sub 6}H{sub 10}N{sub 3}O{sub 2}){sub 2}Na(H{sub 2}O){sub 2}[Al(OH){sub 6}Mo{sub 6}O{sub 18}]·6H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Thabet, Safa, E-mail: safathabet@hotmail.fr [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia); Ayed, Brahim, E-mail: brahimayed@yahoo.fr [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia); Haddad, Amor [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia)

    2012-11-15

    Graphical abstract: Display Omitted Highlights: ► Synthesis of a novel inorganic–organic hybrid compound based on Anderson polyoxomolybdates. ► Characterization by X-ray diffraction, IR and UV–Vis spectroscopies of the new compound. ► Potential applications in catalysis, biochemical analysis and electrical conductivity of the organic–inorganic compound. -- Abstract: A new organic–inorganic hybrid compound based on Anderson polyoxomolybdates, (C{sub 6}H{sub 10}N{sub 3}O{sub 2}){sub 2}Na(H{sub 2}O){sub 2}[Al(OH){sub 6}Mo{sub 6}O{sub 18}]·6H{sub 2}O (1) have been isolated by the conventional solution method and characterized by single-crystal X-ray diffraction, infrared, ultraviolet spectroscopy and Thermogravimetric Analysis (TGA). This compound crystallized in the triclinic system, space group P−1, with a = 94.635(1) Å, b = 10.958(1) Å, c = 11.602(1) Å, α = 67.525(1)°, β = 71.049(1)°, γ = 70.124(1)° and Z = 1. The crystal structures of the compounds exhibit three-dimensional supramolecular assembly based on the extensive hydrogen bonding interactions between organic cations, sodium cations, water molecules and Anderson polyoxoanions. The infrared spectrum fully confirms the X-ray crystal structure and the UV spectrum of the title compound exhibits an absorption peak at 210 nm.

  1. A new Schiff base compound N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone): synthesis, experimental and theoretical studies on its crystal structure, FTIR, UV-visible, 1H NMR and 13C NMR spectra.

    Science.gov (United States)

    Saheb, Vahid; Sheikhshoaie, Iran

    2011-10-15

    The Schiff base compound, N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone) (NDHA) is synthesized through the condensation of 2-hydroxylacetophenone and 2,2-dimethyl 1,3-amino propane in methanol at ambient temperature. The yellow crystalline precipitate is used for X-ray single-crystal determination and measuring Fourier transform infrared (FTIR), UV-visible, (1)H NMR and (13)C NMR spectra. Electronic structure calculations at the B3LYP, PBEPBE and PW91PW91 levels of theory are performed to optimize the molecular geometry and to calculate the FTIR, (1)H NMR and (13)C NMR spectra of the compound. Time-dependent density functional theory (TDDFT) method is used to calculate the UV-visible spectrum of NDHA. Vibrational frequencies are determined experimentally and compared with those obtained theoretically. Vibrational assignments and analysis of the fundamental modes of the compound are also performed. All theoretical methods can well reproduce the structure of the compound. The (1)H NMR and (13)C NMR chemical shifts calculated by all DFT methods are consistent with the experimental data. However, the NMR shielding tensors computed at the B3LYP/6-31+G(d,p) level of theory are in better agreement with experimental (1)H NMR and (13)C NMR spectra. The electronic absorption spectrum calculated at the B3LYP/6-31+G(d,p) level by using TD-DFT method is in accordance with the observed UV-visible spectrum of NDHA. In addition, some quantum descriptors of the molecule are calculated and conformational analysis is performed and the results were compared with the crystallographic data. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Synthesis, crystal structure, and photoluminescence of a lithium isothiocyanate compound with 18-crown-6

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Shan; Fu, Bo; Zhao, Zhen; Liu, Xi [Chongqing Normal Univ. (China). Chongqing Key Lab. of Inorganic Functional Materials

    2018-04-01

    The investigation of the supramolecular interactions between the lithium isothiocyanate salt and 18-crown-6 (18C-6) in commercial tetrahydrofuran leads to the formation of a lithium compound, LiNCS(H{sub 2}O)(18C-6) (1). In the crystal structure the asymmetric unit contains two similar LiNCS(H{sub 2}O)(18C-6) molecules. Solid-state photoluminescence experiments have shown that compound 1 emits violet luminescence, and its possible emission mechanism was investigated in detail based on theoretical calculations.

  3. Synthesis and some coordination chemistry of the PSnP pincer-type stannylene Sn(NCH2PtBu2)2C6H4, attempts to prepare the PSiP analogue, and the effect of the E atom on the molecular structures of E(NCH2PtBu2)2C6H4 (E = C, Si, Ge, Sn).

    Science.gov (United States)

    Brugos, Javier; Cabeza, Javier A; García-Álvarez, Pablo; Pérez-Carreño, Enrique; Polo, Diego

    2018-03-26

    The non-donor-stabilized PSnP pincer-type stannylene Sn(NCH2PtBu2)2C6H4 (1) has been prepared by treating SnCl2 with Li2(NCH2PtBu2)2C6H4. All attempts to synthesize the analogous PSiP silylene by reduction of the (previously unknown) silanes SiCl2(NCH2PtBu2)2C6H4 (2), SiHCl(NCH2PtBu2)2C6H4 (3) and SiH(HMDS)(NCH2PtBu2)2C6H4 (4; HMDS = N(SiMe3)2) have been unsuccessful. The almost planar (excluding the tert-butyl groups) molecular structure of stannylene 1 (determined by X-ray crystallography) has been rationalized with the help of DFT calculations, which have shown that, in the series of diphosphanetetrylenes E(NCH2PtBu2)2C6H4 (E = C, Si, Ge, Sn), the most stable conformation of the compounds with E = Ge and Sn has both P atoms very close to the EN2C6H4 plane, near (interacting with) the E atom, whereas for the compounds with E = C and Si, both phosphane groups are located at one side of the EN2C6H4 plane and far away from the E atom. The size of the E atom and the strength of stabilizing donor-acceptor PE interactions (both increase on going down in group 14) are key factors in determining the molecular structures of these diphosphanetetrylenes. The syntheses of the chloridostannyl complexes [Rh{κ2Sn,P-SnCl(NCH2PtBu2)2C6H4}(η4-cod)] (5), [RuCl{κ2Sn,P-SnCl(NCH2PtBu2)2C6H4}(η6-cym)] (6) and [IrCl{κ2Sn,P-SnCl(NCH2PtBu2)2C6H4}(η5-C5Me5)] (7) have demonstrated the tendency of stannylene 1 to insert its Sn atom into M-Cl bonds of transition metal complexes and the preference of the resulting PSnP chloridostannyl group to act as a κ2Sn,P-chelating ligand, maintaining an uncoordinated phosphane fragment. X-ray diffraction data (of 6), 31P{1H} NMR data (of 5-7) and DFT calculations (on 6) are consistent with the existence of a weak PSn interaction involving the non-coordinated P atom of complexes 5-7, similar to that found in stannylene 1.

  4. Aziridines in the synthesis of 11C- and 18F-labelled compounds

    International Nuclear Information System (INIS)

    Gillings, N.M.

    1998-01-01

    Racemic [4- 11 C]aspartic acid, [4- 11 C]asparagine and 2,4-diamino[4- 11 C]butyric acid were synthesised by the ring-opening of an N-activated aziridine-2-carboxylate with 11 C]cyanide, followed by preparative HPLC and hydrolysis/reduction. These labelled amino acids arise from nucleophilic attack at the β-carbon of the aziridine ring. A radioactive by-product of ca. 25% was attributed to the product of α-attack. Several N-activated 2-aryl aziridines were synthesised for the attempted synthesis of β-[ 18 F] fluorophenylalanine and β-[ 18 F]fluorodopa. Ring-opening with [ 18 F]fluoride showed no evidence of β-fluorinated products and it is proposed that attack occurs exclusively at the α-carbon, giving the corresponding α-[ 18 F]fluoro-β-amino acids. Further evidence for this was the reaction of the β-unsubstituted N-activated aziridine-2-carboxylate with [ 18 F]fluoride. This reaction was totally regiospecific and afforded exclusively the α-substituted product, α-[ 18 F]fluoro-β-alanine. Aziridine precursors were resolved by chiral HPLC. On labelling the chiral aziridines, however, racemic 11 C- and 18 F-labelled amino acids were obtained. This was attributed to racemisation of the initially formed ring-opened products. The use of [ 11 C]methyl lithium as a nucleophile for aziridine ring-opening was investigated. Reaction was expected to occur at low temperature, thus potentially avoiding racemisation. No products corresponding to aziridine ring-opening with [ 11 C]methyl lithium were, however, observed. A difluorinated analogue of amphetamine was synthesised by fluorination of an azirine (via an aziridine). This racemic compound was resolved as its chiral tartarate salts and subsequently labelled by methylation with [ 11 C]methyl iodide, giving the novel compound β, β-difluoro[N-methyl- 11 C]methamphetamine in high specific activity for in vivo binding studies using positron emission tomography. The non-radioactive reference compound was also

  5. H1-A, a compound isolated from Fusarium oxysporum inhibits hepatitis C virus (HCV) NS3 serine protease.

    Science.gov (United States)

    Yang, Li-Yuan; Lin, Jun; Zhou, Bin; Liu, Yan-Gang; Zhu, Bao-Quan

    2016-04-01

    The present study was aimed to isolate the active compounds from the fermentation products of Fusarium oxysporum, which had hepatitis C virus (HCV) NS3 protease inhibitory activity. A bioactive compound was isolated by reverse-phase silica-gel column chromatography, silica-gel column chromatography, semi-preparative reverse-phase High Performance Liquid Chromatography (HPLC), and then its molecular structure was elucidated based on the spectrosopic analysis. As a result, the compound (H1-A, 1) Ergosta-5, 8 (14), 22-trien-7-one, 3-hydroxy-,(3β, 22E) was isolated and identified. To the best of our knowledge, this was the first report on the isolation of H1-A from microorganisms with the inhibitory activity of NS3 protease. Copyright © 2016 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  6. Bis(1H-imidazole-κN3bis(1-naphthaleneacetato-κ2O,O′cadmium(II

    Directory of Open Access Journals (Sweden)

    Hong-Mian Wu

    2008-05-01

    Full Text Available In the mononuclear title compound, [Cd(C12H9O22(C3H4N22], the CdII centre has a distorted octahedral coordination geometry defined by four O atoms from two naphthaleneacetate ligands and two N atoms from two imidazole ligands. The molecules are linked by N—H...O hydrogen bonds, forming a layer network.

  7. 4′-Methyl-1H-14′,19′-dioxa-4′-azaspiro[indole-3,5′-tetracyclo[18.4.0.02,6.08,13]tetracosane]-1′(24′,8′,10′,12′,20′,22′-hexaene-2,7′(3H-dione

    Directory of Open Access Journals (Sweden)

    Sibi Narayanan

    2012-12-01

    Full Text Available In the title compound, C29H28N2O4, the indoline ring system is essentially planar, with a maximum deviation of 0.027 (2 Å; the carbonyl O atom lies 0.102 (1 Å out of the least-squares plane of the indole ring. The pyrrolidine ring adopts a C-envelope conformation, with a C atom displaced by 0.643 (2 Å from the mean plane formed by the remaining ring atoms. The pyrrolidine ring makes a dihedral angle of 86.1 (8° with the indoline ring system. In the crystal, N—H...O hydrogen bonds result in the formation of cyclic centrosymmetric dimers [R22(8]. C—H...π interactions also occur, leading to a chain along the b-axis direction. There is a rather weak π–π electron interaction between the pyrrazole and benzene rings, with a centroid–centroid distance of 3.765 (1 Å.

  8. (E,E-6,6′-Dimethoxy-2,2′-[o-phenylenebis(nitrilomethylidyne]diphenol

    Directory of Open Access Journals (Sweden)

    Yong Wang

    2009-04-01

    Full Text Available In the title compound, C22H20N2O4, the central benzene ring forms dihedral angles of 3.2 (2 and 61.1 (1° with the two outer substituted benzene rings. Intramolecular O—H...N hydrogen bonds are formed by both hydroxyl groups.

  9. 2,2-Dimethyl-2,3-dihydro-1H-perimidine

    Directory of Open Access Journals (Sweden)

    Sarah Maloney

    2013-02-01

    Full Text Available The title compound, C13H14N2, was obtained from reaction of diaminonaphthalene with acetone. In both independent molecules in the asymmetric unit, the tricyclic perimidine consists of a planar (r.m.s. deviations = 0.0125 and 0.0181 Å naphthalene ring system and an envelope conformation C4N2 ringwith the NCN group hinged with respect to the naphthalene backbone by 36.9 (2 and 41.3 (2° in the two independent molecules. The methyl substituents are arranged approximately axial and equatorial on the apical C atom. In the crystal, one of the N—H groups of one independent molecule is involved in classical N—H...N hydrogen bonding. Short intermolecular (C/N—H...π(arene interactions, near the short T-shaped limit, link molecules in the absence of strong acceptors.

  10. (S-2-(2-Pyrrolidinio-1H-benzimidazol-3-ium dichloride monohydrate

    Directory of Open Access Journals (Sweden)

    Dai Jing

    2009-06-01

    Full Text Available In the title compound, C11H15N32+·2Cl−·H2O, one N atom of the imidazole ring and the N atom of the pyrrolidine ring are protonated. The crystal structure is stabilized by aromatic π–π interactions between the benzene rings of neighbouring benzimidazole systems [centroid–centroid duistance = 3.712 (2 Å]. The crystal structure is further stabilized by intermolecular N—H...Cl, O—H...Cl and N—H...O hydrogen bonds.

  11. Bis[2-(2H-benzotriazol-2-yl-4-methylphenolato]palladium(II

    Directory of Open Access Journals (Sweden)

    Chen-Yen Tsai

    2009-06-01

    Full Text Available In the title complex, [Pd(C13H10N3O2], the PdII atom is tetracoordinated by two N atoms and two O atoms from two bidentate 2-(2H-benzotriazol-2-yl-4-methylphenolate ligands, forming a square-planar environment. The asymmetric unit contains one half molecule in which the Pd atom lies on a centre of symmetry.

  12. NCI calculations for understanding a physical phase transition in (C6H14N2)[Mn(H2O)6](SeO4)2

    Science.gov (United States)

    Naïli, Houcine; François, Michel; Norquist, Alexander J.; Rekik, Walid

    2017-12-01

    An organically templated manganese selenate, (C6H14N2)[Mn(H2O)6](SeO4)2, has been synthesized by slow evaporation and crystallographically characterized. The title compound crystallizes at room temperature in the monoclinic centrosymmetric space group P21/n, with the following unit cell parameters: a = 7.2373(4) Å; b = 12.5600(7) Å; c = 10.1945(7) Å; β = 91.155(4)°, V = 926.50(10) Å3and Z = 2. Its crystal structure is built of manganese(II) cations coordinated by six water molecules in octahedral geometry, disordered dabcodiium cations and selenate anions, resulting in an extensive hydrogen-bonding network. Differential scanning calorimetry (DSC) measurement indicated that the precursor undergoes a reversible phase transition at about 216 and 218 K during the cooling and heating processes respectively. Below this temperature the title compound is noncentrosymmetric with space group P21 and lattice parameters a = 7.2033(8) Å; b = 12.4981(13) Å; c = 10.0888(11) Å; β = 91.281(2)°, V = 908.04(17) Å3 and Z = 2. The disorder-order transformation of the C atoms of (C6H14N2)2+ cation may drive the structural phase transition. The low temperature phase obtained by breaking symmetry presents a fully ordered structure. The noncovalent interaction (NCI) method was used not only to locate, quantify, and visualize intermolecular interactions in the high and low temperature phases but also to confirm the phase transition detected by DSC measurement. The thermal decomposition of this new compound proceeds through four stages giving rise to the manganese oxide as final product at 850 °C.

  13. 3,5-Bis(4-meth­oxy­phen­yl)-1-phenyl-4,5-dihydro-1H-pyrazole

    OpenAIRE

    Baktır, Zeliha; Akkurt, Mehmet; Samshuddin, S.; Narayana, B.; Yathirajan, H. S.

    2011-01-01

    In the title compound, C23H22N2O2, the central pyrazole ring is nearly planar (r.m.s. deviation = 0.046 Å) and it makes a dihedral angle of 18.5 (2)° with the phenyl ring. The dihedral angles between the phenyl and the two methoxy-substituted phenyl rings are 26.2 (2) and 80.6 (2)°. The crystal structure is stabilized by C—H...π stacking interactions and weak π–π interactions [cen...

  14. 7-Chloro-11a-phenyl-2,3,5,10,11,11a-hexahydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11-dione

    Directory of Open Access Journals (Sweden)

    Vahan Martirosyan

    2008-03-01

    Full Text Available The title compound, C18H15ClN2O2, is a potential human immunodeficiency virus type-1 (HIV-1 non-nucleoside reverse transcriptase inhibitor. The pyrrolidine ring adopts an envelope and the diazepine ring a boat conformation. In the crystal structure, two isomers (R and S form centrosymmetric dimers via N—H...O hydrogen bonds.

  15. 3-Ethyl-4-[(E-(4-fluorobenzylideneamino]-1H-1,2,4-triazole-5(4H-thione

    Directory of Open Access Journals (Sweden)

    Alphonsus D'souza

    2012-05-01

    Full Text Available In the title compound, C11H11FN4S, the dihedral angle between the 1,2,4-triazole ring and the benzene ring is 25.04 (12° and an intramoleuclar C—H...S interaction leads to an S(6 ring. In the crystal, inversion dimers linked by pairs of N—H...S hydrogen bonds generate R22(8 loops.

  16. Electronic and electrochemical properties of platinum(II) and platinum-mercury-carboxylato complexes containing 2-Me2NCH2C6H4, 2,6-(Me2NCH2)2C6H3- and 2-Me2NC6H4CH2 - ligands

    NARCIS (Netherlands)

    Koten, G. van; Ploeg, A.F.M.J. van der; Schmitz, J.E.J.; Linden, J.G.M. van der

    1982-01-01

    The organoplatinum(II) compounds [{2, 6-(Me{2}NCH{2}){2}C{6}H{3}}PtBr] and cis-[(C-N){2}Pt] (C-N = 2-Me{2}NCH{2}C{6}H{4}, 2-Me{2}NC{6}H{4}CH{2}) can be chemically irreversibly oxidized in the potential range 1.00 to 1.35 V vs. an Ag/AgCl electrode, whereas the organoplatinum@?mercury complexes

  17. 3,5-Bis(4-meth-oxy-phen-yl)-1-phenyl-4,5-dihydro-1H-pyrazole.

    Science.gov (United States)

    Baktır, Zeliha; Akkurt, Mehmet; Samshuddin, S; Narayana, B; Yathirajan, H S

    2011-01-12

    In the title compound, C(23)H(22)N(2)O(2), the central pyrazole ring is nearly planar (r.m.s. deviation = 0.046 Å) and it makes a dihedral angle of 18.5 (2)° with the phenyl ring. The dihedral angles between the phenyl and the two meth-oxy-substituted phenyl rings are 26.2 (2) and 80.6 (2)°. The crystal structure is stabilized by C-H⋯π stacking inter-actions and weak π-π inter-actions [centriod-centroid distance = 3.891 (2) Å].

  18. 3,5-Bis(4-methoxyphenyl-1-phenyl-4,5-dihydro-1H-pyrazole

    Directory of Open Access Journals (Sweden)

    Zeliha Baktır

    2011-02-01

    Full Text Available In the title compound, C23H22N2O2, the central pyrazole ring is nearly planar (r.m.s. deviation = 0.046 Å and it makes a dihedral angle of 18.5 (2° with the phenyl ring. The dihedral angles between the phenyl and the two methoxy-substituted phenyl rings are 26.2 (2 and 80.6 (2°. The crystal structure is stabilized by C—H...π stacking interactions and weak π–π interactions [centriod–centroid distance = 3.891 (2 Å].

  19. trans-(1,8-Dibenzyl-1,3,6,8,10,13-hexaazacyclotetradecanediisonicotinatonickel(II

    Directory of Open Access Journals (Sweden)

    Kil Sik Min

    2008-02-01

    Full Text Available In the centrosymmetric title compound, [Ni(C6H4NO22(C22H34N6], the NiII ion is bonded to the four secondary N atoms of the macrocyclic ligand in a square-planar fashion and two carboxylate O atoms of the isonicotinate ions in axial positions, resulting in a tetragonally distorted octahedron. An offset face-to-face π–π stacking interaction [centroid–centroid distance = 3.674(4 Å] and N—H...N and N—H...O hydrogen-bonding interactions give rise to a one-dimensional supramolecular structure in the solid state.

  20. 4′-Methyl-14′,19′-dioxa-4′-azaspiro[acenaphthylene-1,5′-tetracyclo[18.4.0.02,6.08,13]tetracosane]-1′(24′,8′,10′,12′,20′,22′-hexaene-2,7′(1H-dione

    Directory of Open Access Journals (Sweden)

    Sibi Narayanan

    2012-12-01

    Full Text Available In the title compound, C33H29NO4, the acenaphthylene ring system is essentially planar (r.m.s. deviation = 0.0290 Å. The pyrrolidine ring adopts a C-envelope conformation with a C atom displaced by 0.671 (2 Å from the mean-plane formed by the remaining ring atoms. The pyrrolidine ring is fused to acenaphthylene ring system making a dihedral angle of 88.0 (7°. In the crystal, molecules are linked into R22(9 dimers via C—H...N and C—H...O hydrogen bonds. Two C atoms act as donors to the same O atom acceptor, resulting in the formation of R21(7 ring motifs. These two motifs combine to form hydrogen-bonded sheets running along the a- and b-axis directions.

  1. Olbaltumvielu un peptīdu sorbcijas īpašību izpēte AEŠH apstākļos uz dažādām C18 kolonnām

    OpenAIRE

    Marduseviča, Aļona

    2014-01-01

    Olbaltumvielu un peptīdu sorbcijas īpašību izpēte AEŠH apstākļos uz dažādām C18 kolonnām. A. Marduseviča, darba vadītāji Dr. Chem. Asoc. Prof. P. Mekšs, O. Rotkāja. Maģistra darbs, 51 lappuses, 3 tabulas, 37 attēli, 42 literatūras avoti. Latviešu valodā. Atslēgas vārdi: OLBALUMVIELAS, PEPTĪDI, AEŠH, C18 KOLONNAS, IZDALĪŠANAS FAKTORS, GRADIENTA SLĪPUMS. Darbā apskatīti olbaltumvielu un peptīdu atdalīšanas mehānismi, gradients, organisko šķīdinātāju, kolonnas un temperatūras ietekme uz ol...

  2. Tert-butyl 3-oxo-2,3,4,5,6,7-hexahydro-1H-pyrazolo[4,3-c]pyridine-5-carboxylate

    Directory of Open Access Journals (Sweden)

    Tara Shahani

    2010-01-01

    Full Text Available In the title compound, C11H17N3O3, the pyrazole ring is approximately planar, with a maximum deviation of 0.005 (2 Å, and forms a dihedral angle of 5.69 (13° with the plane through the six atoms of the piperidine ring. In the crystal, pairs of intermolecular N—H...O hydrogen bonds form dimers with neighbouring molecules, generating R22(8 ring motifs. These dimers are further linked into two-dimensional arrays parallel to the bc plane by intermolecular N—H...O and C—H...O hydrogen bonds.

  3. Bis(2,2′-bipyridyl-κ2N,N′(sulfato-κ2O,O′cobalt(II ethane-1,2-diol monosolvate

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    Lin Chen

    2011-01-01

    Full Text Available The title compound, [Co(SO4(C10H8N22C2H6O2, has the Co2+ ion in a distorted octahedral CoN4O2 coordination geometry. A twofold rotation axis passes through the Co and S atoms, and through the mid-point of the C—C bond of the ethanediol molecule. In the crystal, the [CoSO4(C10H8N22] and C2H6O2 units are held together by a pair of O—H...O hydrogen bonds.

  4. Catalyst-Dependent Chemoselective Formal Insertion of Diazo Compounds into C-C or C-H Bonds of 1,3-Dicarbonyl Compounds.

    Science.gov (United States)

    Liu, Zhaohong; Sivaguru, Paramasivam; Zanoni, Giuseppe; Anderson, Edward A; Bi, Xihe

    2018-05-08

    A catalyst-dependent chemoselective one-carbon insertion of diazo compounds into the C-C or C-H bonds of 1,3-dicarbonyl species is reported. In the presence of silver(I) triflate, diazo insertion into the C(=O)-C bond of the 1,3-dicarbonyl substrate leads to a 1,4-dicarbonyl product containing an all-carbon α-quaternary center. This reaction constitutes the first example of an insertion of diazo-derived carbenoids into acyclic C-C bonds. When instead scandium(III) triflate was applied as the catalyst, the reaction pathway switched to formal C-H insertion, affording 2-alkylated 1,3-dicarbonyl products. Different reaction pathways are proposed to account for this powerful catalyst-dependent chemoselectivity. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. 2-{[(2-Methoxynaphthalen-1-ylmethyl]amino}phenol

    Directory of Open Access Journals (Sweden)

    Sara Mahdjoub

    2016-07-01

    Full Text Available The asymmetric unit of the title compound, C18H17NO2, contains two independent molecules (A and B. The dihedral angle between the naphthalene ring system and the benzene ring is 74.67 (10° in molecule A and 78.81 (9° in molecule B. In the crystal, molecules are linked by a series of C—H...π interactions, forming sheets parallel to the ab plane.

  6. Diethyl 3H-naphtho[2,1-b]pyran-2,3-dicarboxylate

    Directory of Open Access Journals (Sweden)

    Abdullah Mohamed Asiri

    2009-04-01

    Full Text Available The sp3-hybridized methine C atom in the title compound, C19H18O5, lies out of the mean plane of the remaining 13 atoms of the naphthopyran fused-ring system by 0.571 (1 Å, and its H atom occupies a pseudo-equatorial site.

  7. 4,4′-Di-tert-butyl-2,2′-bipyridine

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    Tatiana R. Amarante

    2009-08-01

    Full Text Available In the title compound, C18H24N2, the molecular unit adopts a trans conformation around the central C—C bond [N—C—C—N torsion angle of 179.2 (3°], with the two aromatic rings almost coplanar [dihedral angle of only 0.70 (4°]. The crystal packing is driven by co-operative contacts involving weak C—H...N and C—H...π interactions, and also the need to fill effectively the available space.

  8. meso-4,4′-Difluoro-2,2′-{[(3aR,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylene}diphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2013-02-01

    Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, there are two intramolecular O—H...N hydrogen bonds involving the N atoms of the imidazolidine ring and the hydroxy groups. The crystal studied was a meso compound obtained by the reaction of the aminal (2S,7R,11S,16R-1,8,10,17-tetraazapentacyclo[8.8.1.18,17.02,7.011,16]cosane with 4-fluorophenol. The imidazolidine ring has a twisted conformation with a CH—CH—N—CH2 torsion angle of 44.99 (14° and, surprisingly, the lone pairs of the N atoms are disposed in a syn isomerism, making the title compound an exception to the typical `rabbit-ear effect' in 1,2-diamines. In the crystal, molecules are linked via C—H...F hydrogen bonds, forming chains along the c-axis direction. These chains are linked via another C—H...F hydrogen bond, forming a three-dimensional network.

  9. Crystal structure of ethyl (2S-9-methoxy-2-methyl-4-oxo-3,4,5,6-tetrahydro-2H- 2,6-methanobenzo[g][1,3,5]oxadiazocine-11-carboxylate

    Directory of Open Access Journals (Sweden)

    A. Dhandapani

    2015-02-01

    Full Text Available In the title compound, C15H18N2O5, the methoxyphenyl ring makes a dihedral angle of 84.70 (12° with the mean plane of the tetrahydropyrimidin-2(1H-one ring. Both the pyran and tetrahydropyrimidin-2(1H-one rings have distorted envelope conformations with the carboxylate-substituted C atom as the flap. In the crystal, molecules are linked via pairs of N—H...O hydrogen bonds, forming zigzag chains propagating along [010], which enclose R22(8 ring motifs. The chains are linked by C—H...π interactions, forming a two-dimensional network parallel to (100.

  10. Synthesis and X-ray structure of the dysprosium(III complex derived from the ligand 5-chloro-1,3-diformyl-2-hydroxybenzene-bis-(2-hydroxybenzoylhydrazone [Dy2(C22H16ClN4O53](SCN 3.(H2O.(CH3OH

    Directory of Open Access Journals (Sweden)

    Aliou H. Barry

    2003-12-01

    Full Text Available The title compound [Dy2(C22H16ClN4O53](SCN 3.(H2O.(CH3OH has been synthesized and its crystal structure determined by single X-ray diffraction at room temperature. The two nine coordinated Dy(III are bound to three macromolecules ligand through the phenolic oxygens of the p-chlorophenol moieties, the nitrogen atoms and the carbonyl functions of the hydrazonic moieties. The phenolic oxygen atoms of the 2-hydroxybenzoyl groups are not bonded to the metal ions. In the bases of the coordination polyhedra the six Dy-N bonds are in the range 2.563(13-2.656(13 Å and the twelve Dy-O bonds are in the range 2.281(10-2.406(10 Å.

  11. Index to Nuclear Safety: a technical progress review by chronology, permuted title, and author, Volume 18 (1) through Volume 22 (6)

    International Nuclear Information System (INIS)

    Cottrell, W.B.; Passiakos, M.

    1982-06-01

    This index to Nuclear Safety covers articles published in Nuclear Safety, Volume 18, Number 1 (January-February 1977) through Volume 22, Number 6 (November-December 1981). The index is divided into three section: a chronological list of articles (including abstracts), a permuted-title (KWIC) index, and an author index. Nuclear Safety, a bimonthly technical progress review prepared by the Nuclear Safety Information Center, covers all safety aspects of nuclear power reactors and associated facilities. Over 300 technical articles published in Nuclear Safety in the last 5 years are listed in this index

  12. Index to Nuclear Safety: a technical progress review by chronology, permuted title, and author, Volume 18 (1) through Volume 22 (6)

    Energy Technology Data Exchange (ETDEWEB)

    Cottrell, W.B.; Passiakos, M.

    1982-06-01

    This index to Nuclear Safety covers articles published in Nuclear Safety, Volume 18, Number 1 (January-February 1977) through Volume 22, Number 6 (November-December 1981). The index is divided into three section: a chronological list of articles (including abstracts), a permuted-title (KWIC) index, and an author index. Nuclear Safety, a bimonthly technical progress review prepared by the Nuclear Safety Information Center, covers all safety aspects of nuclear power reactors and associated facilities. Over 300 technical articles published in Nuclear Safety in the last 5 years are listed in this index.

  13. Coloring problem and magnetocaloric effect of Gd{sub 3}Co{sub 2.2}Si{sub 1.8}

    Energy Technology Data Exchange (ETDEWEB)

    Yao, Jinlei, E-mail: materyao@gmail.com [Research Center for Solid State Physics and Materials, School of Mathematics and Physics, Suzhou University of Science and Technology, Suzhou 215009 (China); Department of Chemistry and Chemical Biology, McMaster University, 1280 Main Street West, Hamilton, Ontario, Canada L8S 4M1 (Canada); Morozkin, A.V. [Department of Chemistry, Moscow State University, Leninskie Gory, House 1, Building 3, GSP-2, Moscow 119992 (Russian Federation); Mozharivskyj, Yurij [Department of Chemistry and Chemical Biology, McMaster University, 1280 Main Street West, Hamilton, Ontario, Canada L8S 4M1 (Canada)

    2013-02-15

    Highlights: Black-Right-Pointing-Pointer Gd{sub 3}Co{sub 2.2}Si{sub 1.8} adopts the Er{sub 3}Ge{sub 4} structure (space group Cmcm). Black-Right-Pointing-Pointer Si and Co show site preference. Black-Right-Pointing-Pointer The electronic factors determine the site occupation of Si and Co. Black-Right-Pointing-Pointer Gd{sub 3}Co{sub 2.2}Si{sub 1.8} order ferromagnetically below 172 K. - Abstract: The Gd{sub 3}Co{sub 2.2}Si{sub 1.8} compound was synthesized by arc melting the constituent elements and subsequent annealing at 1070 K for 120 h. It adopts the Dy{sub 3}Co{sub 2.2}Si{sub 1.8}-type structure with the space group Cmcm and the unit cell parameters of a = 4.1176(7) A, b = 10.305(2) A, c = 12.778(2) A and V = 542.2(2) A{sup 3}. The Co and Si atoms preferentially occupy the 8f and 4a/4c sites, respectively. The atomic electronegativity and electron density at a given site determine its site occupation, according to the analysis of the electronic structure. Gd{sub 3}Co{sub 2.2}Si{sub 1.8} orders ferromagnetically with the Curie temperature of 172 K. The isothermal magnetic entropy change, -{Delta}S{sub m}, reaches the maximum value of 7.09 J/kg K at 170 K for a field change of 0-50 kOe.

  14. Bis[2-(2-aminoethyl-1H-benzimidazole-κ2N2,N3](nitrato-κ2O,O′cobalt(II chloride trihydrate

    Directory of Open Access Journals (Sweden)

    Jing Zhao

    2012-06-01

    Full Text Available In the title compound, [Co(NO3(C9H11N32]Cl·3H2O, the CoII atom is coordinated by four N atoms from two chelating 2-(2-aminoethyl-1H-benzimidazole ligands and two O atoms from one nitrate anion in a distorted octahedral coordination environment. In the crystal, N—H...Cl, N—H...O, O—H...Cl and O—H...O hydrogen bonds link the complex cations, chloride anions and solvent water molecules into a three-dimensional network. π–π interactions between the imidazole and benzene rings and between the benzene rings are observed [centroid–centroid distances = 3.903 (3, 3.720 (3, 3.774 (3 and 3.926 (3 Å].

  15. First-principles study on the structure, elastic properties, hardness and electronic structure of TMB4 (TM=Cr, Re, Ru and Os) compounds

    International Nuclear Information System (INIS)

    Pan, Y.; Zheng, W.T.; Guan, W.M.; Zhang, K.H.; Fan, X.F.

    2013-01-01

    The structural formation, elastic properties, hardness and electronic structure of TMB 4 (TM=Cr, Re, Ru and Os) compounds are investigated using first-principles approach. The value of C 22 for these compounds is almost two times bigger than the C 11 and C 33 . The intrinsic hardness, shear modulus and Young's modulus are calculated to be in a sequence of CrB 4 >ReB 4 >RuB 4 >OsB 4 , and the Poisson's ratio and B/G ratio of TMB 4 follow the order of CrB 4 4 4 4 . The intrinsic hardness of CrB 4 and ReB 4 by LDA is bigger than 40 GPa. The high hardness of TMB 4 compounds is derived from the feature of B–B bonds cage and higher C 22 value. The B–B covalent bonds as bonds cage enhances the resistance to shear deformation and improve the hardness. We predict that the TMB 4 compounds with CrB 4 -type are the potential superhard materials. - Graphical abstract: The first-principles calculations show that the intrinsic hardness of CrB 4 and ReB 4 are bigger than 40 GPa, which are the potential superhard materials due to the B–B bonds cage structure. Display Omitted - Highlights: • The intrinsic hardness of CrB 4 and ReB 4 is bigger than 40 GPa. • The hardness of TMB 4 is calculated to be in a sequence of CrB 4 >ReB 4 >RuB 4 >OsB 4 . • The trend of hardness for TMB 4 is consistent with the variation of elastic modulus. • The C 22 value of TMB 4 is bigger than that of C 11 and C 33 . • The high hardness of TMB 4 is originated from the B–B bonds cage

  16. Aziridines in the synthesis of {sup 11}C- and {sup 18}F-labelled compounds

    Energy Technology Data Exchange (ETDEWEB)

    Gillings, N.M

    1998-07-01

    Racemic [4-{sup 11}C]aspartic acid, [4-{sup 11}C]asparagine and 2,4-diamino[4-{sup 11}C]butyric acid were synthesised by the ring-opening of an N-activated aziridine-2-carboxylate with [{sup 11}C]cyanide, followed by preparative HPLC and hydrolysis/reduction. These labelled amino acids arise from nucleophilic attack at the {beta}-carbon of the aziridine ring. A radioactive by-product of ca. 25% was attributed to the product of {alpha}-attack. Several N-activated 2-aryl aziridines were synthesised for the attempted synthesis of {beta}-[{sup 18}F] fluorophenylalanine and {beta}-[{sup 18}F]fluorodopa. Ring-opening with [{sup 18}F]fluoride showed no evidence of {beta}-fluorinated products and it is proposed that attack occurs exclusively at the {alpha}-carbon, giving the corresponding {alpha}-[{sup 18}F]fluoro-{beta}-amino acids. Further evidence for this was the reaction of the {beta}-unsubstituted N-activated aziridine-2-carboxylate with [{sup 18}F]fluoride. This reaction was totally regiospecific and afforded exclusively the {alpha}-substituted product, {alpha}-[{sup 18}F]fluoro-{beta}-alanine. Aziridine precursors were resolved by chiral HPLC. On labelling the chiral aziridines, however, racemic {sup 11}C- and {sup 18}F-labelled amino acids were obtained. This was attributed to racemisation of the initially formed ring-opened products. The use of [{sup 11}C]methyl lithium as a nucleophile for aziridine ring-opening was investigated. Reaction was expected to occur at low temperature, thus potentially avoiding racemisation. No products corresponding to aziridine ring-opening with [{sup 11}C]methyl lithium were, however, observed. A difluorinated analogue of amphetamine was synthesised by fluorination of an azirine (via an aziridine). This racemic compound was resolved as its chiral tartarate salts and subsequently labelled by methylation with [{sup 11}C]methyl iodide, giving the novel compound {beta}, {beta}-difluoro[N-methyl-{sup 11}C]methamphetamine in high

  17. N-(3-Chloro-4-ethoxy-1-methyl-1H-indazol-5-yl-4-methoxybenzenesulfonamide

    Directory of Open Access Journals (Sweden)

    Hakima Chicha

    2014-06-01

    Full Text Available The indazole ring system of the title compound, C17H18ClN3O4S, is almost planar (r.m.s. deviation = 0.0113 Å and forms dihedral angles of 32.22 (8 and 57.5 (3° with the benzene ring and the mean plane through the 4-ethoxy group, respectively. In the crystal, molecules are connected by pairs of N—H...O hydrogen bonds into inversion dimers, which are further linked by π–π interactions between the diazole rings [intercentroid distance = 3.4946 (11 Å], forming chains parallel to [101].

  18. 2-Oxo-2H-chromen-7-yl 4-tert-butylbenzoate

    Directory of Open Access Journals (Sweden)

    Mohammad Ouédraogo

    2018-04-01

    Full Text Available In the title compound, C20H18O4, the benzoate ring is oriented at an acute angle of 33.10 (12° with respect to the planar (r.m.s deviation = 0.016 Å coumarin ring system. An intramolecular C—H...O hydrogen bond closes an S(6 ring motif. In the crystal, C—H...O contacts generate infinite C(6 chains along the b-axis direction. Also present are π–π stacking interactions between neighbouring pyrone and benzene rings [centroid–centroid distance = 3.7034 (18 Å] and C=O...π interactions [O...centroid = 3.760 (3 Å]. The data obtained from quantum chemical calculations performed on the title compound are in good agreement with the observed structure, although the calculated C—O—C—C torsion angle between the coumarin ring system and the benzoate ring (129.1° is somewhat lower than the observed value [141.3 (3°]. Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions.

  19. Bis(μ-carboxylatoethylphosphonatobis[aqua(2,2′-bipyridinemanganese(II

    Directory of Open Access Journals (Sweden)

    Shao-Ming Ying

    2008-01-01

    Full Text Available The title compound, [Mn2(HO3PCH2CH2COO2(C8H8N22(H2O2], was obtained by hydrothermal synthesis. The manganese(II ions are six-coordinate and are linked by two 2-carboxyethylphosphonate ligands, forming a centrosymmetric dimer. The Mn ions adopts a distorted octahedral coordination geometry. The dimers are further linked by O—H...O hydrogen bonds and π–π stacking interactions [centroid–centroid distance 4.2754 (4 Å].

  20. Bromine-rich Zinc Bromides: Zn6Br12(18-crown-6)2×(Br2)5, Zn4Br8(18-crown-6)2×(Br2)3, and Zn6Br12(18-crown-6)2×(Br2)2.

    Science.gov (United States)

    Hausmann, David; Feldmann, Claus

    2016-06-20

    The bromine-rich zinc bromides Zn6Br12(18-crown-6)2×(Br2)5 (1), Zn4Br8(18-crown-6)2×(Br2)3 (2), and Zn6Br12(18-crown-6)2×(Br2)2 (3) are prepared by reaction of ZnBr2, 18-crown-6, and elemental bromine in the ionic liquid [MeBu3N][N(Tf)2] (N(Tf)2 = bis(trifluoromethylsulfonyl)amide). Zn6Br12(18-crown-6)2×(Br2)5 (1) is formed instantaneously by the reaction. Even at room temperature, compound 1 releases bromine, which was confirmed by thermogravimetry (TG) and mass spectrometry (MS). The release of Br2 can also be directly followed by the color and density of the title compounds. With controlled conditions (2 weeks, 25 °C, absence of excess Br2) Zn6Br12(18-crown-6)2×(Br2)5 (1) slowly releases bromine with conconcurrent generation of Zn4Br8(18-crown-6)2×(Br2)3 (2) (in ionic liquid) and Zn6Br12(18-crown-6)2×(Br2)2 (3) (in inert oil). All bromine-rich zinc bromides contain voluminous uncharged (e.g., Zn3Br6(18-crown-6), Zn2Br4(18-crown-6)) or ionic (e.g., [Zn2Br3(18-crown-6)](+), [(Zn2Br6)×(Br2)2](2-)) building units with dibromine molecules between the Zn oligomers and partially interconnecting the Zn-containing building units. Due to the structural similarity, the bromine release is possible via crystal-to-crystal transformation with retention of the crystal shape.

  1. Synthesis, crystal structure and biological activity of a novel 1,2,3-thidiazole compound

    International Nuclear Information System (INIS)

    Ke, W.

    2013-01-01

    A new 1,2,3-thiadiazole compound was synthesized and characterized by 1H NMR, MS and HRMS. The crystal structure of the title compound (C/sub 12/H/sub 11/ClN/sub 2/O/sub 4/S/sub 2/, Mr = 346.80) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 with a = 8.4425(17) A, b = 8.9801(18) A, c = 9.859(2) A, alpha = 84.36(3) degree, beta = 86.71(3)degree, lambda = 83.25(3) degree, V = 737.9(3)A3, Z 2, F(000) = 356, Dc = 1.561 g/cm/sup 3/, mu = 0.557 mm-1, the final R1 0.0380 and wR2 = 0.0982 for 2160 observed reflections with I > 2sigma(I). A total of 12585 reflections were collected, of which 2601 were independent (Rint 0.0364). The herbicidal activity of title compound was determined, the results showed the title compound displayed excellent herbicidal activity against Brassica campestris. (author)

  2. 18 CFR 415.1 - Short title.

    Science.gov (United States)

    2010-04-01

    ... 18 Conservation of Power and Water Resources 2 2010-04-01 2010-04-01 false Short title. 415.1 Section 415.1 Conservation of Power and Water Resources DELAWARE RIVER BASIN COMMISSION ADMINISTRATIVE MANUAL BASIN REGULATIONS-FLOOD PLAIN REGULATIONS Generally § 415.1 Short title. This part shall be known...

  3. (1E,2E-1,2-Bis(2,2-diphenylhydrazin-1-ylideneethane

    Directory of Open Access Journals (Sweden)

    Angel Mendoza

    2010-09-01

    Full Text Available In the crystal structure of the title compound, C26H22N4, the molecule is located on an inversion centre and shows an E configuration with respect to each C=N bond. The dihedral angle between the phenyl rings in the diphenylhydrazone group is 83.69 (11°. These two rings make dihedral angles of 30.53 (15 and 84.53 (16° with the central N—N=C—C=N—N dihydrazonoethane plane. Intermolecular C—H...π interactions are observed.

  4. Disruption of the rice nitrate transporter OsNPF2.2 hinders root-to-shoot nitrate transport and vascular development

    Science.gov (United States)

    Li, Yuge; Ouyang, Jie; Wang, Ya-Yun; Hu, Rui; Xia, Kuaifei; Duan, Jun; Wang, Yaqin; Tsay, Yi-Fang; Zhang, Mingyong

    2015-01-01

    Plants have evolved to express some members of the nitrate transporter 1/peptide transporter family (NPF) to uptake and transport nitrate. However, little is known of the physiological and functional roles of this family in rice (Oryza sativa L.). Here, we characterized the vascular specific transporter OsNPF2.2. Functional analysis using cDNA-injected Xenopus laevis oocytes revealed that OsNPF2.2 is a low-affinity, pH-dependent nitrate transporter. Use of a green fluorescent protein tagged OsNPF2.2 showed that the transporter is located in the plasma membrane in the rice protoplast. Expression analysis showed that OsNPF2.2 is nitrate inducible and is mainly expressed in parenchyma cells around the xylem. Disruption of OsNPF2.2 increased nitrate concentration in the shoot xylem exudate when nitrate was supplied after a deprivation period; this result suggests that OsNPF2.2 may participate in unloading nitrate from the xylem. Under steady-state nitrate supply, the osnpf2.2 mutants maintained high levels of nitrate in the roots and low shoot:root nitrate ratios; this observation suggests that OsNPF2.2 is involved in root-to-shoot nitrate transport. Mutation of OsNPF2.2 also caused abnormal vasculature and retarded plant growth and development. Our findings demonstrate that OsNPF2.2 can unload nitrate from the xylem to affect the root-to-shoot nitrate transport and plant development. PMID:25923512

  5. 2,2′-Dimethyl-1,1′-[2,2-bis(bromomethylpropane-1,3-diyl]dibenzimidazole hemihydrate

    Directory of Open Access Journals (Sweden)

    Yong-Sheng Yan

    2012-03-01

    Full Text Available The title compound, C21H22Br2N4·0.5H2O, contains two benzimidazole groups which may provide two potential coordination nodes for the construction of metal–organic frameworks. The mean planes of the two imidazole groups are almost perpendicular, with a dihedral angle of 83.05 (2°, and adjacent molecules are linked into a one-dimensional chain by π–π stacking interactions between imidazole groups of different molecules [centroid-to-centroid distances of 3.834 (2 and 3.522 (2 Å].

  6. Crystal structures of N-(4-chlorophenyl-2-[(4,6-diaminopyrimidin-2-ylsulfanyl]acetamide and N-(3-chlorophenyl-2-[(4,6-diaminopyrimidin-2-ylsulfanyl]acetamide

    Directory of Open Access Journals (Sweden)

    S. Subasri

    2017-04-01

    Full Text Available The title compounds, C12H12ClN5OS, (I, and C12H12ClN5OS, (II, are 2-[(diaminopyrimidin-2-ylsulfanyl]acetamides. Compound (II, crystallizes with two independent molecules (A and B in the asymmetric unit. In each of the molecules, in both (I and (II, an intramolecular N—H...N hydrogen bond forms an S(7 ring motif. The pyrimidine ring is inclined to the benzene ring by 42.25 (14° in (I, and by 59.70 (16 and 62.18 (15° in molecules A and B, respectively, of compound (II. In the crystal of (I, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(8 ring motif. The dimers are linked via bifurcated N—H...O and C—H...O hydrogen bonds, forming corrugated layers parallel to the ac plane. In the crystal of (II, the A molecules are linked through N—H...O and N—H...Cl hydrogen bonds, forming layers parallel to (100. The B molecules are also linked by N—H...O and N—H...Cl hydrogen bonds, also forming layers parallel to (100. The parallel layers of A and B molecules are linked via N—H...N hydrogen bonds, forming a three-dimensional structure.

  7. Microwave assistant synthesis, crystal structure and biological activity of a 1,2,4-triazole compound

    International Nuclear Information System (INIS)

    Ke, W.; Sun, N.B.

    2013-01-01

    The title compound (C/sub 17/H/sub 14/F/sub 2/N/sub 4/SO) were synthesized and recrystallized from CH/sub 3/CN. The compound was characterized by 1h-nmr, ftir, ms, hrms and x-ray diffraction. the compound crystallized in the monoclinic space group c2/c with a = 27.532(6), b 8.9596(18), c 14.609(3) alpha = 90, beta = 112.59(3), lambda =90 degree, gamma = 3327.1(12) alpha 3, z = 8 and r = 0.0327 for 2596 observed reflections with 1 > 2 (i). x-ray analysis reveals that not only intermolecular N-H-N interactions, but also C-H Pie stacking interactions exist in the adjacent molecules. The biological activities results showed that it exhibited significant herbicidal activity towards brassica napus. (author)

  8. (3-Benzoyl-1,7,7-trimethylbicyclo[2.2.1]heptan-2-olato-κ2O,Obis[2-(2-pyridylphenyl-κ2C1,N]iridium(III

    Directory of Open Access Journals (Sweden)

    Kaijun Luo

    2011-11-01

    Full Text Available The title compound, [Ir(C11H8N2(C17H19O2], has an octahedral coordination geometry around the IrIII atom, retaining the cis-C,C,trans–N,N chelate disposition of the two 2-phenylpyridine ligands. The chelate rings are nearly mutually perpendicular [the interplanar angles range from 85.48 (17 to 89.17 (19°]. The two 2-(2-pyridylphenyl ligands are approximately planar, with the plane of the phenyl ring being inclined to that of the pyridine ring by 2.3 (3 and 5.1 (3° in the two ligands. The interplanar angle between the phenyl ring in 3-benzoyl-camphor and the IrO2C3 chelate ring is 35.5 (2°.

  9. Crystal structure and thermochemical properties of a novel coordination compound sodium pyruvate C3H3O3Na(s)

    International Nuclear Information System (INIS)

    Gao, Zhen-Fei; Di, You-Ying; Liu, Su-Zhou; Lu, Dong-Fei; Dou, Jian-Min

    2014-01-01

    Graphical abstract: A novel coordination compound sodium pyruvate C 3 H 3 O 3 Na(s) is synthesised. Elemental analysis and X-ray crystallography are used to characterise the composition and crystal structure of the compound. The lattice potential energy and ionic volume of the anion are obtained from crystallographic data. The standard molar enthalpy of formation of the compound is calculated by an isoperibol solution-reaction calorimeter. Molar enthalpies of dissolution of the compound at various molalities are measured at T = 298.15 K. According to Pitzer’s theory, molar enthalpy of dissolution of the title compound at infinite dilution is calculated. The values of relative apparent molar enthalpies and relative partial molar enthalpies of the solvent and the compound at different concentrations m/(mol · kg −1 ) are derived. - Highlights: • The sodium pyruvate was synthesised and crystal structure was determined. • The enthalpy change of the synthesis reaction was obtained. • Standard molar enthalpy of formation was obtained. • Molar enthalpy of dissolution at infinite dilution was calculated. - Abstract: A novel coordination compound sodium pyruvate C 3 H 3 O 3 Na(s) is synthesised by a liquid phase reaction. The compound has an obvious bioactivity and can be used as the biological carbon source and the chemical identification of primary and secondary alcohols. It can be also used to determinate transaminase. Elemental analysis and X-ray crystallography are used to characterise the composition and crystal structure of the compound. Single crystal X-ray analysis reveals that the compound is formed by one CH 3 COCOO − anion and one Na + cation. An obvious feature of the crystal structure is the formation of the five-membered chelate ring by the coordination of O1 of carboxylate and O3 of keto form with Na + cation, and it is good for the stability of the compound in structure. The lattice potential energy and ionic volume of the anion are obtained

  10. 5-[(E-(2-Hydroxybenzylideneamino]-1H-1,3-benzimidazole-2(3H-thione

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2011-01-01

    Full Text Available There are two molecules in the asymmetric unit of the title compound, C14H11N3OS. In each, the benzimidazole ring system is essentially planar, with maximum deviations of 0.010 (2 and 0.006 (2 Å, and makes dihedral angles of 8.70 (9 and 13.75 (8°, respectively, with the hydroxy-substituted benzene rings. Each molecule adopts an E configuration about the central C=N double bond. In the crystal, the two independent molecules are connected via intermolecular N—H...S hydrogen bonds, forming dimers. Furthermore, the dimers are connected by N—H...O hydrogen bonds into molecular ribbons along the c axis. There is an intramolecular O—H...N hydrogen bond in each molecule, which generates an S(6 ring motif.

  11. rac-1-[6-Hydroxy-4-(4-methoxyphenyl-3,6-dimethyl-4,5,6,7-tetrahydro-2H-indazol-5-yl]ethanone

    Directory of Open Access Journals (Sweden)

    Konstantin A. Potekhin

    2013-02-01

    Full Text Available The title compound, C18H22N2O3, represents a (4S,5R,6S-stereoisomer, crystallizing as a racemate in a centrosymmetric space group. The six-membered aliphatic ring adopts a half-chair conformation, with the hydroxy- and acetyl-substituted C atoms deviating by 0.458 (2 and −0.366 (2 Å, respectively, from the plane defined by other four ring atoms. The pyrazole ring is essentially planar [r.m.s deviation = 0.004 (2 Å]. In the crystal, the molecules are linked into chains along the b axis by N—H...N hydrogen bonds. The chains are linked by O—H...N hydrogen bonds into layers parallel to the bc plane.

  12. 1-Methyl-1H-2,1-benzothiazin-4(3H-one 2,2-dioxide

    Directory of Open Access Journals (Sweden)

    Muhammad Nadeem Arshad

    2008-03-01

    Full Text Available In the crystal structure of the title compound, C9H9NO3S, there is distorted tetrahedral geometry around the S atom. The sulfonyl group is almost normal to the benzene ring, while the carbonyl O atom and methyl C atom are on opposite sides of this ring. The heterocyclic ring adopts a half-boat conformation with the S atom out of the plane. The molecules are dimerized by hydrogen bonding involving the benzene ring and the sulfonyl group. These dimers are linked to each other in the same way. There is an intramolecular hydrogen bond between a methyl C—H group and a sulfonyl O atom, and a π–π interaction between the aromatic rings of two dimers at a centroid-to-centroid distance of 3.6373 (13 Å.

  13. Gold electrodes modified with 16H, 18H-dibenzo[c,l]-7,9-dithia-16,18-diazapentacene for electrocatalytic oxidation of NADH

    NARCIS (Netherlands)

    Rosca, V.; Muresan, L.; Popescu, I.C.; Cristea, C.; Silberg, I.A.

    2001-01-01

    16H,18H-Dibenzo[c,l]-7,9-dithia-16,18-diazapentacene (DDDP), a new phenothiazine derivative containing two linearly condensed phenothiazine rings, strongly adsorbs on polyoriented gold resulting in a modified electrode with electrocatalytic activity for ß-nicotinamide adenine dinucleotide (NADH)

  14. (O-Methyl di-thio-carbonato-κS)tri-phenyl-tin(IV).

    Science.gov (United States)

    Javed, Fatima; Ali, Saqib; Shah, Wajid; Tahir, M Nawaz; Ullah, Hameed

    2013-06-01

    In the title compound, [Sn(C6H5)3(C2H3OS2)], the Sn(IV) atom adopts a distorted SnC3S tetra-hedral coordination geometry. A short Sn⋯O contact [2.988 (4) Å] is also present. The phenyl rings are each disordered over two sets of sites with an occupancy ratio of 0.550 (8):0.450 (8). The crystal studied was found to be a racemic twin with a twin component ratio of 0.57 (18):0.43 (18).

  15. First-principles study on the structure, elastic properties, hardness and electronic structure of TMB{sub 4} (TM=Cr, Re, Ru and Os) compounds

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Y. [Department of Materials Science, Key Laboratory of Automobile Materials of MOE and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Zheng, W.T., E-mail: WTZheng@jlu.edu.cn [Department of Materials Science, Key Laboratory of Automobile Materials of MOE and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China); Guan, W.M.; Zhang, K.H. [State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Kunming 650106 (China); Fan, X.F. [Department of Materials Science, Key Laboratory of Automobile Materials of MOE and State Key Laboratory of Superhard Materials, Jilin University, Changchun 130012 (China)

    2013-11-15

    The structural formation, elastic properties, hardness and electronic structure of TMB{sub 4} (TM=Cr, Re, Ru and Os) compounds are investigated using first-principles approach. The value of C{sub 22} for these compounds is almost two times bigger than the C{sub 11} and C{sub 33}. The intrinsic hardness, shear modulus and Young's modulus are calculated to be in a sequence of CrB{sub 4}>ReB{sub 4}>RuB{sub 4}>OsB{sub 4}, and the Poisson's ratio and B/G ratio of TMB{sub 4} follow the order of CrB{sub 4}OsB{sub 4}. The intrinsic hardness of CrB{sub 4} and ReB{sub 4} by LDA is bigger than 40 GPa. The high hardness of TMB{sub 4} compounds is derived from the feature of B–B bonds cage and higher C{sub 22} value. The B–B covalent bonds as bonds cage enhances the resistance to shear deformation and improve the hardness. We predict that the TMB{sub 4} compounds with CrB{sub 4}-type are the potential superhard materials. - Graphical abstract: The first-principles calculations show that the intrinsic hardness of CrB{sub 4} and ReB{sub 4} are bigger than 40 GPa, which are the potential superhard materials due to the B–B bonds cage structure. Display Omitted - Highlights: • The intrinsic hardness of CrB{sub 4} and ReB{sub 4} is bigger than 40 GPa. • The hardness of TMB{sub 4} is calculated to be in a sequence of CrB{sub 4}>ReB{sub 4}>RuB{sub 4}>OsB{sub 4}. • The trend of hardness for TMB{sub 4} is consistent with the variation of elastic modulus. • The C{sub 22} value of TMB{sub 4} is bigger than that of C{sub 11} and C{sub 33}. • The high hardness of TMB{sub 4} is originated from the B–B bonds cage.

  16. Acetylene–ammonia–18-crown-6 (1/2/1

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    Tobias Grassl

    2012-10-01

    Full Text Available The title compound, C2HC12H24O6·2NH3, was formed by co-crystallization of 18-crown-6 and acetylene in liquid ammonia. The 18-crown-6 molecule has threefold rotoinversion symmetry. The acteylene molecule lies on the threefold axis and the whole molecule is generated by an inversion center. The two ammonia molecules are also located on the threefold axis and are related by inversion symmetry. In the crystal, the ammonia molecules are located below and above the crown ether plane and are connected by intermolecular N—H...O hydrogen bonds. The acetylene molecules are additionally linked by weak C—H...N interactions into chains that propagate in the direction of the crystallographic c axis. The 18-crown-6 molecule [occupancy ratio 0.830 (4:0.170 (4] is disordered and was refined using a split model.

  17. Heterocyclic Analogues of Xanthone and Xanthione. 1H-Pyrano[2,3-c:6,5-c]dipyrazol-4(7H-ones and Thiones: Synthesis and NMR Data

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    Wolfgang Holzer

    2010-09-01

    Full Text Available The synthesis of the title compounds is described. Reaction of 1-substituted 2-pyrazolin-5-ones with 5-chloro-1-phenyl-1H-pyrazole-4-carbonyl chloride or 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carbonyl chloride, respectively, using calcium hydroxide in refluxing 1,4-dioxane gave the corresponding 4-heteroaroylpyrazol-5-ols, which were cyclized into 1H-pyrano[2,3-c:6,5-c]dipyrazol-4(7H-ones by treatment with K2CO3/DMF. The latter were converted into the corresponding thiones upon reaction with Lawesson’s reagent. Detailed NMR spectroscopic investigations (1H, 13C, 15N of the ring systems and their precursors are presented.

  18. C_6_0"3"- versus C_6_0"4"- /C_6_0"2"- - synthesis and characterization of five salts containing discrete fullerene anions

    International Nuclear Information System (INIS)

    Boeddinghaus, M. Bele; Klein, Wilhelm; Wahl, Bernhard; Faessler, Thomas F.; Jakes, Peter; Eichel, Ruediger A.

    2014-01-01

    Five new compounds, [Rb(18crown-6)]_3[C_6_0] (1), [Rb(18crown-6)]_6[C_6_0]_2(C_3H_7NO)_2(C_4H_8O)_2 (2), [Rb(benzo18crown-6)]_6[C_6_0]_2(C_2H_8N_2)_5 (3), [Cs(benzo18crown-6)]_3C_6_0(C_2H_8N_2)_2 (4), and [Cs_3(benzo18crown-6)_5]C_6_0(C_2H_8N_2)_(_4_._5_+_x_) (5) were synthesized and characterized by single-crystal X-ray structure determination. All compounds contain discrete C_6_0 anions, which are ordered in 1, 2, and 4, where direct cation-anion contacts occur. The unit cells of 1 and 2 contain two independent fullerides, which coordinate to the rubidium atoms either of two or of four [Rb(18crown-6)] units. Owing to the presence of differently coordinated fullerene units in compounds 1 and 2, a possible disproportionation of C_6_0"3"- into C_6_0"2"- and C_6_0"4"- anions is discussed. In 3 and 4 the C_6_0 anions are coordinated by three Rb and Cs atoms, respectively. In all compounds the average charge of the anion is -3. Magnetic data reveal a doublet spin state for 3. The EPR spectra are discussed for compounds 3 and 5. The role of a dynamic Jahn-Teller distortion is discussed, and we report the first IR spectroscopic data of fullerene trianions, which have been obtained in solution. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  19. Bis(2,2′-bipyrid­yl)bromidocopper(II) bromide bromo­acetic acid hemihydrate

    OpenAIRE

    Liu, Yaru; Sun, Junshan; Wang, Xinli

    2009-01-01

    In the title compound, [CuBr(C10H8N2)2]Br·BrCH2COOH·0.5H2O, the CuII ion is coordinated by four N atoms [Cu—N = 1.985 (6)–2.125 (7) Å] from two 2,2′-bipyridine ligand molecules and a bromide anion [Cu—Br = 2.471 (2) Å] in a distorted trigonal-bipyramidal geometry. Short centroid–centroid distances [3.762 (5) and 3.867 (5) ...

  20. 4-{(E-[2-(4-Iodobutoxybenzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one

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    Hoong-Kun Fun

    2010-07-01

    Full Text Available The title Schiff base compound, C22H24IN3O2, adopts an E configuration about the central C=N bond. The pyrazolone ring makes a dihedral angle of 49.68 (10° with its attached phenyl ring. The phenolate plane makes dihedral angles of 16.78 (9 and 50.54 (9°, respectively, with the pyrazolone ring and the terminal phenyl ring. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, an intermolecular C—H...O hydrogen bond is also observed.

  1. 2,2-Dimethyl-2,3-dihydropyrano[2,3-a]carbazol-4(11H-one

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    Makuteswaran Sridharan

    2008-11-01

    Full Text Available The title compound, C17H15NO2, was prepared from 1-hydroxycarbazole and 3,3-dimethylacrylic acid with a mixture of AlCl3 and POCl3 as the cyclization catalyst. Owing to the presence of the –CMe2– group, the molecule is not quite planar. In the crystal structre, strong N—H...O hydrogen bonds and weaker C—H...π interactions occur, and a slipped π–π stacking interaction [centroid–centroid separation = 3.8425 (8 Å] is also observed.

  2. Methyl 5,7-dihydroxy-2,2,9-trimethyl-6,11-dioxo-6,11-dihydro-2H-anthra[2,3-b]pyran-8-carboxylate

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    Annelise Lobstein

    2008-12-01

    Full Text Available The title compound, C22H18O7, also known as laurentiquinone B, is a new anthraquinone which was isolated from Vismia laurentii, a Cameroonian medicinal plant. The asymmetric unit contains two independent molecules. Each of them contains four fused rings, three of which are coplanar and typical of anthracene, while the heterocyclic rings adopt envelope conformations. Intramolecular O—H...O hydrogen bonds result in the formation of two planar rings, which are also almost coplanar with the adjacent rings. In the crystal structure, intermolecular O—H...O and C—H...O hydrogen bonds link the molecules and a π–π contact is also present [centroid-centroid distance = 3.967 (3 Å].

  3. Crystal structure of methyl 2-(2H-1,3-benzodioxol-5-yl-7,9-dibromo-8-oxo-1-oxaspiro[4.5]deca-2,6,9-triene-3-carboxylate

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    Lucimara Julio Martins

    2014-12-01

    Full Text Available The title compound, C18H12Br2O6, was synthesized from Morita–Baylis–Hillman adducts. It incorporates the brominated spiro-hexadienone moiety typically exhibited by compounds of this class that exhibit biological activity. Both the brominated cyclohexadienone and the central five-membered rings are nearly planar (r.m.s. deviations of 0.044 and 0.016 Å, respectively, being almost perpendicularly oriented [interplanar angle = 89.47 (5°]. With respect to the central five-membered ring, the brominated cyclohexadienone ring, the benzodioxol ring and the carboxylate fragment make C—O—C—C, O—C—C—C and C—C—C—O dihedral angles of −122.11 (8, −27.20 (11 and −8.40 (12°, respectively. An intramolecular C—H...O hydrogen bond occurs. In the crystal, molecules are linked by non-classical C—H...O and C—H...Br hydrogen bonds resulting in a molecular packing in which the brominated rings are in a head-to-head orientation, forming well marked planes parallel to the b axis.

  4. Redox-neutral rhodium-catalyzed C-H functionalization of arylamine N-oxides with diazo compounds: primary C(sp(3))-H/C(sp(2))-H activation and oxygen-atom transfer.

    Science.gov (United States)

    Zhou, Bing; Chen, Zhaoqiang; Yang, Yaxi; Ai, Wen; Tang, Huanyu; Wu, Yunxiang; Zhu, Weiliang; Li, Yuanchao

    2015-10-05

    An unprecedented rhodium(III)-catalyzed regioselective redox-neutral annulation reaction of 1-naphthylamine N-oxides with diazo compounds was developed to afford various biologically important 1H-benzo[g]indolines. This coupling reaction proceeds under mild reaction conditions and does not require external oxidants. The only by-products are dinitrogen and water. More significantly, this reaction represents the first example of dual functiaonalization of unactivated a primary C(sp(3) )H bond and C(sp(2) )H bond with diazocarbonyl compounds. DFT calculations revealed that an intermediate iminium is most likely involved in the catalytic cycle. Moreover, a rhodium(III)-catalyzed coupling of readily available tertiary aniline N-oxides with α-diazomalonates was also developed under external oxidant-free conditions to access various aminomandelic acid derivatives by an O-atom-transfer reaction. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Synthesis and characteristics of a novel 3-D organic amine oxalate: (enH2)1.5[Bi3(C2O4)6(CO2CONHCH2CH2NH3)].6.5H2O

    International Nuclear Information System (INIS)

    Yu Xiaohong; Zhang Hanhui; Cao Yanning; Chen Yiping; Wang Zhen

    2006-01-01

    A novel 3-D compound of (enH 2 ) 1.5 [Bi 3 (C 2 O 4 ) 6 (CO 2 CONHCH 2 CH 2 NH 3 )].6.5H 2 O has been hydrothermally synthesized and characterized by IR, ultraviolet-visible diffuse reflection integral spectrum (UV-Vis DRIS), fluorescence spectra, TGA and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group C2/c with a=31.110(8)A, b=11.544(3)A, c=22.583(6)A, β=112.419(3) o , V=7497(3)A 3 , Z=8, R 1 =0.0463 and wR 2 =0.1393 for unique 7686 reflections I>2σ(I). In the title compound, the Bi atoms have eight-fold and nine-fold coordination with respect to the oxygen atoms, with the Bi atoms in distorted dodecahedron and monocapped square antiprism, respectively. The 3-D framework of the title compound contains channels and is composed of linkages between Bi atoms and oxalate units, forming honeycomb-like layers with two kinds of 6+6 membered aperture, and pillared by oxalate ligands and monamide groups. The channels have N-ethylamine oxalate monamide group - CO 2 CONHCH 2 CH 2 NH 3 + , which is formed by the in situ reaction of en and oxalate acid. At room temperature, the complex exhibits intense blue luminescence with an emission peak at 445nm

  6. 5-(4-Methoxyphenyl-4-methyl-1-phenyl-3-p-tolyl-1H-pyrazole

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    Yahya Ben Soumane

    2017-11-01

    Full Text Available The title compound, C24H22N2O, crystallizes with two independent molecules (A and B in the asymmetric unit. The phenyl, p-tolyl and p-methoxyphenyl rings are inclined to the pyrazole ring by 42.5 (2, 17.68 (19 and 52.20 (19°, respectively, in molecule A, and by 39.5 (2, 40.77 (19 and 59.76 (18°, respectively, in molecule B. In the asymmetric unit, the pyrarole ring of molecule A makes a dihedral angle of 3.7 (2° with that of molecule B. In the crystal, the two independent molecules are linked to each other by a C—H...O hydrogen bond.

  7. Crystal structure of 5,5′-dibromo-3,3′-di-tert-butyl-6,6′-dimethylbiphenyl-2,2′-diol

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    Rika Obata

    2015-05-01

    Full Text Available The whole molecule of the title compound, C22H28Br2O2, is generated by twofold rotation symmetry. The dihedral angle of the biphenyl moiety is 85.05 (11°. The hydroxy groups show intramolecular O—H...π interactions without any other hydrogen-bond acceptors. In the crystal, there are no other significant intermolecular interactions present.

  8. N,N',N",N"'-Tetrakis(5,7-dimethyl-1,8-naphthyridine-2-yl-3,3',5,5'-diphenylmethanetetracarboxamide

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    Ute Schmidt

    2015-02-01

    Full Text Available Diphenylmethane-based compounds bearing heterocyclic recognition groups, capable to act as hydrogen bonding sites were established to be powerful receptors for carbohydrates. In this paper, we describe the synthesis of a further representative of this class of compounds, containing four 1,8-naphthyridine groups as recognition units. The title compound has been characterized by elemental analysis, 1H-NMR, 13C-NMR and mass spectrometry.

  9. SINTESIS SENYAWA C18H26O9 DARI HIPTOLIDA HASIL ISOLASI DAUN HYPTIS PECTINATA

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    Meiny Suzery

    2012-05-01

    Full Text Available SYNTHESIS OF C18H26O9 COMPOUNDS FROM HYPTOLIDE ISOLATED FROM HYPTIS PECTINATA LEAVES. Isolation of hyptolide has been done from Hyptis pectinata, and alkene group transformation through oxidation reactions using H3B: OEt2 to the isolated compound was also conducted. Product analyses were carried out using TLC, UV spectrometry, IR, and LC-MS. Pure crystal with melting point of 86-87oC was isolated. The yield was 1.75% (w/w. After analysing and compilating of spectroscopic data it was confirmed as hyptolide compound. Hydroboration of this compound (followed by hydrolysis using H2O2 under alkaline conditions produce its alcohol derivatives, with 28.9% the percentage of transformation, it was demonstrated by LCMS data. IR spectrum at 3600cm-1, confirming the replacement of hydroxyl bond by alkene. Regioselectivity of addition reaction is proposed through simulation with Chem Office. The reaction product was suspected as 6-hydroxy-7-(6-oxo-3,6-dihydro-2H-pyran-2-yl heptane-2,3,5-tryil triacetate. Extension of reaction time to 24 hours, has increase hydroboration product to 78.3%. This research has opened other studies of natural materials in accordance to the roadmap set.  Telah dilakukan isolasi hiptolida dari bahan alam Hyptis pectinata, dan transformasinya melalui reaksi oksidasi menggunakan H3B:OEt2 terhadap gugus alkena pada senyawa hasil isolasi. Analisis produk dilakukan menggunakan KLT, spektrometri UV, IR, dan LC-MS. Kristal murni dengan titik leleh 86-87oC berhasil diisolasi dengan rendemen 1,75 % (b/b, dirujuk sebagai senyawa hiptolida setelah melalui analisis dan kompilasi data-data spektroskopi. Hidroborasi terhadap senyawa hiptolida (yang diikuti hidrolisis menggunakan H2O2 dalam suasana basa menghasilkan senyawa alkohol turunannya, dengan persentase transformasi sebesar 28,9%, dapat ditunjukkan melalui data LCMS. Data spectrum IR menunjukkan adanya puncak pada 3600cm-1, memperkuat dugaan  adanya ikatan hidroksil menggantikan gugus

  10. Crystal structure of {μ-6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolato}(methanol(nitratonickel(IIsodium

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    Olesia V. Moroz

    2014-11-01

    Full Text Available In the molecular structure of the title compound, [NaNi(C18H18N2O4(NO3(CH3OH], the Ni2+ ion has a slightly distorted square-planar coordination environment defined by two N and two O atoms which belong to a Schiff base ligand, viz. 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolate. Seven O atoms form the coordination environment of the Na+ ion: four from the Schiff base ligand, two from a bidentate chelating nitrate anion and one O atom from a coordinating methanol molecule. In the crystal, the bimetallic complexes are assembled into chains along the b-axis direction via weak C—H...O hydrogen-bond interactions. Neighbouring chains are in turn connected through bifurcated O—H...O hydrogen bonds that involve the coordinating methanol molecules and the nitrate anions, and through π–π stacking interactions between phenyl rings of neighbouring molecules.

  11. H-D exchange in metal carbene complexes: Structure of cluster (μ-H)(μ-OCD3)Os3(CO)9{:C(CD3)NC2H8O}

    Science.gov (United States)

    Savkov, Boris; Maksakov, Vladimir; Kuratieva, Natalia

    2015-10-01

    X-ray and spectroscopic data for the new complex (μ-H)(μ-OCH3)Os3(CO)9{:C(CD3)NC2H8O} (2) obtained in the reaction of the (μ-H)(μ-Cl)Os3(CO)9{:C(CH3)NC2H8O} (1) with NaOCD3 in CD3OD solution are reported. It is shown that cluster 1 has the property of CH-acidity inherent of Fisher type carbenes. This had demonstrated using hydrogen deuterium exchange reaction in the presence of a strong base. Bridging chlorine to metoxide ligand substitution takes place during the reaction. The molecular structure of 2 is compared with known analogues.

  12. 5-Imino-3,4-diphenyl-1H-pyrrol-2-one

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    Evgeny Bulatov

    2014-02-01

    Full Text Available The title compound, C16H12N2O, exists in the crystalline state as the 5-imino-3,4-diphenyl-1H-pyrrol-2-one tautomer. The dihedral angles between the pyrrole and phenyl rings are 35.3 (2 and 55.3 (2°. In the crystal, inversion dimers linked by pairs of N—H...N hydrogen bonds generate a graph-set motif of R22(8 via N—H...N hydrogen bonds.

  13. 3,5-Bis(4-meth­oxy­phen­yl)-1-phenyl-4,5-dihydro-1H-pyrazole

    Science.gov (United States)

    Baktır, Zeliha; Akkurt, Mehmet; Samshuddin, S.; Narayana, B.; Yathirajan, H. S.

    2011-01-01

    In the title compound, C23H22N2O2, the central pyrazole ring is nearly planar (r.m.s. deviation = 0.046 Å) and it makes a dihedral angle of 18.5 (2)° with the phenyl ring. The dihedral angles between the phenyl and the two meth­oxy-substituted phenyl rings are 26.2 (2) and 80.6 (2)°. The crystal structure is stabilized by C—H⋯π stacking inter­actions and weak π–π inter­actions [centriod–centroid distance = 3.891 (2) Å]. PMID:21523013

  14. 9-Benzyl-6-benzylsulfanyl-9H-purin-2-amine

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    Maywan Hariono

    2014-03-01

    Full Text Available In the title compound, C19H17N5S, the dihedral angles between the purine ring system (r.m.s. deviation = 0.009 Å and the S-bound and methylene-bound phenyl rings are 74.67 (8 and 71.28 (7°, respectively. In the crystal, inversion dimers linked by pairs of N—H...N hydrogen bonds generate R22(8 loops. C—H...N interactions link the dimers into (100 sheets.

  15. Dibromido(6-methyl-2,2′-bipyridine-κ2N,N′zinc(II

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    Vahid Amani

    2010-10-01

    Full Text Available In the title compound, [ZnBr2(C11H10N2], the ZnII atom is four-coordinated in a distorted tetrahedral configuration by two N atoms from a 6-methyl-2,2′-bipyridine ligand and two terminal Br atoms. Weak intermolecular C—H...Br hydrogen bonds and π–π stacking interactions between the pyridine rings [centroid–centroid distances = 3.763 (5 and 3.835 (6 Å] contribute to crystal-packing effects.

  16. tert-Butyl 3-(8-bromo-4H,10H-1,2-oxazolo[4,3-c][1]benzoxepin-10-yl-2-methyl-1H-indole-1-carboxylate

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    Ankur Trigunait

    2010-08-01

    Full Text Available In the title compound, C25H23BrN2O4, the seven-membered ring adopts a twisted-boat conformation. The indole ring system is planar within 0.021 (2 Å and the ester group [–C(=O—O—C–] is almost coplanar with it [dihedral angle = 3.0 (2°]. The conformation of the ester group is influenced by intramolecular C—H...O interactions. In the crystal structure, molecules are linked into chains along the b axis by C—H...N hydrogen bonds.

  17. Isolation and survival of Yersinia enterocolitica in ice cream at different pH values, stored at -18°c Isolamento e sobrevivência de Yersinia enterocolitica em sorvetes de distintos pH, armazenados a -18°C

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    Norma B. Barbini de Pederiva

    2000-09-01

    Full Text Available The presence of Yersinia enterocolitica was investigated in 203 samples of industrial (123 and non-industrial ice cream (80. Two Y. enterocolitica strains were isolated from non-industrial ice cream, which suggests the possibility of post-manufacturing contamination. One strain was typed as B:1A, O: 3,50,51; lis Xz, while the other one was biotyped as: B:1A but not serologically typed. Survival of Y. enterocolitica was investigated by inoculating nine samples of industrially manufactured ice cream to contain 20 CFU/ml of Y. enterocolitica and stored at -18°C for 480 days. The inoculated samples were classified into three different groups according to their pH (Group 1: pH 4-5; Group 2: pH 5-6 and Group 3: pH 6-7. Viability was determined by a combination of direct plating and enrichment. In Group 1, Y. enterocolitica was not detected after 150 days of storage, while in Groups 2 and 3, this microorganism was isolated until day 480 of storage. These findings suggest that the survival time of Y. enterocolitica in ice cream stored at -18°C is significantly (p Neste estudo pesquisou-se a presença de Yersinia enterocolitica em 203 amostras de sorvetes, sendo 123 de fabricação industrial e 80 de fabricação artesanal. Isolaram-se 2 cepas a partir de sorvetes artesanais, uma das quais foi caracterizada como B:1A, O:3,50, 51; lis Xz e a outra se tipificou como Y. enterocolitica B:1A mas não se tipificou sorologicamente, o que sugere uma contaminação pós processo. Em 9 dos sorvetes de fabricação industrial de distintos pH, estudou-se a sobrevivência desse microrganismo, inoculando-os com 20 UFC/ml de Y. enterocolitica, quando armazenados durante 480 dias a -18°C. Esses sorvetes, segundo seu pH, agruparam-se em: Grupo 1: pH: 4-5, Grupo 2: pH 5-6 e Grupo 3: pH: 6-7. Determinou-se a viabilidade pelas curvas de morte usando semeadura direta e enriquecimento. Nos sorvetes do grupo 1, Y. enterocolitica só foi detectada até o 150° dia de

  18. 2-(1H-Imidazol-1-yl)-3-isopropyl-1-benzothieno[3,2-d]pyrimidin-4(3H)-one

    OpenAIRE

    Xu, Sheng-Zhen

    2007-01-01

    In the title compound, C16H14N4OS, the three fused rings of the benzothieno[3,2-d]pyrimidinone unit are essentially coplanar, the maximum deviation from the mean plane being 0.067 (3) Å. The dihedral angle between the mean plane of the fused rings and the imidazole ring is 72.00 (3)°. Offset π–π stacking interactions involving the fused rings are effective in the stabilization of the crystal structure. The centroid–centroid distances between t...

  19. Synthesis and structure of [(NH2)2CSSC(NH2)2]2[OsBr6]Br2 . 3H2O

    International Nuclear Information System (INIS)

    Rudnitskaya, O. V.; Kultyshkina, E. K.; Stash, A. I.; Glukhova, A. A.; Venskovskii, N. U.

    2008-01-01

    The complex [(NH 2 ) 2 CSSC(NH 2 ) 2 ] 2 [OsBr 6 ]Br 2 . 3H 2 O is synthesized by the reaction of K 2 OsBr 6 with thiocarbamide in concentrated HBr and characterized using electronic absorption and IR absorption spectroscopy. Its crystal structure is determined by X-ray diffraction. The crystals are orthorhombic, a = 11.730(2) A, b = 14.052(3) A, c = 16.994(3) A, space group Cmcm, and Z = 4. The [OsBr 6 ] 2- anionic complex has an octahedral structure. The Os-Br distances fall in the range 2.483-2.490 A. The α,α'-dithiobisformamidinium cation is a product of the oxidation of thiocarbamide. The S-S and C-S distances are 2.016 and 1.784 A, respectively. The H 2 O molecules, Br - ions, and NH 2 groups of the cation are linked by hydrogen bonds.

  20. (O-Methyl di­thio­carbonato-κS)tri­phenyl­tin(IV)

    Science.gov (United States)

    Javed, Fatima; Ali, Saqib; Shah, Wajid; Tahir, M. Nawaz; Ullah, Hameed

    2013-01-01

    In the title compound, [Sn(C6H5)3(C2H3OS2)], the SnIV atom adopts a distorted SnC3S tetra­hedral coordination geometry. A short Sn⋯O contact [2.988 (4) Å] is also present. The phenyl rings are each disordered over two sets of sites with an occupancy ratio of 0.550 (8):0.450 (8). The crystal studied was found to be a racemic twin with a twin component ratio of 0.57 (18):0.43 (18). PMID:23794982

  1. Homoleptic Diphosphacyclobutadiene Complexes [M(η(4)-P2C2R2)(2]x- (M = Fe, Co; x=0, 1)

    NARCIS (Netherlands)

    Wolf, R.; Ehlers, A.W.; Khusniyarov, M.M.; Hartl, F.; de Bruin, B.; Long, G.J.; Grandjean, F.; Schappacher, F.M.; Pöttgen, R.; Slootweg, J.C.; Lutz, M.; Spek, A.L.; Lammertsma, K.

    2010-01-01

    The preparation and comprehensive characterization of a series of homoleptic sandwich complexes containing diphosphacyclobutadiene ligands are reported. Compounds [K([18]crown-6)(thf)(2)[Fe(η(4)-P(2)C(2)tBu(2))(2)] (K1), [K([18]crown-6)(thf)(2)][Co(η(4)-P(2)C(2)tBu(2))(2)] (K2), and

  2. The molecular structure and vibrational spectra of N-(2,2-diphenylacetyl)- N'-(naphthalen-1yl)-thiourea by Hartree-Fock and density functional methods

    Science.gov (United States)

    Arslan, Hakan; Mansuroglu, Demet Sezgin; VanDerveer, Don; Binzet, Gun

    2009-04-01

    N-(2,2-Diphenylacetyl)- N'-(naphthalen-1yl)-thiourea (PANT) has been synthesized and characterized by elemental analysis, IR spectroscopy and 1H NMR spectroscopy. The crystal and molecular structure of the title compound has been determined from single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1, Z = 2 with a = 10.284(2) Å, b = 10.790(2) Å, c = 11.305(2) Å, α = 64.92(3)°, β = 89.88(3)°, γ = 62.99(3)°, V = 983.7(3) Å 3 and Dcalc = 1.339 Mg/m 3. The molecular structure, vibrational frequencies and infrared intensities of PANT were calculated by the Hartree-Fock and density functional theory methods (BLYP and B3LYP) using the 6-31G* basis set. The calculated geometric parameters were compared to the corresponding X-ray structure of the title compound. We obtained 22 stable conformers for the title compound; however Conformer 1 is approximately 9.53 kcal/mol more stable than Conformer 22. The comparison of the theoretical and experimental geometry of the title compound shows that the X-ray parameters fairly well reproduce the geometry of Conformer 17. The harmonic vibrations computed for this compound by the B3LYP/6-31G* method are in good agreement with the observed IR spectral data. Theoretical vibrational spectra of the title compound were interpreted by means of PEDs using the VEDA 4 program. A general better performance of the investigated methods was calculated by PAVF 1.0 program.

  3. Et2NH2C6H3(CO23SnBr2.4H2O: SYNTHESIS AND INFRARED STUDY

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    DAOUDA NDOYE

    2014-01-01

    Full Text Available The title compound has been obtained on allowing [C6H3(CO23(Et2NH23] to react with SnBr4. The molecular structure of Et2NH2C6H3(CO23SnBr2.4H2O has been determined on the basis of the infrared data. The suggested structure is a dimer in which each tin atom is hexacoordinated by two chelating C6H3(CO233- anions and two Br atoms. Cy2NH2+cations are involved through hydrogen bonds with non-coordinating CO2 groups. The suggested structure is a cage.

  4. 1-(Furan-2-yl-2-(2H-indazol-2-ylethanone

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    Özden Özel Güven

    2014-04-01

    Full Text Available The asymmetric unit of the title compound, C13H10N2O2, contains two crystallographically independent molecules (A and B. The indazole ring systems are approximately planar [maximum deviations = 0.0037 (15 and −0.0198 (15 Å], and their mean planes are oriented at 80.10 (5 and 65.97 (4° with respect to the furan rings in molecules A and B, respectively. In the crystal, pairs of C—H...N hydrogen bonds link the B molecules, forming inversion dimers. These dimers are bridged by the A molecules via C—H...O hydrogen bonds, forming sheets parallel to (011. There are also C—H...π interactions present, and π–π interactions between neighbouring furan and the indazole rings [centroid–centroid distance = 3.8708 (9 Å] of inversion-related molecules, forming a three-dimensional structure.

  5. Dimethyl 4,4′-dihydroxy-3,3′-{[(3aRS,7aRS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylene}dibenzoate

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2011-11-01

    Full Text Available The title compound, C25H30N2O6, has the imidazolidine ring in an envelope conformation. There are two intramolecular O—H...N hydrogen-bond interactions with graph-set motif S(6. The cyclohexane ring adopts a slightly distorted chair conformation. One methyl carboxylate substituent forms a dihedral angle of 12.00 (5° with the plane of the benzene ring, while the other methyl carboxylate group is almost coplanar, making a dihedral angle of 2.26 (9°. In the crystal, pairs of intermolecular C—H...O hydrogen bonds form racemic dimers, corresponding to an R22(18 graph-set motif. Further weak C—H...O interactions generate a chain running along the c axis.

  6. Crystal structures of the 2:2 complex of 1,1′-(1,2-phenylenebis(3-m-tolylurea and tetrabutylammonium chloride or bromide

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    Chao Huang

    2017-09-01

    Full Text Available The title compounds, tetrabutylammonium chloride–1,1′-(1,2-phenylenebis(3-m-tolylurea (1/1, C16H36N+·Cl−·C22H22N4O2 or [(n-Bu4N+·Cl−(C22H22N4O2] (I and tetrabutylammonium bromide–1,1′-(1,2-phenylenebis(3-m-tolylurea (1/1, C16H36N+·Br−·C22H22N4O2 or [(n-Bu4N+·Br−(C22H22N4O2] (II, both comprise a tetrabutylammonium cation, a halide anion and an ortho-phenylene bis-urea molecule. Each halide ion shows four N—H...X (X = Cl or Br interactions with two urea receptor sites of different bis-urea moieties. A crystallographic inversion centre leads to the formation of a 2:2 arrangement of two halide anions and two bis-urea molecules. In the crystals, the dihedral angle between the two urea groups of the bis-urea molecule in (I [defined by the four N atoms, 165.4 (2°] is slightly smaller than that in (II [167.4 (2°], which is probably due to the smaller ionic radius of chloride compared to bromide.

  7. Homoleptic diphosphacyclobutadiene complexes [M(η(4)-P2C2R2)2]x- (M = Fe, Co; x = 0, 1).

    Science.gov (United States)

    Wolf, Robert; Ehlers, Andreas W; Khusniyarov, Marat M; Hartl, František; de Bruin, Bas; Long, Gary J; Grandjean, Fernande; Schappacher, Falko M; Pöttgen, Rainer; Slootweg, J Chris; Lutz, Martin; Spek, Anthony L; Lammertsma, Koop

    2010-12-27

    The preparation and comprehensive characterization of a series of homoleptic sandwich complexes containing diphosphacyclobutadiene ligands are reported. Compounds [K([18]crown-6)(thf)(2)][Fe(η(4)-P(2)C(2)tBu(2))(2)] (K1), [K([18]crown-6)(thf)(2)][Co(η(4)-P(2)C(2)tBu(2))(2)] (K2), and [K([18]crown-6)(thf)(2)][Co(η(4)-P(2)C(2)Ad(2))(2)] (K3, Ad = adamantyl) were obtained from reactions of [K([18]crown-6)(thf)(2)][M(η(4)-C(14)H(10))(2)] (M = Fe, Co) with tBuC[triple bond]P (1, 2), or with AdC[triple bond]P (3). Neutral sandwiches [M(η(4)-P(2)C(2)tBu(2))(2)] (4: M = Fe 5: M = Co) were obtained by oxidizing 1 and 2 with [Cp(2)Fe]PF(6). Cyclic voltammetry and spectro-electrochemistry indicate that the two [M(η(4)-P(2)C(2)tBu(2))(2)](-)/[M(η(4)-P(2)C(2)tBu(2))(2)] moieties can be reversibly interconverted by one electron oxidation and reduction, respectively. Complexes 1-5 were characterized by multinuclear NMR, EPR (1 and 5), UV/Vis, and Mössbauer spectroscopies (1 and 4), mass spectrometry (4 and 5), and microanalysis (1-3). The molecular structures of 1-5 were determined by using X-ray crystallography. Essentially D(2d)-symmetric structures were found for all five complexes, which show the two 1,3-diphosphacyclobutadiene rings in a staggered orientation. Density functional theory calculations revealed the importance of covalent metal-ligand π bonding in 1-5. Possible oxidation state assignments for the metal ions are discussed.

  8. Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic perchlorates: (C6H18N3)·(ClO4)3H2O (I) and (C9H11N2)·ClO4(II)

    Science.gov (United States)

    Bayar, I.; Khedhiri, L.; Soudani, S.; Lefebvre, F.; Ferretti, V.; Ben Nasr, C.

    2018-06-01

    The reaction of perchloric acid with 1-(2-aminoethyl)piperazine or 5,6-dimethyl-benzimidazole results in the formation of 1-(2-amonioethyl)piperazine-1,4-dium triperchlorate hydrate (C6H18N3)·(ClO4)3·H2O (I) or 5,6-dimethyl-benzylimidazolium perchlorate (C9H11N2)·ClO4(II). Both compounds were fully structurally characterized including single crystal X-ray diffraction analysis. Compound (I) crystallizes in the centrosymmetric triclinic space group P 1 bar with the lattice parameters a = 7.455 (2), b = 10.462 (2), c = 10.824 (2) Å, α = 80.832 (2), β = 88.243 (2), γ = 88.160 (2) °, Z = 2 and V = 832.77 (3) Å3. Compound (II) has been found to belong to the P21/c space group of the monoclinic system, with a = 7.590 (3), b = 9.266 (3), c = 16.503 (6) Å, β = 107.38 (2) °, V = 1107.69 (7) Å3 and Z = 4. The structures of (I) and (II) consist of slightly distorted [ClO4]- tetrahedra anions and 1-(2-amonioethyl)piperazine-1,4-dium trication (I) or 5,6-dimethyl-benzylimidazolium cations (II) and additionally a lattice water in (I). The crystal structures of (I) and (II) exhibit complex three-dimensional networks of H-bonds connecting all their components. In the atomic arrangement of (I), the ClO4- anions form corrugated chains, while in (II) the atomic arrangement exhibits wide pseudo-hexagonal channels of ClO4 tetrahedra including the organic entities. The lattice water serves as a link between pairs of cations and pairs of anions via several Osbnd H⋯O and N-H⋯O interactions in compound (I). The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived.

  9. Synthesis and Molecular Structure of 6-Amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one

    Directory of Open Access Journals (Sweden)

    Gene-Hsiang Lee

    2006-03-01

    Full Text Available The title compound 6-amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]-triazin-8(7H-one (4, molecular formula C11H10N6OS, was obtained by the reaction of3-amino-2-benzyl-6-hydrazino-1,2,4-triazin-5(2H-one (3 with carbon disulfide in awater/pyridine mixture. Compound 4 can also be synthesized by reacting6-amino-3(2Hmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (7 with benzylbromide in methanolic ammonia water. The compound crystallizes in the monoclinicspace group P21/c with a = 7.2926(15, b = 14.456(2, c = 11.436(2 å, β = 105.30(2°, V= 1162.9(4 å3 and Z = 4, resulting in a density Dcalc of 1.567 g/cm3. Molecules of 4 arelinked by extensive intermolecular N-H···N and N-H···O hydrogen bonding [graph set R22 (9]. The structure is further stabilized by π-π stacking interactions. 2

  10. 9-(3-Bromo-5-chloro-2-hydroxyphenyl-10-(2-hydroxyethyl-3,6-diphenyl-3,4,9,10-tetrahydroacridine-1,8(2H,5H-dione

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2014-06-01

    Full Text Available In the title compound, C33H27BrClNO4, the dihydropyridine ring adopts a flattened boat conformation. The molecular conformation is stabilized by an intramolecular O—H...O hydrogen bond, with an S(8 ring motif. In the crystal, O—H...O, C—H...O and C—H...Cl hydrogen bonds, and C—H...π interactions link the molecules, forming a three-dimensional network. In the acridinedione ring system, the two ring C atoms at the 2- and 3-positions, and the C atom at the 6-position and the atoms of the phenyl ring attached to the C atom at the 6-position are disordered over two sets of sites with occupancy ratios of 0.783 (5:0.217 (5 and 0.526 (18:0.474 (18, respectively.

  11. (E-2-(2-Nitroethenylfuran

    Directory of Open Access Journals (Sweden)

    Pedro Valerga

    2009-08-01

    Full Text Available The title compound, C6H5NO3, was synthesized via condensation of furfural with nitromethane in the presence of isobutylamine. The compound crystallizes exclusively as the E isomer. The angle between the mean planes of the furan ring and the nitroalkenyl group is 1.3 (2°.

  12. trans-(2-Benzoylpyridine-κ2N,Odichlorido[2-(2-pyridylcarbonylphenyl-κ2C1,N]iridium(III dichloromethane solvate

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The title compound, [Ir(C12H8NOCl2(C12H9NO]·CH2Cl2, which was obtained from the reaction of iridium(III chloride trihydrate and 2-benzoylpyridine, contains an IrIII atom coordinated by two N, one O, one C and two Cl atoms in trans positions, forming a distorted octahedral environment. The solvent molecule CH2Cl2 is disordered over two positions with an occupancy of 0.8:0.2.

  13. Crystal structure of 26-(4-methylphenyl-8,11,14,17-tetraoxa-28-azatetracyclo[22.3.1.02,7.018,23]hexacosa-2,4,6,18(23,19,21,24(1,25,27-nonaene

    Directory of Open Access Journals (Sweden)

    T. Thanh Van Tran

    2016-05-01

    Full Text Available The title compound, C30H29NO4, is a tetracyclic system containing a 4-arylpyridine fragment, two benzene rings and an aza-17-crown-5 ether moiety, in a bowl-like arrangement. The pyridine ring is inclined to the 4-methylphenyl ring by 26.64 (6°, and by 57.43 (6 and 56.81 (6° to the benzene rings. The benzene rings are inclined to one another by 88.32 (6°. In the crystal, molecules are linked by pairs of C—H...N hydrogen bonds, forming inversion dimers with an R22(14 ring motif. The dimers are linked via a number of C—H...π interactions, forming a three-dimensional architecture.

  14. 5,5′-(Ethyne-1,2-diyldiisophthalic acid dimethyl sulfoxide tetrasolvate

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    Alexander S. Münch

    2013-06-01

    Full Text Available In the title compound, C18H10O8·4C2H6OS, the mid-point of the triple bond of the main molecule is located on a special position, i.e. about an inversion center. The carboxyl groups are twisted slightly out of the planes of the aromatic rings to which they are attached, making dihedral angles of 24.89 (1 and 7.40 (2°. The cystal packing features strong O—H...O hydrogen bonds, weaker C—H...O interactions and O...S contacts [3.0981 (11 Å] and displays channel-like voids extending along the a-axis direction which contain the dimethyl sulfoxide solvent molecules.

  15. (4,4′-Dimethoxy-2,2′-bipyridine-κ2N,N′bis[2-(pyridin-2-ylphenyl-κC1]iridium(III hexafluoridophosphate unknown solvate

    Directory of Open Access Journals (Sweden)

    Yano Natsumi

    2016-03-01

    Full Text Available The asymmetric unit of the title complex, [Ir(C11H8N2(C12H12N2O2]PF6, comprises a [Ir(ppy2(diMeO-bpy]+ cation (Hppy = 2-phenylpyridine and diMeO-bpy = 4,4′-dimethoxy-2,2′-bipyridine and a PF6− anion. The IrIII atom is coordinated by two anionic ppy− ligands, each coordinating in a C^N cyclometalated mode, and one neutral diMeO-bpy ligand, leading to a distorted octahedral geometry defined by a cis-C2N4 donor set. Intermolecular C—F...H contacts lead to a three-dimensional architecture that define columns parallel to a. Unknown disordered solvent molecules reside in these columns with the electron density being treated with SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18]. The unit-cell data do not reflect the presence of the unresolved solvent.

  16. Di-tert-butyl-bis(N-isopropyl-N-methyl-dithio-carbamato-κS,S')tin(IV).

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Samsudin, Mohd Wahid; Ng, Seik Weng

    2010-03-03

    The dithio-carbamate anions in the title compound, [Sn(C(4)H(9))(2)(C(5)H(10)NS(2))(2)], chelate to the Sn(IV) atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol-ecule lies across a twofold rotation axis. The crystal studied was a non-merohedral twin, the ratio of the twin components being 0.82 (1):0.18 (1).

  17. Di-tert-butylbis(N-isopropyl-N-methyldithiocarbamato-κ2S,S′tin(IV

    Directory of Open Access Journals (Sweden)

    Amirah Faizah Muthalib

    2010-04-01

    Full Text Available The dithiocarbamate anions in the title compound, [Sn(C4H92(C5H10NS22], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The molecule lies across a twofold rotation axis. The crystal studied was a non-merohedral twin, the ratio of the twin components being 0.82 (1:0.18 (1.

  18. 5-Fluoro-6′H,7′H,8′H-spiro[indoline-3,7′-pyrano[3,2-c:5,6-c′]di-1-benzopyran]-2,6′,8′-trione

    Directory of Open Access Journals (Sweden)

    J. Suresh

    2012-03-01

    Full Text Available In the title compound, C26H12FNO6, the central pyran ring and both benzopyran systems are nonplanar, having total puckering amplitudes of 0.139 (2, 0.050 (1 and 0.112 (2 Å, respectively. The central pyran ring adopts a boat conformation. The crystal structure is stabilized by C—H...O, N—H...O, N—H...F and C—H...π interactions.

  19. Synthesis of 7-[α-(2-amino-[2-14C]thiazol-4-yl)-α-(Z)-methoxyimin oacetamido]-3-(1-methylpyrrolidinio)methyl-3-cephem-4-carboxylate hydrochloride ([14C]cefepime hydrochloride)

    International Nuclear Information System (INIS)

    Standridge, R.T.; Swigor, J.E.

    1993-01-01

    The title compound ([ 14 C]cefepime hydrochloride) was prepared as follows:- [ 14 C]Thiourea was condensed with ethyl 4-bromo-3-oxo-2-methoxyimino-acetate providing ethyl 2-(2-amino-4-[2- 14 C] thiazolyl)-2-methoxyi-minoacetate as the pure Z-isomer. Saponification gave the amino acid this was reacted with 1-hydroxybenzotriazole to give the activated ester. Condensation in situ with 7-amino-3-(1-methylpyrrolidinio) methyl-3-cephem-4-carboxylate yielded the product as the pure sulfate salt. Treatment of the sulfate salt with base provided the zwitterion isolated as the stable N-methyl-2-pyrrolidinone adduct. An aqueous solution of the adduct was converted to the crystalline title compound, [ 14 C]Cefepime hydrochloride hydrate, with hydrochloric acid/acetone. Radiochemical purity was 99.0% and specific activity, 34.2 μCi/mg. Overall yield from [ 14 C]thiourea was 18%. (Author)

  20. Crystal structure of 2-isopropyl-4-methoxy-5-methylphenyl 4-methylbenzenesulfonate

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    Yassine Laamari

    2018-03-01

    Full Text Available The title compound, C18H22O4S, an hemisynthetic product, was obtained by the tosylation reaction of the naturally occurring meroterpene p-methoxythymol. The molecule comprises a tetrasubstitued phenyl ring linked to a toluenesulfonate through one of its O atoms. In the crystal, C—H...O and C—H...π interactions link the molecules, forming a three-dimensional network.

  1. Structure and bonding of transition metal-boryl compounds. Theoretical study of [(PH3)2(CO)ClOs-BR2] and [(PH3)2(CO)2ClOs-BR2] (BR2 = BH2, BF2, B(OH)2, B(OCH=CHO), Bcat).

    Science.gov (United States)

    Giju, K T; Bickelhaupt, F M; Frenking, G

    2000-10-16

    Quantum chemical DFT calculations using the B3LYP functionals have been carried out for the electronically unsaturated 16 VE five-coordinate osmium boryl-complexes [(PH3)2(CO)ClOs-BR2] and the 18 VE six-coordinate complexes [(PH3)2(CO)2ClOs-BR2] with BR2 = BH2, BF2, B(OH)2, B(OHC=CHO), and Bcat (cat = catecholate O2C6H4). The bonding situation of the Os-BR2 bond was analyzed with the help of the NBO partitioning scheme. The Os-B bond dissociation energies of the 16 VE complexes are very high, and they do not change very much for the different boryl ligands. The 18 VE complexes have only slightly lower bond energies than the 16 VE species. The Os-B bond in both classes of compounds is provided by a covalent sigma-bond which is polarized toward osmium and by strong charge attraction. Os-->B pi-donation is not important for the Os-B binding interactions, except for the Os-BH2 complexes. The stability of the boryl complexes [Os]-BR2 comes mainly from BB pi-donation. The intraligand charge distribution of the BR2 group changes little when the Os-B bond is formed, except for BH2. The CO ligand in [(PH3)2(CO)2ClOs-BR2] which is trans to BR2 has a relatively weak bond to the osmium atom.

  2. Three closely related 4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridines: synthesis, molecular conformations and hydrogen bonding in zero, one and two dimensions.

    Science.gov (United States)

    Sagar, Belakavadi K; Harsha, Kachigere B; Yathirajan, Hemmige S; Rangappa, Kanchugarakoppal S; Rathore, Ravindranath S; Glidewell, Christopher

    2017-03-01

    In each of 1-(4-fluorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 F 4 N 3 O 2 S, (I), 1-(4-chlorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 ClF 3 N 3 O 2 S, (II), and 1-(3-methylphenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 22 H 22 F 3 N 3 O 2 S, (III), the reduced pyridine ring adopts a half-chair conformation with the methylsulfonyl substituent occupying an equatorial site. Although compounds (I) and (II) are not isostructural, having the space groups Pbca and P2 1 2 1 2 1 , respectively, their molecular conformations are very similar, but the conformation of compound (III) differs from those of (I) and (II) in the relative orientation of the N-benzyl and methylsulfonyl substituents. In compounds (II) and (III), but not in (I), the trifluoromethyl groups are disordered over two sets of atomic sites. Molecules of (I) are linked into centrosymmetric dimers by C-H...π(arene) hydrogen bonds, molecules of (II) are linked by two C-H...O hydrogen bonds to form ribbons of R 3 3 (18) rings, which are themselves further linked by a C-Cl...π(arene) interaction, and a combination of C-H...O and C-H...π(arene) hydrogen bonds links the molecules of (III) into sheets. Comparisons are made with the structures of some related compounds.

  3. Synthesis and pharmacological properties of new derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones.

    Science.gov (United States)

    Sladowska, Helena; Sabiniarz, Aleksandra; Sapa, Jacek; Filipek, Barbara

    2009-01-01

    Synthesis of 2-(2-hydroxy-3-amino)propyl derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (24-35) is described. The chlorides used in the above synthesis exist mainly in the cyclic forms (18, 20-23). Only chloride with benzhydryl substituent at the nitrogen atom of piperazine has the chain structure (19). Among the studied imides the most active analgesics in the "writhing" syndrome test proved to be compounds 30 and 31 (with LD50 > 2000 mg/kg) containing 4-benzylpiperidino group. Furthermore, all imides suppressed significantly spontaneous locomotor activity of mice.

  4. A novel synthesis of octahydropyrido[3,2-c]carbazole framework of aspidospermidine alkaloids and a combined computational, FT-IR, NMR, NBO, NLO, FMO, MEP study of the cis-4a-Ethyl-1-(2hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole

    Science.gov (United States)

    Uludağ, Nesimi; Serdaroğlu, Goncagul; Yinanc, Abdullah

    2018-06-01

    In this study, we performed a novel synthesis of the octahydropyrido[3,2-c]carbazole derivative 6 from 1 in five steps with a 34% overall yield. We also developed a unique compound 2 by a cyclization reaction from the cyanoethylation of compound 1, which is an intermediate step in the synthesis of Aspidospermidine. The parent compound of Aspidospermidine alkaloids, comprise a large family of diverse structures. As a result, we obtained octahydropyrido[3,2-c]carbazole (6)and the proposed method may be applicable to other alkaloids. All quantum chemical calculations of the cis-4a-Ethyl-1-(2-hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole have been performed with the DFT/B3LYP and HF methods by using the Gaussian 09W software package. The most stable conformer obtained from the Potential Energy Surface (PES) scan analysis at the B3LYP/6-31G** level of theory in the gas phase was used as the starting structure of the title compound to further computational analysis. The Natural Bond Orbital (NBO) and NLO analyses were performed to evaluate the intra-molecular interactions contributing to the molecular stability and to predict the optical properties of the title compound, respectively. Gauge-Independent Atomic Orbital (GIAO) approach was used to determine the 1H and 1C NMR chemical shifts of the title compound by subtracting the shielding constants of TMS at both methods. The calculated vibrational frequencies of the title compound were assigned by using the VEDA program and were scaled down by using the scaling factor 0.9668 for B3LYP/6-311++G(d, p) and 0.9050 for HF/6-311++G(d, p) to improve the calculated vibrational frequencies. The FMO (frontier molecular orbital) analysis was evaluated to predict the chemical and physical properties of the title compound and the HOMO, LUMO, and MEP diagrams were visualized by GaussView 4.1 program to present the reactive site of the title compound.

  5. Syntheses, Raman spectra, and X-ray crystal structures of [XeF(5)][mu-F(OsO(3)F(2))(2)] and [M][OsO(3)F(3)] (M = XeF(5)(+), Xe(2)F(11)(+)).

    Science.gov (United States)

    Hughes, Michael J; Mercier, Hélène P A; Schrobilgen, Gary J

    2010-04-05

    Stoichiometric amounts of XeF(6) and (OsO(3)F(2))(infinity) react at 25-50 degrees C to form salts of the known XeF(5)(+) and Xe(2)F(11)(+) cations, namely, [XeF(5)][mu-F(OsO(3)F(2))(2)], [XeF(5)][OsO(3)F(3)], and [Xe(2)F(11)][OsO(3)F(3)]. Although XeF(6) is oxophilic toward a number of transition metal and main-group oxides and oxide fluorides, fluoride/oxide metathesis was not observed. The series provides the first examples of noble-gas cations that are stabilized by metal oxide fluoride anions and the first example of a mu-F(OsO(3)F(2))(2)(-) salt. Both [XeF(5)][mu-F(OsO(3)F(2))(2)] and [Xe(2)F(11)][OsO(3)F(3)] are orange solids at room temperature. The [XeF(5)][OsO(3)F(3)] salt is an orange liquid at room temperature that solidifies at 5-0 degrees C. When the salts are heated at 50 degrees C under 1 atm of N(2) for more than 2 h, significant XeF(6) loss occurs. The X-ray crystal structures (-173 degrees C) show that the salts exist as discrete ion pairs and that the osmium coordination spheres in OsO(3)F(3)(-) and mu-F(OsO(3)F(2))(2)(-) are pseudo-octahedral OsO(3)F(3)-units having facial arrangements of oxygen and fluorine atoms. The mu-F(OsO(3)F(2))(2)(-) anion is comprised of two symmetry-related OsO(3)F(2)-groups that are fluorine-bridged to one another. Ion pairing results from secondary bonding interactions between the fluorine/oxygen atoms of the anions and the xenon atom of the cation, with the Xe...F/O contacts occurring opposite the axial fluorine and from beneath the equatorial XeF(4)-planes of the XeF(5)(+) and Xe(2)F(11)(+) cations so as to avoid the free valence electron lone pairs of the xenon atoms. The xenon atoms of [XeF(5)][mu-F(OsO(3)F(2))(2)] and [Xe(2)F(11)][OsO(3)F(3)] are nine-coordinate and the xenon atom of [XeF(5)][OsO(3)F(3)] is eight-coordinate. Quantum-chemical calculations at SVWN and B3LYP levels of theory were used to obtain the gas-phase geometries, vibrational frequencies, and NBO bond orders, valencies, and NPA charges of

  6. Nonacarbonyl-1κ3C,2κ3C,3κ3C-μ-bis(diphenylarsinomethane-1:2κ2As:As'-[tris(2-chloroethyl phosphite-3κP]-triangulo-triruthenium(0

    Directory of Open Access Journals (Sweden)

    Omar bin Shawkataly

    2010-08-01

    Full Text Available In the title triangulo-triruthenium(0 compound, [Ru3(C25H22As2(C6H12Cl3O3P(CO9], the bis(diphenylarsinomethane ligand bridges an Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. In the crystal packing, the molecules are linked by intermolecular C—H...O hydrogen bonds into a three-dimensional framework. Weak intermolecular C—H...π interactions further stabilize the crystal structure.

  7. Activation of sp3-CH Bonds in a Mono(pentamethylcyclopentadienyl)yttrium Complex. X-ray Crystal Structures and Dynamic Behavior of Cp*Y(o-C6H4CH2NMe2)2 and Cp*Y[o-C6H4CH2NMe(CH2-μ)][μ-o-C6H4CH2NMe(CH2-μ)]YCp*[THF

    NARCIS (Netherlands)

    Booij, Martin; Kiers, Niklaas H.; Meetsma, Auke; Teuben, Jan H.; Smeets, Wilberth J.J.; Spek, Anthony L.

    1989-01-01

    Reaction of Y(o-C6H4CH2NMe2)3 (1) with Cp*H gives Cp*Y(o-C6H4CH2NMe2)2 (2), which crystallizes in the monoclinic space group P21/n (No. 14) with a = 18.607 (4) Å, b = 15.633 (3) Å, c = 8.861 (3) Å, β = 102.73 (3)°, and Z = 4. Least-squares refinement with 3006 independent reflections (F > 4.0σ(F))

  8. Magnetic measurements and neutron diffraction study of the layered hybrid compounds Mn(C8H4O4)(H2O)2 and Mn2(OH)2(C8H4O4)

    International Nuclear Information System (INIS)

    Sibille, Romain; Mesbah, Adel; Mazet, Thomas; Malaman, Bernard; Capelli, Silvia; François, Michel

    2012-01-01

    Mn(C 8 H 4 O 4 )(H 2 O) 2 and Mn 2 (OH) 2 (C 8 H 4 O 4 ) layered organic–inorganic compounds based on manganese(II) and terephthalate molecules (C 8 H 4 O 4 2− ) have been studied by DC and AC magnetic measurements and powder neutron diffraction. The dihydrated compound behaves as a 3D antiferromagnet below 6.5 K. The temperature dependence of its χT product is typical of a 2D Heisenberg system and allows determining the in-plane exchange constant J≈−7.4 K through the carboxylate bridges. The magnetic structure confirms the in-plane nearest neighbor antiferromagnetic interactions and the 3D ordering. The hydroxide based compound also orders as a 3D antiferromagnet with a higher Néel temperature (38.5 K). Its magnetic structure is described from two antiferromagnetically coupled ferromagnetic sublattices, in relation with the two independent metallic sites. The isothermal magnetization data at 2 K are consistent with the antiferromagnetic ground-state of these compounds. However, in both cases, a slope change points to field-induced modification of the magnetic structure. - Graphical abstract: The macroscopic magnetic properties and magnetic structures of two metal-organic frameworks based on manganese (II) and terephthalate molecules are presented. Highlights: ► Magnetic study of Mn(C 8 H 4 O 4 )(H 2 O) 2 and Mn 2 (OH) 2 (C 8 H 4 O 4 ). ► Two compounds with common features (interlayer linker/distance, S=5/2 spin). ► Magnetic measurements quantitatively analyzed to deduce exchange constants. ► Magnetic structures determined from neutron powder diffraction experiments.

  9. Diethyl 2,2′-({[1,4-phenylenebis(azanediyl]bis(methylene}bis(1H-pyrrole-2,1-diyldiacetate

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    Jasim Alshawi

    2016-01-01

    Full Text Available The complete molecule of the title compound, C24H30N4O4, is generated by crystallographic inversion symmetry. The molecule is S-shaped and the pyrrole groups have an anti or trans confirmation with respect to the central benzene ring, to which they are inclined by 76.38 (9°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming layers parallel to the ac plane. Within the layers there are C—H...π interactions present. There are, however, no significant interactions between the layers.

  10. 3H-1,2-Benzodithiole-3-thione

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    Khaled Boukebbous

    2016-10-01

    Full Text Available The almost planar (r.m.s. deviation = 0.034 Å title compound, C7H4S3, was synthesized by reacting 2,2-dithiodibenzoic acid with phosphorus pentasulfide in xylene solution. In the crystal, short S...S [3.3727 (14, 3.3765 (13 and 3.4284 (13 Å] contacts and aromatic π–π stacking [shortest centroid–centroid separation = 3.618 (2 Å] are observed.

  11. Crystallographic characterization of divalent organosamarium compound (C5H5)2Sm(THF)2

    International Nuclear Information System (INIS)

    Jagannatha Swamy, S.

    2002-01-01

    The single pot reaction between SmX 2 (X = Cl - , I - ) and BuLi in THF at -40 degC, followed by the addition of C 5 H 5 - Na + results in a dark red solution. Leaving the concentrated reaction mixture at -25 degC for two days in a deep freezer results in the formation of the crystals of the compound, (C 5 H 5 ) 2 ; Sm(THF) 2 . The compound is insoluble in any solvent and it has been characterized by conventional methods. The crystals are monoclinic with space group C2/c, and a = 13.416(1), b = 9.644(1), c = 14.129(2) pm, β109.873(9) 0 and z = 4 for ρcalcd = 1.64 g cm -3 . Least squares refinement on the basis of 1804 observed reflections has led to a final R value of 0.037 and R w = 0.054. (author)

  12. Ethyl 2-(2-oxo-3-phenyl-1,2-dihydroquinoxalin-1-ylacetate

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    Nadeem Abad

    2018-04-01

    Full Text Available In the title compound, C18H16N2O3, the dihydroquinoxaline moiety is planar (r.m.s. deviation = 0.0115 Å and the majority of the ester substituent is nearly perpendicular to its mean plane. In the crystal, the molecules form oblique stacks along the b-axis direction through slipped π–π stacking interactions between adjacent dihydroquinoxaline units. C—H...O hydrogen bonds between the ester substituents on adjacent stacks form thick layers with the stacks on their outside surfaces. These layers extend along the c-axis direction and are coupled through C—H...π(ring interactions. The structure was refined as a two-component twin.

  13. (2S-1,1-Dichloro-2-(2-chlorophenyl-2-(4-chlorophenylethane

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    Lars Eriksson

    2009-02-01

    Full Text Available The title compound, C14H10Cl4, is easily crystallized while the other enantiomorph only forms an oil upon crystallization attempts. The title compound has a considerably higher density, ρ ≃ 1.562 Mg m−3 compared to the racemic substance, ρ ≃ 1.514 Mg m−3. This is supported by the fact there are two intermolecular halogen–halogen contacts in the title compound compared with only one the racemic compound. The dihedral angle between the two phenyl rings is 76.83 (5°

  14. Synthesis of heterocyclic compounds through palladium-catalyzed C-H cyclization processes.

    Science.gov (United States)

    Inamoto, Kiyofumi

    2013-01-01

    Herein, we describe our development of synthetic methods for heterocyclic compounds based on the palladium-catalyzed carbon-hydrogen bond (C-H) functionalization/intramolecular carbon-heteroatom (nitrogen or sulfur) bond formation process. By this C-H cyclization method, we efficiently prepared various N-heterocycles, including indazoles, indoles, and 2-quinolinones, as well as S-heterocycles such as benzothiazoles and benzo[b]thiophenes. Yields are typically good to high and good functional-group tolerance is observed for each process, thereby indicating that the method provides a novel, highly applicable synthetic route to the abovementioned biologically important heterocyclic frameworks. As an application of this approach, an auto-tandem-type, one-pot process involving the oxidative Heck reaction and subsequent C-H cyclization using cinnamamides and arylboronic acids as starting materials in the presence of a palladium catalyst was also developed for the rapid construction of the 2-quinolinone nucleus.

  15. mer-Bis[3,5-difluoro-2-(2-pyridylphenyl-κ2C1,N]{5-(2-pyridyl-κN-3-[3-(4-vinylbenzyloxyphenyl]-1,2,4-triazol-1-ido}iridium(III methanol solvate

    Directory of Open Access Journals (Sweden)

    Peter G. Jones

    2010-01-01

    Full Text Available In the title compound, [Ir(C11H6F2N2(C22H17N4O]·CH3OH, the coordination at iridium is essentially octahedral, but with distortions associated with the bite angles of the ligands [76.25 (9–80.71 (12°] and the differing trans influences of C and N ligands [Ir—N = 2.04 Å (average trans to N but 2.14 Å trans to C]. All three bidentate ligands have coordinating ring systems that are almost coplanar [interplanar angles = 1.7 (1–3.8 (2°]. The vinylbenzyl group is disordered over two positions with occupations of 0.653 (4 and 0.347 (4. The methanol solvent molecule is involved in a classical O—H...N hydrogen bond to a triazole N atom.

  16. 22 CFR 18.22 - Notice of disciplinary action.

    Science.gov (United States)

    2010-04-01

    ... 22 Foreign Relations 1 2010-04-01 2010-04-01 false Notice of disciplinary action. 18.22 Section 18... INTEREST Administrative Enforcement Proceedings § 18.22 Notice of disciplinary action. Upon the issuance of... Department during the period of suspension. The Director General shall take other appropriate disciplinary...

  17. Crystal structure and thermochemical properties of n-decylammonium ethyl sulfate (C10H21NH3SO4C2H5)(s)

    International Nuclear Information System (INIS)

    Zhang, Li-Jun; Di, You-Ying; Dou, Jian-Min

    2013-01-01

    Graphical abstract: Crystal structure of n-decylammonium ethyl sulfate was determined by X-ray crystallography. Lattice potential energy and molar volume of the solid compound and its anion were respectively obtained. Molar enthalpies of dissolution of the compound at different concentrations were measured by an isoperibol solution–reaction calorimeter. According to the Pitzer’s electrolyte solution theory, molar enthalpy of dissolution of the compound at infinite dilution and Pitzer parameters were obtained. The values of apparent relative molar enthalpies of the title compound and relative partial molar enthalpies of the solute and the solvent at different concentrations were derived. Finally, enthalpies of hydration of the compound and its anion were calculated. Highlights: ► Crystal structure of n-decylammonium ethyl sulfate was determined. ► Lattice potential energy was calculated. ► Molar enthalpy of dissolution at infinite dilution was determined. ► Enthalpies of hydration of the compound and its anion were derived. - Abstract: Crystal structure of n-decylammonium ethyl sulfate was determined by X-ray crystallography. Lattice potential energy and molar volume of the solid compound and its anion were respectively obtained. Ionic radius of the anion was calculated from the corresponding effective volume of the anion. Molar enthalpies of dissolution of the compound at different concentrations m /(mol · kg –1 ) were measured by an isoperibol solution–reaction calorimeter at T = 298.15 K. According to the Pitzer’s electrolyte solution theory, molar enthalpy of dissolution of the compound at infinite dilution (Δ sol H m ∞ ) was determined to be (21.284 ± 0.042) kJ·mol –1 , and enthalpy of hydration of the anion SO 4 C 2 H 5 − was calculated to be ΔH – = −340.68 kJ·mol –1 . The values of apparent relative molar enthalpies ( Φ L) of the title compound and relative partial molar enthalpies (L 2 ¯ and L 1 ¯ ) of the solute and

  18. N-{2-[2-(5-Methyl-1H-pyrazol-3-ylacetamido]phenyl}benzamide monohydrate

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    Karim Chkirate

    2017-02-01

    Full Text Available The asymmetric unit of the title compound, C19H18N4O2·H2O, comprises the U-shaped pyrazole derivative and a solvent water molecule. The molecular conformation is partly determined by an intramolecular N—H...O hydrogen bond. The crystal packing is directed by an extensive network of O—H...O, N—H...O, N—H...N and C—H...O hydrogen bonds together with C—H...π(ring contacts that generate a three-dimensional network.

  19. Di-tert-butyl­bis(N-isopropyl-N-methyl­dithio­carbamato-κ2 S,S′)tin(IV)

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Samsudin, Mohd Wahid; Ng, Seik Weng

    2010-01-01

    The dithio­carbamate anions in the title compound, [Sn(C4H9)2(C5H10NS2)2], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol­ecule lies across a twofold rotation axis. The crystal studied was a non-merohedral twin, the ratio of the twin components being 0.82 (1):0.18 (1). PMID:21580471

  20. Synthesis and crystal structures of new complexes of Np(V) glycolate with 2,2'-bipyridine, [NpO2(C10H8N2)(OOC2H2OH)].1.5H2O and [NpO2(C10H8N2)(OOC2H2OH)].2.5H2O

    International Nuclear Information System (INIS)

    Charushnikova, I.A.; Krot, N.N.; Starikova, Z.A.

    2009-01-01

    Single crystals were prepared, and the structures of two complexes of Np(V) glycolate with 2,2'-bipyridine of the compositions [NpO 2 (C 10 H 8 N 2 )(OOC 2 H 2 OH)].1.5H 2 O (I) and [NpO 2 (C 10 H 8 N 2 )(OOC 2 H 2 OH)]2.5H 2 O (II) were studied. The structures of the compounds are based on neptunyl-glycolate chains in which the glycolate anion manifests its complexation ability in different manner. In structure I, the bidentate-bridging anion links the adjacent NpO 2 - cations through the oxygen atoms of the carboxylate group. The neptunyl-glycolate chains of I exhibits the mutual coordination of the NpO 2 - cations acting toward each other simultaneously as ligands and coordinating centers. In compound II, the glycolate anion is bidentately coordinated to one neptunium atom to form a planar five-membered metallocycle [NpOCCO]. The O atom external with respect to the metallocycle is in the coordination environment of the adjacent neptunyl. The nitrogen-containing molecular ligand Bipy is included into the coordination environment of Np. The coordination polyhedron of the Np atoms in both structures is a pentagonal bipyramid in which the average Np-N bond length is 2.666 Aa (I) and 2.596 Aa (II). (orig.)

  1. Bis(acetylacetonato-κ2O,O′(2-amino-1-methyl-1H-benzimidazole-κN3oxidovanadium(IV

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    Zukhra Ch. Kadirova

    2009-07-01

    Full Text Available The title mixed-ligand oxidovanadium(IV compound, [VO(C5H7O22(C8H9N3], contains a VIV atom in a distorted octahedral coordination, which is typical for such complexes. The vanadyl group and the N-heterocyclic ligand are cis to each other. The coordination bond is located at the endocyclic N atom of the benzimidazole ligand. Intramolecular hydrogen bonds between the exo-NH2 group H atoms and acetylacetonate O atoms stabilize the crystal structure.

  2. 1-[3-(4-Chlorophenyl-5-(4-methoxyphenyl-4,5-dihydro-1H-pyrazol-1-yl]ethanone

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    Hoong-Kun Fun

    2012-04-01

    Full Text Available In the title compound, C18H17ClN2O2, the benzene rings form dihedral angles of 6.69 (6 and 74.88 (5° with the 4,5-dihydro-1H-pyrazole ring. The benzene rings form a dihedral angle of 76.67 (5° with each other. In the crystal, molecules are linked via bifurcated (C,C–H...O hydrogen bonds into chains along [010]. The crystal structure is further consolidated by C—H...π interactions.

  3. 2,2′-[Biphenyl-2,2′-diylbis(oxy]diacetic acid monohydrate

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    Kuldip Singh

    2008-10-01

    Full Text Available In the crystal structure of the title compound, C16H14O6·H2O, the dihedral angle between the benzene rings is 60.8 (3°. Molecules are linked through a bifurcated O—H...O hydrogen bond, forming a zigzag chain along the b axis. The chains are further linked by O—H...O hydrogen bonds mediated by water molecules.

  4. (2aR*,5S*,6aS*,8aS*,E-Ethyl 5-hydroxy-7,7,8a-trimethyl-8-oxo-2,2a,6,6a,7,8,8a,8b-octahydro-1H-pentaleno[1,6-bc]oxepine-4-carboxylate

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    Goverdhan Mehta

    2012-12-01

    Full Text Available The title compound, C17H24O5, featuring a 2-carbethoxy-3-oxepanone unit in its intramolecularly O—H...O hydrogen-bonded enol form, was obtained via [(CF3CO22Rh]2-catalysed intramolecular O—H bond insertion in the α-diazo-ω-hydroxy-β-ketoester, ethyl 4-[(1S,3aS,6R,6aS-6-hydroxy-2,2,3a-trimethyl-3-oxo-octahydropentalen-1-yl]-2-diazo-3-oxobutanoate. The seven-membered oxacyclic ring, thus constructed on a cis-fused diquinane platform, was found to adopt a distorted boat–sofa conformation.

  5. Synthesis, spectral characterization and anti-microbial activity of 6- Substituted [(2-aminoethylamino]-6λ 5-dibenzo [d, h] [1, 3,6,2]oxathiaza- phosphonin-6-ones

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    Chinta Raveendra Reddy

    2011-01-01

    Full Text Available Synthesis of a series of a new class of phosphorus macrocycles was accomplished in two steps by condensation of (Z-2-((2-mercaptophenylimino methyl phenol (1 with phosphorus oxychloride (2 in dry THF in the presence of triethylamine at 0-5 °C. In the second step ethylene diols/ amino alcohols/ diamine/ aminothiols/ phenols were reacted at room temperature in THF to afford the title compounds (5a-l. The chemical structures of the title products were characterized by IR, 1H, 13C, 31P-NMR, mass spectral studies and elemental analysis. All the title compounds were evaluated for antimicrobial activity to determine their efficacy and they were found role effective in suppressing the growth of bacteria and fungi.

  6. 10a-Hydroxy-9-(4-methoxyphenyl-3,4,5,6,7,8a,9,10a-octahydro-1H-xanthene-1,8(2H-dione

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    Hoong-Kun Fun

    2012-08-01

    Full Text Available In the title compound, C20H22O5, the tetrahydropyran, cyclohexene and cyclohexane rings of the xanthene ring system adopt half-chair, half-boat and chair conformations, respectively. The mean plane of the four roughly planar atoms of the tetrahydropyran ring (r.m.s. deviation = 0.111 Å forms a dihedral angle of 82.91 (4° with the methoxybenzene group. In the crystal, molecules are linked via O—H...O and C—H...O hydrogen bonds into sheets lying parallel to the ac plane. The crystal is further consolidated by weak C—H...π interactions.

  7. Crystal structure of N′-diphenylmethylidene-5-methyl-1H-pyrazole-3-carbohydrazide

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    Khalid Karrouchi

    2015-11-01

    Full Text Available In the title compound, C18H16N4O, the planes of the phenyl rings are approximately perpendicular to each other [dihedral angle = 78.07 (8°] and form dihedral angles of 56.43 (8 and 24.59 (8° with the pyrazole ring. In the crystal, molecules are linked by N—H...O hydrogen bonds to form one-dimensional chains parallel to the [010] direction.

  8. (Acetato-κO{bis[(2,4-dimethyl-1H-pyrazol-1-ylmethyl][(pyridin-2-ylmethyl]amine}cobalt(II hexafluoridophosphate

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    Fan Yu

    2012-10-01

    Full Text Available In the title compound, [Co(CH3CO2(C18H24N6]PF6, the CoII atom is pentacoordinated in a distorted trigonal–bipyramidal geometry by four N atoms from a tripodal ligand and one O atom from a monodentate acetate ligand. The crystal packing is stabilized by intermolecular C—H...F and C—H...O hydrogen bonds.

  9. Quinolactacins A, B and C: novel quinolone compounds from Penicillium sp. EPF-6. II. Physico-chemical properties and structure elucidation.

    Science.gov (United States)

    Takahashi, S; Kakinuma, N; Iwai, H; Yanagisawa, T; Nagai, K; Suzuki, K; Tokunaga, T; Nakagawa, A

    2000-11-01

    Three novel quinolone compounds, quinolactacins A (1), B (2) and C (3), have been found from the fermentation broth of Penicillium sp. EPF-6, a fungus isolated from the larvae of mulberry pyralid (Margaronia pyloalis Welker). The molecular formulas of 1, 2 and 3 were determined to be C16H18N2O2, C15H16N2O2 and C16H18N2O3, respectively by FAB-MS and NMR spectral analyses. The structures of these compounds have a novel quinolone skeleton with a gamma-lactam ring consisting of C12H8N2O2 as the common chromophore.

  10. (3R,4Z-1,3-Diethyl-4-(2-oxopropylidene-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one

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    Laila El Foujji

    2018-04-01

    Full Text Available In the title compound, C16H20N2O2, the seven-membered ring adopts a bowl-shaped conformation while the orientation of the 2-oxopropylidene substituent is determined by an intramolecular N—H...O hydrogen bond, which generates an S(6 ring. In the crystal, inversion dimers linked by pairs of very weak C—H...O interactions occur, which generate R22(8 loops.

  11. Crystal strucutre of rac-methyl (11aR*,12S*,13R*,15aS*,15bS*-11-oxo-11,11a,12,13-tetrahydro-9H,15bH-13,15a-epoxyisoindolo[1,2-c]pyrrolo[1,2-a][1,4]benzodiazepine-12-carboxylate

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    Vladimir P. Zaytsev

    2014-12-01

    Full Text Available The title compound, C21H18N2O4, obtained as a racemate, contains a novel heterocyclic system, viz. isoindolo[1,2-c]pyrrolo[1,2-a][1,4]benzodiazepine. The central diazepane ring has a distorted boat conformation with two phenylene-fused and one methine C atom deviating by 0.931 (1, 0.887 (1 and 0.561 (1 Å, respectively, from the mean plane of the rest of the ring. The γ-lactone ring has an envelope conformation, with the C atom opposite to amide bond deviating by 0.355 (1 Å from its plane. In the crystal, molecules form centrosymmetric dimers through pairs of C—H...O hydrogen bonds.

  12. Crystal structure of catena-poly[[aqua(2,2′:6′,2′′-terpyridine-κ3N,N′,N′′cobalt(II]-μ-cyanido-κ2N:C-[dicyanidoplatinum(II]-μ-cyanido-κ2C:N

    Directory of Open Access Journals (Sweden)

    Frankie White

    2014-09-01

    Full Text Available The title compound, [Co(C15H11N3(H2O{Pt(CN4}]n, is a one-dimensional coordination polymer formed under hydrothermal reaction conditions. The CoII site has sixfold coordination with a distorted octahedral geometry, while the PtII ion is coordinated by four cyanide groups in an almost regular square-planar geometry. The compound contains twofold rotation symmetry about its CoII ion, the water molecule and the terpyridine ligand, and the PtII atom resides on an inversion center. trans-Bridging by the tetracyanidoplatinate(II anions links the CoII cations, forming chains parallel to [-101]. Additionally, each CoII atom is coordinated by one water molecule and one tridentate 2,2′:6′,2′′-terpyridine ligand. O—H...N hydrogen-bonding interactions are found between adjacent chains and help to consolidate the crystal packing. In addition, relatively weak π–π stacking interactions exist between the terpyridine ligands of adjacent chains [interplanar distance = 3.464 (7 Å]. No Pt...Pt interactions are observed in the structure.

  13. New metal-organic frameworks of [M(C6H5O7)(C6H6O7)(C6H7O7)(H2O)] . H2O (M=La, Ce) and [Ce2(C2O4)(C6H6O7)2] . 4H2O

    International Nuclear Information System (INIS)

    Weng Shengfeng; Wang, Yun-Hsin; Lee, Chi-Shen

    2012-01-01

    Two novel materials, [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2), with a metal-organic framework (MOF) were prepared with hydrothermal reactions and characterized with photoluminescence, magnetic susceptibility, thermogravimetric analysis and X-ray powder diffraction in situ. The crystal structures were determined by single-crystal X-ray diffraction. Compound 1 crystallized in triclinic space group P1-bar (No. 2); compound 2 crystallized in monoclinic space group P2 1 /c (No. 14). The structure of 1 is built from a 1D MOF, composed of deprotonated citric ligands of three kinds. Compound 2 contains a 2D MOF structure consisting of citrate and oxalate ligands; the oxalate ligand arose from the decomposition in situ of citric acid in the presence of Cu II ions. Photoluminescence spectra of compounds 1b and 2 revealed transitions between the 5d 1 excited state and two levels of the 4f 1 ground state ( 2 F 5/2 and 2 F 7/2 ). Compounds 1b and 2 containing Ce III ion exhibit a paramagnetic property with weak antiferromagnetic interactions between the two adjacent magnetic centers. - Graphical Abstract: [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2)—with 1D and 2D structures were synthesized and characterized. Highlights: ► Two MOF – [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2) – with 1D and 2D structures. ► The adjacent chains of the 1D framework were correlated with each other through an oxalate ligand to form a 2D layer structure. ► The source of the oxalate ligand was the decomposition in situ of citric acid oxidized in the presence of Cu II ions.

  14. N,N′-Bis(4-aminobenzyloxalamide

    Directory of Open Access Journals (Sweden)

    Juan Saulo Gonzalez-Gonzalez

    2011-02-01

    Full Text Available In the title compound, C16H18N4O2, the two carbonyl groups are in an antiperiplanar conformation with an O=C—C=O torsion angle of 173.86 (17°. In the crystal, a pair of intermolecular N—H...O hydrogen bonds, forming an R22(10 ring motif, connect the molecules into an inversion dimer. The dimers are further linked by N—H...N and C—H...π interactions, forming a zigzag chain along the b axis.

  15. 1,1′-[Imidazolidine-1,3-diylbis(methylene]bis(1H-benzotriazole

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    Augusto Rivera

    2012-02-01

    Full Text Available In the title compound, C17H18N8, the imidazolidine ring adopts an envelope conformation with the substituents at the N atoms in trans positions with respect to the central ring. The dihedral angle between the two benzotriazole rings is 71.65 (10°. In the crystal, non-classical C—H...N interactions link the molecules into helical chains along the b axis. The crystal packing is further stabilized by weak C—H...π interactions.

  16. (E-3-[5-(Diphenylaminothiophen-2-yl]-1-(pyridin-3-ylprop-2-en-1-one

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    Rui Li

    2013-09-01

    Full Text Available In the title compound, C24H18N2OS, the pyridine and the two phenyl rings are oriented at dihedral angles of 10.1 (5, 71.7 (6 and 68.7 (5°, respectively, to the central thiophene ring. In the crystal, pairs of weak C—H...O hydrogen bonds link inversion-related molecules, forming dimers. The dimers are linked by further weak C—H...O hydrogen bonds, forming chains running along the a-axis direction.

  17. 1,2-Bis(2-methoxy-6-formylphenoxyethane

    Directory of Open Access Journals (Sweden)

    Hongqi Li

    2011-02-01

    Full Text Available In the title compound [systematic name: 3,3′-dimethoxy-2,2′-(ethane-1,2-diyldioxydibenzaldehyde], C18H18O6, prepared from 1,2-dibromoethane and ortho-vanillin in the presence of sodium carbonate, the two vanillin units are linked via a CH2–CH2 bridge. The two benzene rings are inclined at a dihedral angle of 41.6 (5°.

  18. (1R,6R,13R,18R-(Z,Z-1,18-Bis[(4R-2,2-dimethyl-1,3-dioxolan-4-yl]-3,16-dimethylene-8,20-diazadispiro[5.6.5.6]tetracosa-7,19-diene

    Directory of Open Access Journals (Sweden)

    Stéphanie M. Guéret

    2010-07-01

    Full Text Available The crystal structure of the title compound, C34H54N2O4, has been solved in order to prove the relative and absolute chirality of the newly-formed stereocentres which were established using an asymmetric Diels–Alder reaction at an earlier stage in the synthesis. This unprecedented stable dialdimine contains a 14-membered ring and was obtained as the minor diastereoisomer in the Diels–Alder reaction. The absolute stereochemistry of the stereocentres of the acetal functionality was known to be R based on the use of a chiral (R-trisubstituted dienophile derived from enantiopure (S-glyceraldehyde. The assignment of the configuration in the dienophile and the title di-aldimine differs from (S-glyceraldehyde due to a change in the priority order of the substituents. The crystal structure establishes the presence of six stereocentres all attributed to be R. The 14-membered ring contains two aldimine bonds [C—N = 1.258 (2 and 1.259 (2 Å]. It adopts a similar conformation to that proposed for trans–trans-cyclotetradeca-1,8-dienes.

  19. 1,5-Bis(2,5-dimethyl-1H-pyrrol-1-ylnaphthalene

    Directory of Open Access Journals (Sweden)

    A. C. Santos

    2009-11-01

    Full Text Available In the title compound, C22H22N2, the asymmetric unit contains one half-molecule. A crystallographic inversion centre is located at the mid-point of the bond common to both rings, in the central naphthalene unit. Quantum-mechanical ab initio calculations on the isolated molecule showed that the minimum energy configuration occurs when the naphthalene ring system and the pyrrolyl groups deviate only slightly from perpendicularity. In the crystal, due to the effects of crystal packing, the molecule deviates by approximately 4° from the a priori expected ideal value of 90° [C—C—N—C torsion angle = 86.11 (15°].

  20. TGA, Hirshfeld, Raman spectroscopy and computational studies of diethylammonium hexachloroplumbate [(C2H5)2NH2]2PbCl6

    Science.gov (United States)

    Ouasri, A.; El-Adel, L.; Zouihri, H.; Rhandour, A.; Jalbout, A. F.

    2018-04-01

    Diethylammonium hexachloroplumbate [(C2H5)2NH2]2PbCl6 was found to be monoclinic with P21/n (Z = 2) as space group at room temperature. The TGA analysis shows that this compound is slightly hygroscopic and presents moisture in itself. The Raman spectrum (50-4000 cm-1) of this compound recorded at room temperature was discussed on the basis of the factor group analysis using the structural data obtained recently [5]. The experimental frequencies are compared to those obtained by Density Functional Theory (DFT) by using the B3LYP functional and the 6-31G(d) (SDD) basis set. The thermodynamic properties and geometries of this compound have been determinated and characterized. The significant intermolecular interactions in the crystal structure are identified and analyzed using the Hirshfeld surface and fingerprint plots computational methods.

  1. 1-Phenyl-5-{[2-(trimethylsilylethyl]sulfonyl}-1H-tetrazole

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    David Tymann

    2011-09-01

    Full Text Available The title compound, C12H18N4O2SSi, was synthesized to be employed in a Julia–Kocieński olefination. In the molecule, the dihedral angle between the phenyl ring and the tetrazole ring is 41.50 (5°. The significantly longer Si—C(methylene bond [1.8786 (13 Å] and the shortened adjacent C—C bond [1.5172 (18 Å], as well as the significant deviation of the corresponding Si—C—C angle [114.16 (9°] from the ideal tetrahedral angle, can be attributed to the β-effect of silicon. In the crystal, molecules are held together by van der Waals interactions.

  2. 10-Ethyl-3-(5-methyl-1,3,4-oxadiazol-2-yl-10H-phenothiazine

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    Li-Cheng Sun

    2012-03-01

    Full Text Available In the title compound, C17H15N3OS, the phenothiazine ring system is slightly bent, with a dihedral angle of 13.68 (7° between the benzene rings. The dihedral angle between the oxadiazole ring and the adjacent benzene ring is 7.72 (7°. In the crystal, a π–π interaction with a centroid–centroid distance of 3.752 (2 Å is observed between the benzene rings of neighbouring molecules.

  3. 13-Hydroxy-4,16-dimethyl-4,16-diazapentacyclo[12.3.1.01,5.05,13.07,12]octadeca-7(12,8,10-triene-6,18-dione

    Directory of Open Access Journals (Sweden)

    K. Gurunathan

    2009-05-01

    Full Text Available In the title compound, C18H20N2O3, the N-methylpiperidone ring adopts a chair conformation. The pyrrolidine ring and the five-membered cyclopentane rings adopt envelope conformations. The five-membered ring of the ninhydrin system adopts an envelope conformation with the central C atom deviating by 0.217 (1Å from the mean plane through the other atoms. The molecular packing is characterized by intermolecular C—H...O and intramolecular C—H...O and O—H...N interactions.

  4. Crystal structure of 4-allylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine

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    Mohammed El Fal

    2014-09-01

    Full Text Available In the title compound, C8H8N4S, the pyrazolo[3,4-d]pyrimidine ring system is essentially planar, with a maximum deviation from the mean plane of 0.025 (3 Å. The allyl group is disordered over two sites in a 0.512 (6:0.488 (6 ratio. In the crystal, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(8 graph-set motif.

  5. Crystal structure of fac-[2-(4-methyl-5-phenylpyridin-2-ylphenyl-κ2C1,N]bis[2-(pyridin-2-ylphenyl-κ2C1,N]iridium(III

    Directory of Open Access Journals (Sweden)

    Chi-Heon Lee

    2016-12-01

    Full Text Available In the title compound, [Ir(C11H8N2(C18H14N], the IrIII ion adopts a distorted octahedral coordination environment defined by three C,N-chelating ligands, one stemming from a 2-(4-phenyl-5-methylpyridin-2-ylphenyl ligand and two from 2-(pyridin-2-ylphenyl ligands, arranged in a facial manner. The IrIII ion lies almost in the equatorial plane [deviation = 0.0069 (15 Å]. In the crystal, intermolecular π–π stacking interactions, as well as intermolecular C—H...π interactions, are present, leading to a three-dimensional network.

  6. Fluorine-18 labelled compounds

    International Nuclear Information System (INIS)

    Kleijn, J.P. de

    1978-01-01

    The work presented in this thesis deals with the problems involved in the adaption of reactor-produced fluorine-18 to the synthesis of 18 F-labelled organic fluorine compounds. Several 18 F-labelling reagents were prepared and successfully applied. The limitations to the synthetic possibilities of reactor-produced fluoride- 18 become manifest in the last part of the thesis. An application to the synthesis of labelled aliphatic fluoro amino acids has appeared to be unsuccessful as yet, although some other synthetic approaches can be indicated. Seven journal articles (for which see the availability note) are used to compose the four chapters and three appendices. The connecting text gives a survey of known 18 F-compounds and methods for preparing such compounds. (Auth.)

  7. {4,4′,6,6′-Tetraiodo-2,2′-[(2,2-dimethylpropane-1,3-diylbis(nitrilomethanylylidene]diphenolato}nickel(II

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    Hadi Kargar

    2012-07-01

    Full Text Available The asymmetric unit of the title compound, [Ni(C19H16I4N2O2], comprises half of a Schiff base complex. The NiII atom is located on a twofold rotation axis which also bisects the central C atom of the 2,2-dimethylpropane group of the ligand. The geometry around the NiII atom is distorted square-planar, with a dihedral angle of 21.7 (3° between the symmetry-related N/Ni/O coordination planes. The dihedral angle between the symmetry-related benzene rings is 27.9 (3°. In the crystal, short intermolecular I...I [3.8178 (9 and 3.9013 (10 Å] interactions are present.

  8. Computational Material Modeling of Hydrated Cement Paste Calcium Silicate Hydrate (C-S-H) Chemistry Structure - Influence of Magnesium Exchange on Mechanical Stiffness: C-S-H Jennite

    Science.gov (United States)

    2015-04-27

    MODELING OF C-S-H Material chemistry level modeling following the principles and techniques commonly grouped under Computational Material Science is...Henmi, C. and Kusachi, I. Monoclinic tobermorite from fuka, bitchu-cho, Okoyama Perfecture. Japan J. Min. Petr. Econ . Geol. (1989)84:374-379. [22...31] Liu, Y. et al. First principles study of the stability and mechanical properties of MC (M=Ti, V, Zr, Nb, Hf and Ta) compounds. Journal of Alloys and Compounds. (2014) 582:500-504. 10

  9. Crystal structure of bis[μ-S-hexyl 3-(2-oxidobenzylidenedithiocarbazato-κ4O,N3,S:O]dicopper(II

    Directory of Open Access Journals (Sweden)

    M. S. Begum

    2015-12-01

    Full Text Available The title compound, [Cu2(C14H18N2OS22], is a binuclear copper(II complex of an oxybenzylidenedithiocarbazate ligand. The ligand coordinates in a tridentate manner through N-, S- and O-donor atoms. Each O atom also bridges to a second CuII ion to form the binuclear species. It has a central Cu2O2 rhomboid moiety and a metal-to-metal separation of 2.9923 (6 Å. In the crystal, the binuclear complexes stack along the a axis with all the hexyl chains located side-by-side, forming a hydrophobic region. The complexes are linked via C—H...N hydrogen bonds, forming chains along the c-axis direction. One CuII atom has the S atom of a symmetry-related complex located approximately in the apical position at 2.9740 (11 Å. This weak interaction links the chains to form slabs parallel to the ac plane.

  10. Experimental and semi-empirical and DFT calculational studies on (E)-2-((2-morpholinoethyliminio)methyl)-4-nitrophenolate

    International Nuclear Information System (INIS)

    Alpaslan, Y. B.; Agar, E.; Ersahin, F.; Iskeleli, N. O.; Oeztekin, E.

    2010-01-01

    The molecular and crystal structure of the title compound, C 1 3H 1 7N 3 O 4 , has been determined by X-ray single crystal diffraction technique. The compound crystallizes in the triclinic, space group P-1 with unit cell dimensions a=5.3520(4), b=10.9011(8), c=12.4537(9)A 0 , Mr=279.30, V=675.91(9)A 03 , Z=2, R1=0.037 and wR 2 =0.097. The molecule adopts a zwitterionic form, stabilized by an intramolecular N + -H 2 O- type ionic weak hydrogen bond. The molecule pack via intermolecular N-H 2 O hydrogen bonds which, together with an intramolecular N + -H 2 O- bond. Calculational studies were performed by using AM1, PM3, semi-empirical and DFT methods. Geometry optimizations of compound have been carried out by using three semi-empirical methods and DFT method and bond lengths, bond and torsion angles of title compound have been determined. Atomic charge distribution have been obtained from DFT. In order to determine conformational flexibility on the molecule, molecular energy profile of the title compound was obtained with respect to the selected torsion angle T(C2-C1-C7-N1), which is varied from -180 0 degree to +180 0 degree in every 10 via PM3 semi-empirical method.

  11. (3aS,7aS-5-[(S-3,3,3-Trifluoro-2-methoxy-2-phenylpropanoyl]-2,3,4,5,6,7-hexahydro-1H-pyrrolo[3,4-c]pyridin-3(2H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Huichun Zhu

    2010-01-01

    Full Text Available rac-Benzyl 3-oxohexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H-carboxylate was separated by chiral chromatography, and one of the enantiomers ([α]22D = +10° was hydrogenated in the presence of Pd/C in methanol, producing octahydro-3H-pyrrolo[3,4-c]pyridin-3-one. The latter was reacted with (2R-3,3,3-trifluoro-2-methoxy-2-phenylpropanoyl chloride [(R-(−-Mosher acid chloride], giving rise to the title compound, C17H19F3N2O3·H2O. The present structure established the absolute configuration of the pyrrolopiperidine fragment based on the known configuration of the (R-Mosher acid chloride. The piperidine ring has a somewhat distorted chair conformation and is cis-fused with the five-membered envelope-shaped ring; the plane of the exocyclic amide bond is approximately orthogonal to the plane of the phenyl ring, making a dihedral angle of 82.31 (3°. The water molecule acts as an acceptor to the proton of the amino group in an N—H...O interaction, and as a double proton donor in O—H...O hydrogen bonds, generating infinite bands along the a axis.

  12. 2,2′,5,5′-Tetrachlorobenzidine

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    Onome Ugono

    2010-09-01

    Full Text Available In the crystal structure of the title compound, C12H8Cl4N2, molecules lie on crystallographic twofold axes at the centre of the C—C bonds linking the benzene rings, such that the asymmetric unit consists of a half-molecule. The individual molecules participate in intermolecular N—H...N, N—H...Cl, C—H...Cl and Cl...Cl [3.4503 (3 Å] interactions.

  13. 4-Methyl-5-phenyl-1H-pyrazol-3-ol

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    Tara Shahani

    2010-07-01

    Full Text Available The title compound, C10H10N2O, crystallizes with two independent molecules in the asymmetric unit, having closely comparable geometries. The dihedral angles between the 1H-pyrazole and benzene rings in the two molecules are 39.57 (14 and 41.95 (13°. The two molecules are each connected to neighbouring molecules by pairs of intermolecular O—H...N hydrogen bonds, forming dimers with R22(8 ring motifs. These dimers are further linked into R44(10 ring motifs by intermolecular N—H...O hydrogen bonds, forming chains along [101]. The crystal structure is further stabilized by a C—H...π interaction.

  14. (2-Methyl-4-oxo-4H-pyran-3-olato-κ2O3,O4bis(triphenylphosphane-κPcopper(I–triphenylphosphane–methanol (1/1/1

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    Fabian M. A. Muller

    2011-05-01

    Full Text Available In the title compound, [Cu(C6H5O3(C18H15P2]·C18H15P·CH3OH, the pyran-4-one ring is appromimately planar (r.m.s deviation = 0.0138 Å, with the CuI atom 0.451 (5 Å out of the plane. The CuI atom has a distorted tetrahedral coordination. The O—Cu—O angle is 80.07 (8° and the P—Cu—P angle is 123.49 (3°. The crystal packing is stablized by intramolecular C—H...O interactions and intermolecular C—H...O and O—H...O interactions.

  15. Characterization of Rice Homeobox Genes, OsHOX22 and OsHOX24, and Over-expression of OsHOX24 in Transgenic Arabidopsis Suggest their Role in Abiotic Stress Response

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    Annapurna eBhattacharjee

    2016-05-01

    Full Text Available Homeobox transcription factors are well known regulators of plant growth and development. In this study, we carried out functional analysis of two candidate stress-responsive HD-ZIP I class homeobox genes from rice, OsHOX22 and OsHOX24. These genes were highly upregulated under various abiotic stress conditions at different stages of rice development, including seedling, mature and reproductive stages. The transcript levels of these genes were enhanced significantly in the presence of plant hormones, including abscisic acid (ABA, auxin, salicylic acid and gibberellic acid. The recombinant full-length and truncated homeobox proteins were found to be localized in the nucleus. Electrophoretic mobility shift assay established the binding of these homeobox proteins with specific DNA sequences, AH1 (CAAT(A/TATTG and AH2 (CAAT(C/GATTG. Transactivation assays in yeast revealed the transcriptional activation potential of full-length OsHOX22 and OsHOX24 proteins. Homo- and hetero-dimerization capabilities of these proteins have also been demonstrated. Further, we identified putative novel interacting proteins of OsHOX22 and OsHOX24 via yeast-two hybrid analysis. Over-expression of OsHOX24 imparted higher sensitivity to stress hormone, ABA, and abiotic stresses in the transgenic Arabidopsis plants as revealed by various physiological and phenotypic assays. Microarray analysis revealed differential expression of several stress-responsive genes in transgenic lines as compared to wild-type. Many of these genes were found to be involved in transcriptional regulation and various metabolic pathways. Altogether, our results suggest the possible role of OsHOX22/OsHOX24 homeobox proteins as negative regulators in abiotic stress responses.

  16. 4-Benzyl-6-bromo-2-(4-chlorophenyl)-4H-imidazo[4,5-b]pyridine

    OpenAIRE

    Selma Bourichi; Youssef Kandri Rodi; Jerry P. Jasinski; Manpreet Kaur; Younes Ouzidan; El Mokhtar Essassi

    2017-01-01

    In the title compound, C19H13BrClN3, the chlorophenyl ring occupies an equatorial position with respect to the mean plane of the imidazopyridine unit, while the other phenyl ring is twisted by 4.1 (2)° with respect to the mean plane of the imidazopyridine unit. In the crystal, pairwise C—H...Br interactions link the molecules into dimers, forming an R22(16) ring motif. In addition, weak π–π stacking interactions stabilize the crystal packing.

  17. 4-Benzyl-6-bromo-2-(4-chlorophenyl-4H-imidazo[4,5-b]pyridine

    Directory of Open Access Journals (Sweden)

    Selma Bourichi

    2017-06-01

    Full Text Available In the title compound, C19H13BrClN3, the chlorophenyl ring occupies an equatorial position with respect to the mean plane of the imidazopyridine unit, while the other phenyl ring is twisted by 4.1 (2° with respect to the mean plane of the imidazopyridine unit. In the crystal, pairwise C—H...Br interactions link the molecules into dimers, forming an R22(16 ring motif. In addition, weak π–π stacking interactions stabilize the crystal packing.

  18. 2-{[2-Methyl-3-(2-methylphenyl-4-oxo-3,4-dihydroquinazolin-8-yl]oxy}acetonitrile

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    Adel S. El-Azab

    2012-07-01

    Full Text Available In the title compound, C18H15N3O2, the fused ring system is almost planar [the dihedral angle between the six-membered rings is 1.81 (6°]. The 2-tolyl ring is approximately orthogonal to this plane [dihedral angle = 83.03 (7°] as is the acetonitrile group [C—O—C—C torsion angle = 79.24 (14°] which is also syn to the methyl substituent of the tolyl group. In the crystal, supramolecular layers are formed in the bc plane mediated by C—H...O, C—H...N and C—H...π interactions. The tolyl group is disordered over two positions in a 0.852 (3:0.148 (3 ratio.

  19. Syntheses, structures and redox properties of some complexes containing the Os(dppe)Cp* fragment, including [{Os(dppe)Cp*}2(mu-C triple bondCC triple bond C)].

    Science.gov (United States)

    Bruce, Michael I; Costuas, Karine; Davin, Thomas; Halet, Jean-François; Kramarczuk, Kathy A; Low, Paul J; Nicholson, Brian K; Perkins, Gary J; Roberts, Rachel L; Skelton, Brian W; Smith, Mark E; White, Allan H

    2007-12-14

    The sequential conversion of [OsBr(cod)Cp*] (9) to [OsBr(dppe)Cp*] (10), [Os([=C=CH2)(dppe)Cp*]PF6 ([11]PF6), [Os(C triple bond CH)(dppe)Cp*] (12), [{Os(dppe)Cp*}2{mu-(=C=CH-CH=C=)}][PF6]2 ([13](PF6)2) and finally [{Os(dppe)Cp*}(2)(mu-C triple bond CC triple bond C)] (14) has been used to make the third member of the triad [{M(dppe)Cp*}2(mu-C triple bond CC triple bond C)] (M = Fe, Ru, Os). The molecular structures of []PF6, 12 and 14, together with those of the related osmium complexes [Os(NCMe)(dppe)Cp*]PF6 ([15]PF6) and [Os(C triple bond CPh)(dppe)Cp*] (16), have been determined by single-crystal X-ray diffraction studies. Comparison of the redox properties of 14 with those of its iron and ruthenium congeners shows that the first oxidation potential E1 varies as: Fe approximately Os < Ru. Whereas the Fe complex has been shown to undergo three sequential 1-electron oxidation processes within conventional electrochemical solvent windows, the Ru and Os compounds undergo no fewer than four sequential oxidation events giving rise to a five-membered series of redox related complexes [{M(dppe)Cp*}2(mu-C4)]n+ (n = 0, 1, 2, 3 and 4), the osmium derivatives being obtained at considerably lower potentials than the ruthenium analogues. These results are complimented by DFT and DT DFT calculations.

  20. HFE C282Y/H63D Compound Heterozygotes Are at Low Risk of Hemochromatosis-Related Morbidity

    OpenAIRE

    Gurrin, Lyle C.; Bertalli, Nadine A.; Dalton, Gregory W.; Osborne, Nicholas J.; Constantine, Clare C.; McLaren, Christine E.; English, Dallas R.; Gertig, Dorota M.; Delatycki, Martin B.; Nicoll, Amanda J.; Southey, Melissa C.; Hopper, John L.; Giles, Graham G.; Anderson, Gregory J.; Olynyk, John K.

    2009-01-01

    The risk of hemochromatosis-related morbidity is unknown among HFE compound heterozygotes (C282Y/H63D). We used a prospective population-based cohort study to estimate the prevalence of elevated iron indices and hemochromatosis-related morbidity for compound heterozygotes. In all, 31,192 subjects of northern European descent were genotyped for HFE C282Y and H63D. An HFE-genotype stratified random sample of 1,438 subjects, followed for an average of 12 years to a mean age of 65 years, complete...

  1. Preparation of 14c- amd 180-labeled 2-[2-methoxy-4-(methylsulfinyl)phenyl]-1H-imidazo[4,5-c]-pyridine hydrochloride (LY175326), a cardiotonic with inotropic and vasodilator activities

    International Nuclear Information System (INIS)

    Kau, Don; Krushinski, J.H.; Robertson, D.W.

    1985-01-01

    Two different forms of 14 C-labeled 2-methoxy-4-(methyl-thio)benzoic acid were prepared and employed in the synthesis of 14 C-labeled 2-:2-methoxy-4-(methylsulfinyl)phenyl:-1H-imidazo-[4,5-c]pyridine hydrochloride (LY175326), a cardiotonic with inotropic and vasodilator activities that is currently in clinical trials. The synthetic procedures described in this report allowed the introduction of the 14 C-label in the antepenultimate step. Additionally, an 18 0-labeled form of LY175326 was synthesized to facilitate kinetic analysis of the formation of its sulfide and sulfone metabolites. (author)

  2. [2,6-Difluoro-3-(pyridin-2-yl-κNpyridin-4-yl-κC4](pentane-2,4-dionato-κ2O,O′iridium(III

    Directory of Open Access Journals (Sweden)

    Kaijun Luo

    2013-11-01

    Full Text Available The title compound, [Ir(C10H5F2N22(C5H7O2], has a distorted octahedral coordination geometry around the IrIII atom, retaining the cis-C,C/trans-N,N chelate disposition in two 2,6-difluoro-3-(pyridin-2-yl-κNpyridin-4-yl ligands which are nearly mutually perpendicular [dihedral angle = 82.75 (15°]. The molecular structure is stabilized by weak C—H...O and C—H...F hydrogen-bond interactions. The crystal structure is stabilized by π–π stacking interactions (centroid–centroid distance = 3.951 Å.

  3. Poly[diaqua(μ-4,4′-bipyridine-κ2N:N′[μ-2,2′-(p-phenylenedioxydiacetato-κ2O:O′]cadmium

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    Guang-Yin Wang

    2011-09-01

    Full Text Available In the title compound, [Cd(C10H8O6(C10H8N2(H2O2]n, the CdII ion has inversion symmetry and is coordinated by O atoms from two water molecules and two bridging 2,2′-(μ-p-phenylenedioxydiacetate ligands and two N atoms from two 4,4′-bipyridine ligands, giving a slightly distorted octahedral geometry. The diacetate and 4,4′-bipyridine ligands also lie across inversion centers. The bridging ligands form layers parallel to (11overline{1}, with adjacent layers interconnected via O—H...O hydrogen bonds between the coordinated water molecules and the carboxylate O atoms, giving a three-dimensional supramolecular architecture.

  4. 5-tert-Butyl 3-ethyl 1-isopropyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine-3,5-dicarboxylate

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    Huan-Mei Guo

    2011-12-01

    Full Text Available In the title compound, C17H27N3O4, the six-membered ring adopts a half-chair conformation with the N atom and the adjacent methylene C atom displaced by −0.391 (2 and 0.358 (2 Å, respectively, from the plane of the other four atoms. In the crystal, molecules are linked by weak C—H...O interactions.

  5. N,N-Diethyl-2-[5-(4-methoxybenzylidene-2,4-dioxo-1,3-thiazolidin-3-yl]acetamide

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    Vijayan Viswanathan

    2017-05-01

    Full Text Available In the title compound, C17H20N2O4S, the thiazolidine (r.m.s. deviation = 0.022 Å and phenyl rings (major and minor occupancies are inclined to one another by 6.3 (3 and 10.5 (3°, respectively. The molecular conformation is stabilized by an intramolecular C—H...S interaction. In the crystal, molecules are linked by C—H...O hydrogen bonds, which generate R22(18, R22(24 and R21(7 ring motifs. Aromatic π–π stacking interactions are also observed.

  6. (E-1-(2-Aminophenyl-3-(benzo[d][1,3]dioxol-5-ylprop-2-en-1-one

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    Rodrigo Abonia

    2016-12-01

    Full Text Available The title chalcone (E-1-(2-aminophenyl-3-(benzo[d][1,3]dioxol-5-ylprop-2-en-1-one was obtained in 76% yield from a NaOH catalyzed Claisen–Schmidt condensation reaction between o-aminoacetophenone and piperonal. This product will be used as a key precursor for the development of an alternative route for the total synthesis of the alkaloid Graveoline. Single crystals of the title compound suitable for X-ray diffraction were grown via slow evaporation in ethanol at room temperature. A complete crystallographic study was performed in depth to unequivocally confirm its structure. The crystal structure of the title o-aminochalcone, C16H13NO3, shows two molecules per asymmetric unit (Z = 4 and adopts an E configuration about the C=C double bond. In the title compound, the mean plane of the non-H atoms of the central chalcone fragment C—C(O—C—C—C is as follow: [root-mean-square (r.m.s. deviation = 0.0210 Å for A–B and 0.0493 for C–D molecules]. In the crystal, molecules are linked by N–H...O and C–H...O, hydrogen bonds forming S(6, R22(6 and edge-fused R44(24rings along with C(18 chains running parallel to (110.

  7. Aquabis(3,5-dimethyl-1H-pyrazole-κN(oxalato-κ2O,O′copper(II

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    Andrii I. Buvailo

    2008-01-01

    Full Text Available In the title compound, [Cu(C2O4(C5H8N22(H2O], the CuII atom is coordinated in a slightly distorted square-pyramidal geometry by two N atoms belonging to the two 3,5-dimethyl-1H-pyrazole ligands, two O atoms of the oxalate anion providing an O,O′-chelating coordination mode, and an O atom of the water molecule occupying the apical position. The crystal packing shows a well defined layer structure. Intra-layer connections are realised through a system of hydrogen bonds while the nature of the inter-layer interactions is completely hydrophobic, including no hydrogen-bonding interactions.

  8. μ-Oxalato-κ4O1,O2:O1′,O2′-bis[aqua(2,2′-bipyridine-κN(nitrato-κ2O,O′lead(II

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    Gang-Hong Pan

    2012-10-01

    Full Text Available The title compound, [Pb2(C2O4(NO32(C10H8N22(H2O2], was synthesized hydrothermally. The binuclear complex molecule is centrosymmetric, the inversion centre being located at the mid-point of the oxalate C—C bond. The PbII ion is heptacoordinated by the O atom of one water molecule, two oxalate O atoms, two nitrate O atoms and two 2,2′-bipyridine N atoms, forming an irregular coordination environemnt. Intermolecular O—H...O hydrogen bonds between water molecules and oxalate and nitrate ions result in the formation of layers parallel to (010. π–π interactions between pyridine rings in adjacent layers, with centroid–centroid distances of 3.584 (2 Å, stabilize the structural set-up.

  9. P(O)R2-Directed Enantioselective C-H Olefination toward Chiral Atropoisomeric Phosphine-Olefin Compounds.

    Science.gov (United States)

    Li, Shi-Xia; Ma, Yan-Na; Yang, Shang-Dong

    2017-04-07

    An effective synthesis of chiral atropoisomeric biaryl phosphine-olefin compounds via palladium-catalyzed enantioselective C-H olefination has been developed for the first time. The reactions are operationally simple, tolerate wide functional groups, and have a good ee value. Notably, P(O)R 2 not only acts as the directing group to direct C-H activation in order to make a useful ligand but also serves to facilitate composition of the product in a useful manner in this transformation.

  10. Tris[2-(2-thienylmethylaminoethyl]ammonium triiodide

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    Muhammet Işıklan

    2010-11-01

    Full Text Available In the title compound, C21H33N4S33+·3I−, three secondary amines are protonated, while the central amine remains unprotonated. One thiophene is disordered with an occupancy ratio of 0.868 (6/0.132 (6. Each protonated amine is involved in N—H...I hydrogen-bonding interactions with the iodide anions.

  11. Non-Classical Transformation of Benzendiazonium Hydrogen Sulfates. Access to 1,3-Dimethylisochromeno[4,3-c]pyrazol-5(1H-one, a Potential Benzodiazepine Receptor Ligand

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    Giuseppe Daidone

    2013-10-01

    Full Text Available The compound 2-((1,3-dimethyl-1H-pyrazol-5-yl(methylcarbamoylbenzene-diazonium hydrogen sulfate (10 was reacted with copper sulfate and sodium chloride, in the presence of ascorbic acid as reducing agent, to afford a mixture of the chlorinated epimers 4′-chloro-2,2′,5′-trimethyl-2′,4′-dihydrospiro[isoindoline-1,3′-pyrazol]-3-one (18 and (19, the epimers 4′-hydroxy-2,2′,5′-trimethyl-2′,4′-dihydrospiro[isoindoline-1,3′-pyrazol]-3-one (20 and (21, and N-(1,3-dimethyl-1H-pyrazol-5-ylbenzamide (22. Under the foregoing conditions, diazonium salt 10 affords neither the 2-chloro-N-(1,3-dimethyl-1H-pyrazol-5-yl-N-methylbenzamide (23 nor the tricyclic derivative 24, the classical products of the Sandmeyer and Pschorr reactions, respectively. Finally, by heating 20 at 210 °C the compound 1,3-dimethylisochromeno[4,3-c]pyrazol-5(1H-one (24 was obtained. The transformation under the above conditions of 2-((4-chloro-3-methyl-1-phenyl- 1H-pyrazol-5-yl(methylcarbamoylbenzendiazonium hydrogen sulphate (11 afforded 4′,4′-dichloro-2,5′-dimethyl-2′-phenyl-2′,4′-dihydrospiro[isoindoline-1,3′-pyrazol]-3-one (29 as the sole reaction product.

  12. 5-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione

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    Salman A. Khan

    2010-03-01

    Full Text Available The title compound, 5-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione, has been synthesized by condensation of 1,3-diethyl-2-thiobarbituric acid and 3,5-dimethyl-1-phenylpyrazole-4-carbaldehyde in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and EI-MS spectral analysis.

  13. Spectroscopic (FT-IR, FT-Raman, UV, 1H and 13C NMR insights, electronic profiling and DFT computations on ({(E-[3-(1H-imidazol-1-yl-1-phenylpropylidene] amino}oxy(4-nitrophenylmethanone, an imidazole-bearing anti-Candida agent

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    Al-Wahaibi Lamya H.

    2018-02-01

    Full Text Available The anti-Candida agent, ({(E-[3-(1H-imidazol-1-yl-1-phenylpropylidene]amnio}oxy(4-nitropheny methanone (IPAONM, was subjected to comprehensive spectroscopic (FT-IR, FT-Raman, UV–Vis 1H and 13C NMR characterization as well as Hartree Fock and density functional theory computation studies. The selected optimized geometric bond lengths and bond angles of the IPAONM molecule were compared with the experimental values. The calculated wavenumbers have been scaled and compared with the experimental spectra. Mulliken charges and natural bond orbital analysis of the title molecule were calculated and interpreted. The energy and oscillator strengths of the IPAONM molecule were calculated by time-dependent density functional theory (TD-DFT. In addition, frontier molecular orbitals and molecular electrostatic potential diagram of the title compound were computed and analyzed. A study on the electronic properties, such as HOMO, HOMO-1, LUMO and LUMO+1 energies was carried out using TD-DFT approach. The 1H and 13C NMR chemical shift values of the title compound were calculated by the gauge independent atomic orbital method and compared with the experimental results.

  14. 2-[2-Chloro-5-(trifluoromethylphenyl]hexahydropyrimidine monohydrate

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    Reza Kia

    2008-09-01

    Full Text Available The molecule of the title compound, C11H12ClF3N2·H2O, is a substituted hexahydropyrimidine. There are two crystallographically independent molecules (A and B and two water molecules in the asymmetric unit of the title compound. Intermolecular C—H...Cl (× 2, C—H...F, and C—H...N (× 2 hydrogen bonds generate S(5 ring motifs. The dihedral angle between the two benzene rings is 8.17 (11°. The F atoms in molecule B are disordered over four positions with refined site-occupancies of ca 0.35/0.19/0.29/0.17 for the four components. In the crystal structure, molecules are arranged into one-dimensional extended chains along the c axis and are further stacked along the a axis by directed four-membered O—H...O—H interactions, forming two-dimensional networks parallel to the ac plane. The short distances between the centroids of the benzene rings (3.8002–3.8327 Å indicate the existence of π–π interactions. In addition, the crystal structure is further stabilized by N—H...O, O—H...N (× 4, N—H...Cl and C—H...O (× 2 hydrogen-bonding interactions.

  15. Niveles de anticuerpos bactericidas frente a meningococo C tras la vacunación de niños de 2 a 6 años de edad en Andalucía

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    Delgado Torralbo Elena

    2000-01-01

    Full Text Available FUNDAMENTO: En 1997 el 18,5% de los casos de Enfermedad Meningocócica por serogrupo C en Andalucía fueron niños de 2 a 4 años de edad; edades donde respuesta inmune inicial y duración de la vacuna antimeningocócica de polisacárido capsular A+C, es menor que en edades superiores. Se diseñó una investigación para medir la respuesta inmune producida por esta vacuna, en niños de 2 a 6 años de edad, y compararla con la inmunidad natural presente en niños no vacunados. MÉTODOS: I.- Doble estudio de seguimiento: a grupos de niños previamente vacunados y grupos control, b grupo de niños que iba a ser vacunado, para análisis pre y postvacunal (1, 6 y 12 meses y grupo control. II.- La actividad bactericida se midió según protocolo estandarizado del CDC frente a cepa de N. meningítidis C-11. Los sueros con título de actividad bactericida (TAB > o = 1:8 se consideraron protectores. RESULTADOS: Al mes y a los 2 meses de vacunarse la proporción de TAB > o = 1:8 era significativamente superior a la del grupo control (65,5% y 73,9% frente a 2,2% y 12%. En el prevacunal y en el postvacunal a los 6, 7, 12 y 13 meses no se observó diferencia significativa entre vacunados y controles. CONCLUSIONES: Las diferencias entre vacunados y no vacunados 1 y 2 meses después de la vacunación indican seroconversión en los vacunados. Para el grupo de edad de 2 a 6 años la actividad bactericida adquirida declina rápidamente, ya que a los 6 meses dejan de observarse diferencias con el grupo control.

  16. Niveles de anticuerpos bactericidas frente a meningococo C tras la vacunación de niños de 2 a 6 años de edad en Andalucía

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    Elena Delgado Torralbo

    2000-01-01

    Full Text Available FUNDAMENTO: En 1997 el 18,5% de los casos de Enfermedad Meningocócica por serogrupo C en Andalucía fueron niños de 2 a 4 años de edad; edades donde respuesta inmune inicial y duración de la vacuna antimeningocócica de polisacárido capsular A+C, es menor que en edades superiores. Se diseñó una investigación para medir la respuesta inmune producida por esta vacuna, en niños de 2 a 6 años de edad, y compararla con la inmunidad natural presente en niños no vacunados. MÉTODOS: I.- Doble estudio de seguimiento: a grupos de niños previamente vacunados y grupos control, b grupo de niños que iba a ser vacunado, para análisis pre y postvacunal (1, 6 y 12 meses y grupo control. II.- La actividad bactericida se midió según protocolo estandarizado del CDC frente a cepa de N. meningítidis C-11. Los sueros con título de actividad bactericida (TAB ³ 1:8 se consideraron protectores. RESULTADOS: Al mes y a los 2 meses de vacunarse la proporción de TAB³ 1:8 era significativamente superior a la del grupo control (65,5% y 73,9% frente a 2,2% y 12%. En el prevacunal y en el postvacunal a los 6, 7, 12 y 13 meses no se observó diferencia significativa entre vacunados y controles. CONCLUSIONES: Las diferencias entre vacunados y no vacunados 1 y 2 meses después de la vacunación indican seroconversión en los vacunados. Para el grupo de edad de 2 a 6 años la actividad bactericida adquirida declina rápidamente, ya que a los 6 meses dejan de observarse diferencias con el grupo control.

  17. (3R,6S,7aS-3-Phenyl-6-(phenylsulfanylperhydropyrrolo[1,2-c]oxazol-5-one

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    Anthony D. Woolhouse

    2009-05-01

    Full Text Available Molecules of the title compound [systematic name: (2R,5S,7S-2-phenyl-7-phenylsulfanyl-1-aza-3-oxabicyclo[3.3.0]octan-8-one], C18H17NO2S, form high quality crystals even though they are only packed using C—H...O(carbonyl and weak C—H...S interactions. The dihedral angle between the aromatic rings is 85.53 (5°. The fused rings adopt envelope and twist conformations.

  18. HFE C282Y/H63D compound heterozygotes are at low risk of hemochromatosis-related morbidity.

    Science.gov (United States)

    Gurrin, Lyle C; Bertalli, Nadine A; Dalton, Gregory W; Osborne, Nicholas J; Constantine, Clare C; McLaren, Christine E; English, Dallas R; Gertig, Dorota M; Delatycki, Martin B; Nicoll, Amanda J; Southey, Melissa C; Hopper, John L; Giles, Graham G; Anderson, Gregory J; Olynyk, John K; Powell, Lawrie W; Allen, Katrina J

    2009-07-01

    The risk of hemochromatosis-related morbidity is unknown among HFE compound heterozygotes (C282Y/H63D). We used a prospective population-based cohort study to estimate the prevalence of elevated iron indices and hemochromatosis-related morbidity for compound heterozygotes. In all, 31,192 subjects of northern European descent were genotyped for HFE C282Y and H63D. An HFE-genotype stratified random sample of 1,438 subjects, followed for an average of 12 years to a mean age of 65 years, completed questionnaires and gave blood. Clinical examinations were blinded to HFE genotype. A total of 180 (84 males) clinically examined C282Y/H63D participants were compared with 330 (149 males) controls with neither HFE mutation; 132 (65 males) and 270 (122 males), respectively, had serum iron measures at both timepoints. Mean serum ferritin (SF) and transferrin saturation (TS) were significantly greater for male and female compound heterozygotes than for wild-types at baseline and follow-up (all P females who were premenopausal at baseline, where SF was similar in both genotype groups. For subjects with serum measures from both baseline and follow-up, mean SF and TS levels did not change significantly for men or for postmenopausal women, but for premenopausal women SF levels increased from 43 to 109 microg/L for compound heterozygotes and from 35 to 64 microg/L for wild-types (both P female compound heterozygotes had a similar prevalence of hemochromatosis-related morbidity to wild-types. One of 82 males and zero of 95 females had documented iron overload-related disease. For male compound heterozygotes, mean iron indices do not change during middle age but for female compound heterozygotes menopause results in increased mean SF. Although compound heterozygotes might maintain elevated iron indices during middle age, documented iron overload-related disease is rare.

  19. 4-[(3-Phenyl-4,5-dihydroisoxazol-5-ylmethyl]-2H-benzo[b][1,4]thiazin-3(4H-one

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    Nada Kheira Sebbar

    2016-06-01

    Full Text Available In the title compound, C18H16N2O2S, the 5-dihydroisoxazol-5-yl ring and its phenyl substituent are nearly coplanar, with the largest deviation from the mean plane being 0.0184 (16 Å. The thiomorpholin-3-one ring adopts a screw-boat conformation and the attached benzene ring makes a dihedral angle of 42.26 (7° with the mean plane through the 3-phenyl-4,5-dihydroisoxazol-5-yl ring system. In the crystal, molecules are linked by pairs of C—H...N hydrogen bonds, forming inversion dimers. These dimers are linked via C—H...O hydrogen bonds, generating a three-dimensional network.

  20. Ruthenium(II)-Catalyzed C-H Activation of Imidamides and Divergent Couplings with Diazo Compounds: Substrate-Controlled Synthesis of Indoles and 3H-Indoles.

    Science.gov (United States)

    Li, Yunyun; Qi, Zisong; Wang, He; Yang, Xifa; Li, Xingwei

    2016-09-19

    Indoles are an important structural motif that is commonly found in biologically active molecules. In this work, conditions for divergent couplings between imidamides and acceptor-acceptor diazo compounds were developed that afforded NH indoles and 3H-indoles under ruthenium catalysis. The coupling of α-diazoketoesters afforded NH indoles by cleavage of the C(N2 )-C(acyl) bond whereas α-diazomalonates gave 3H-indoles by C-N bond cleavage. This reaction constitutes the first intermolecular coupling of diazo substrates with arenes by ruthenium-catalyzed C-H activation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Bis(O-ethyl dithio-carbonato-κS,S')bis-(pyridine-3-carbonitrile-κN)nickel(II).

    Science.gov (United States)

    Kapoor, Sanjay; Kour, Ramandeep; Sachar, Renu; Kant, Rajni; Gupta, Vivek K; Kapoor, Kamini

    2012-01-01

    The Ni(2+) ion in the title complex, [Ni(C(3)H(5)OS(2))(2)(C(6)H(4)N(2))(2)], is in a strongly distorted octa-hedral coordination environment formed by an N(2)S(4) donor set, with the Ni(2+) ion located on a centre of inversion. In the crystal, weak C-H⋯S and C-H⋯N inter-actions are observed.

  2. Direct C-H alkylation and indole formation of anilines with diazo compounds under rhodium catalysis.

    Science.gov (United States)

    Mishra, Neeraj Kumar; Choi, Miji; Jo, Hyeim; Oh, Yongguk; Sharma, Satyasheel; Han, Sang Hoon; Jeong, Taejoo; Han, Sangil; Lee, Seok-Yong; Kim, In Su

    2015-12-18

    The rhodium(III)-catalyzed direct functionalization of aniline C-H bonds with α-diazo compounds is described. These transformations provide a facile construction of ortho-alkylated anilines with diazo malonates or highly substituted indoles with diazo acetoacetates.

  3. 10,21-Dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.18,12]tetracosa-1(23,2,6,8(24,9,11,13,17,19,21-decaene-23,24-diol cyclohexane 0.33-solvate

    Directory of Open Access Journals (Sweden)

    Sushil K. Gupta

    2011-10-01

    Full Text Available The title compound, C46H40N4O2·0.33C6H12, was obtained unintentionally as a product of an attempted synthesis of a cadmium(II complex of the [2,6-{PhSe(CH22N=CPh}2C6H2(4-Me(OH] ligand. The full tetraiminodiphenol macrocyclic ligand is generated by the application of an inversion centre. The macrocyclic ligand features strong intramolecular O—H...N hydrogen bonds. The dihedral angles formed between the phenyl ring incorporated within the macrocycle and the peripheral phenyl rings are 82.99 (8 and 88.20 (8°. The cyclohexane solvent molecule lies about a site of overline{3} symmetry. Other solvent within the lattice was disordered and was treated with the SQUEEZE routine [Spek (2009. Acta Cryst. D65, 148–155].

  4. 1-Methyl-5-nitro-3-phenyl-1H-indazole

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    Mohammed Naas

    2016-06-01

    Full Text Available The title compound, C14H11N3O2, crystallizes with two molecules in the asymmetric unit. The indazole ring system and the nitro group are nearly coplanar, with the largest deviations from the mean plane being 0.070 (4 Å in one molecule and 0.022 (3 Å in the second. The dihedral angle between the mean plane through the phenyl ring and the mean plane of the indazole ring system is of 23.24 (18° in the first molecule and 26.87 (18° in the second. In the crystal, molecules are linked by two C—H...O hydrogen bonds, forming linear zigzag tapes running along the c-axis direction, and by π–π stacking of molecules along the b axis, generating a three-dimensional structure.

  5. 1,4,9,12-Tetramethoxy-14-octyl-5,8-dihydrodiindolo[3,2-b;2′,3′-h]carbazole with an unknown solvent

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    Norma Wrobel

    2017-03-01

    Full Text Available The title compound, 2C36H39N3O4·H2O, is a linear π-conjugated ladder oligomer with an alkyl chain on the central nitrogen atom. This diindolocarbazole, prepared via a twofold Cadogan reaction, adopts a sligthly convex shape, anti to the disordered octyl group. The unit cell contains nine molecules of the title compound and half a water molecule per main molecule. The water molecule forms hydrogen bridges, connecting the carbazole-NH and methoxy groups of different molecules. The crystal contains solvent molecules which are located in a channel parallel to the c axis. It was not possible to determine the position and nature of the solvent (a mixure of choroform, n-pentane and DMSO. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option of PLATON was used to model the missing electron density. The given chemical formula and other crystal data do not take into account these solvent molecules.

  6. 1-[5-(2-Chlorophenyl-3-(4-methylphenyl-4,5-dihydro-1H-pyrazol-1-yl]ethan-1-one

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    Farook Adam

    2016-01-01

    Full Text Available The title compound, C18H17ClN2O, crystallized with two independent molecules (the S and R enantiomers in the asymmetric unit. The molecules are V-shaped with the two aromatic rings inclined to one another by 78.78 (11 and 81.23 (11°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming chains along the c-axis direction. The chains are linked via C—H...π interactions, forming a three-dimensional framework. The crystal structure was refined as a two-component twin.

  7. Crystallization and preliminary X-ray diffraction analysis of the C-terminal domain of the human spliceosomal DExD/H-box protein hPrp22

    International Nuclear Information System (INIS)

    Kudlinzki, Denis; Nagel, Christian; Ficner, Ralf

    2009-01-01

    The cloning, purification and crystallization of the C-terminal domain of human hPrp22 are reported. This communication also contains data for the preliminary X-ray diffraction analysis. The Homo sapiens DExD/H-box protein hPrp22 is a crucial component of the eukaryotic pre-mRNA splicing machinery. Within the splicing cycle, it is involved in the ligation of exons and generation of the lariat and it additionally catalyzes the release of mature mRNA from the spliceosomal U5 snRNP. The yeast homologue of this protein, yPrp22, shows ATP-dependent RNA-helicase activity and is capable of unwinding RNA/RNA duplex molecules. A truncated construct coding for residues 950–1183 of human Prp22, comprising the structurally and functionally uncharacterized C-terminal domain, was cloned into an Escherichia coli expression vector. The protein was subsequently overproduced, purified and crystallized. The crystals obtained diffracted to 2.1 Å resolution, belonged to the tetragonal space group P4 1 2 1 2 or P4 3 2 1 2, with unit-cell parameters a = b = 78.2, c = 88.4 Å, and contained one molecule in the asymmetric unit

  8. rac-2-(2-Amino-4-oxo-4,5-dihydro-1,3-thiazol-5-yl-2-hydroxyindane-1,3-dione

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    Narsimha Reddy Penthala

    2009-08-01

    Full Text Available In the crystal of the title compound, C12H8N2O4S, molecules are linked into chains by a series of intermolecular O—H...O, N—H...O and N—H...N hydrogen bonds. The ninhydrin and aminothiazolidine units make a dihedral angle of 66.41 (3°. The crystal structure indicates the presence of equimolar R and S enantiomers in the crystal lattice, due to the presence of a chiral centre in the title compound.

  9. Stereochemistry of C18 monounsaturated cork suberin acids determined by spectroscopic techniques including (1) H-NMR multiplet analysis of olefinic protons.

    Science.gov (United States)

    Santos, Sara; Graça, José

    2014-01-01

    Suberin is a biopolyester responsible for the protection of secondary plant tissues, and yet its molecular structure remains unknown. The C18:1 ω-hydroxyacid and the C18:1 α,ω-diacid are major monomers in the suberin structure, but the configuration of the double bond remains to be elucidated. To unequivocally define the configuration of the C18:1 suberin acids. Pure C18:1 ω-hydroxyacid and C18:1 α,ω-diacid, isolated from cork suberin, and two structurally very close C18:1 model compounds of known stereochemistry, methyl oleate and methyl elaidate, were analysed by NMR spectroscopy, Fourier transform infrared (FTIR) and Raman spectroscopy, and GC-MS. The GC-MS analysis showed that both acids were present in cork suberin as only one geometric isomer. The analysis of dimethyloxazoline (DMOX) and picolinyl derivatives proved the double bond position to be at C-9. The FTIR spectra were concordant with a cis-configuration for both suberin acids, but their unambiguous stereochemical assignment came from the NMR analysis: (i) the chemical shifts of the allylic (13) C carbons were shielded comparatively to the trans model compound, and (ii) the complex multiplets of the olefinic protons could be simulated only with (3) JHH and long-range (4) JHH coupling constants typical of a cis geometry. The two C18:1 suberin acids in cork are (Z)-18-hydroxyoctadec-9-enoic acid and (Z)-octadec-9-enedoic acid. Copyright © 2013 John Wiley & Sons, Ltd.

  10. 13b,13c-Di-2-pyridyl-5,7,12,13b,13c,14-hexahydro-6H,13H-5a,6a,12a,13a-tetraazabenz[5,6]azuleno[2,1,8-ija]benz[f]azulene-6,13-dione methanol hemisolvate

    Directory of Open Access Journals (Sweden)

    Lin Li

    2008-01-01

    Full Text Available The title compound, C30H24N6O2·0.5CH3OH, a glycoluril derivative with two pyridine substituents on the convex face of the glycoluril system, is an important intermediate for the synthesis of more complex glycoluril derivatives. The compound crystallizes with two independent molecules in the asymmetric unit, one of which exhibits disorder of one benzene ring over two orientations with refined site occupancy factors 0.65 (4:0.35 (4. The crystal structure contains several short C—H...O contacts, and the methanol molecule forms an O—H...O hydrogen bond to one of the glycoluril molecules.

  11. 2-Oxo-2H-chromen-3-yl 4-tert-butylbenzoate

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    Konan René Kambo

    2016-10-01

    Full Text Available In the title coumarin derivative, C20H18O4, the benzene ring of the benzoate group is oriented at a dihedral angle of 57.55 (9° with respect to the planar chromene ring system [maximum deviation from plane is 0.027 (2 Å]. In the crystal, inversion-related molecules are linked into dimers via C—H...O hydrogen bonds, generating R22(12 loops. The dimers are linked by further C—H...O hydrogen bonds forming layers, parallel to the bc plane, which are linked via C—H...π interactions, forming a three-dimensional framework

  12. Electronic structures of three semiconducting intermetallics: RuAl sub 2 , RuGa sub 2 and OsAl sub 2

    CERN Document Server

    Springborg, M

    1998-01-01

    Results of first-principles, density-functional, LMTO-ASA calculations on the closely related C11, C40, and C54 structures of the three title compounds are reported. Only for OsAl sub 2 in the C11 structure were the structural degrees of freedom optimized; this gave results in good agreement with experimental values. On the other hand, the calculations were not capable of reproducing the correct relative stability of the different structures; this was ascribed to the atomic-sphere approximation. All of the compounds were found to be small-gap semiconductors with, however, a slightly larger gap for OsAl sub 2. The occurrence of a gap at the Fermi level is mainly due to hybridization between d functions of Os or Ru and p functions of Al or Ga, but, in particular for OsAl sub 2 , charge-transfer effects can also be considered to be responsible for the occurrence of a gap. Several flat bands just above the Fermi level lead to a corresponding high density of states there, but also to low carrier velocities. As a b...

  13. Improved modification for the density-functional theory calculation of thermodynamic properties for C-H-O composite compounds.

    Science.gov (United States)

    Liu, Min Hsien; Chen, Cheng; Hong, Yaw Shun

    2005-02-08

    A three-parametric modification equation and the least-squares approach are adopted to calibrating hybrid density-functional theory energies of C(1)-C(10) straight-chain aldehydes, alcohols, and alkoxides to accurate enthalpies of formation DeltaH(f) and Gibbs free energies of formation DeltaG(f), respectively. All calculated energies of the C-H-O composite compounds were obtained based on B3LYP6-311++G(3df,2pd) single-point energies and the related thermal corrections of B3LYP6-31G(d,p) optimized geometries. This investigation revealed that all compounds had 0.05% average absolute relative error (ARE) for the atomization energies, with mean value of absolute error (MAE) of just 2.1 kJ/mol (0.5 kcal/mol) for the DeltaH(f) and 2.4 kJ/mol (0.6 kcal/mol) for the DeltaG(f) of formation.

  14. Dichloridobis[1-(2,4,6-trimethylphenyl-1H-imidazole-κN3]copper(II

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    Yantao Zhang

    2013-11-01

    Full Text Available In the title complex, [CuCl2(C12H14N22], the Cu2+ cation is situated on an inversion centre and is coordinated by two N atoms from symmetry-related 1-mesityl-1H-imidazole ligands and by two chloride anions in a slightly distorted square-planar geometry. In the organic ligand, the dihedral angle between the benzene ring of the mesityl moiety and the imidazole ring is 76.99 (18°. Weak intramolecular C—H...Cl hydrogen-bonding interactions consolidate the molecular conformation.

  15. Solvent-Mediated Synthesis of M(II-Coordination Polymer Part 1: Crystal Structure of Poly(1,2-di(4-pyridylethylene-k2N,N'-bis(1,4-benzenediacetato-k4O,O′,O′′,O′′'zinc(II], C22H18ZnN2O4

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    Stephen Adie Adalikwu

    2017-08-01

    Full Text Available An interaction of water-methanol solution of sodium1,4-benzenediacetate (bda and 4,4′-bipyridylethelene (bpee with aqueous solution of Zn(NO32·6H2O at room temperature yielded colourless crystals of 1 after three weeks in a sealed glass tube. The compound with composition C22H18ZnN2O4 crystallizes in monoclinic space group P21/c, with the following cell dimensions: a = 10.4566(2, b = 13.3085(2, c = 13.7189(2 Å, β = 101.491(1°. In the structure of 1, two Zn(II neighbours are connected by two bda ligands adopting chelating and bidentate-bridging coordination modes to form a dimeric unit (Zn2O8N4 with the Zn–Zn distance of 4.0432(6 Å. The carboxyl-bridged dimeric units are extended along the [001] direction by bpee co-ligands and further linked by bda ligand to form a three-dimensional network structure. The IR shows the characteristic bands of the carboxylates at 1611/1507 cm−1 and 1424/1373 cm−1, respectively, for asymmetric and symmetric stretching −CO2− vibrations. The separation ∆[νasym(CO2− − νsym(CO2−] values of 187 and 134 cm−1 are indicative of chelating and bidentate bridging coordination modes of the carboxylate to the metal centre.

  16. Bis(1-benzyl-1H-benzimidazole-κN3dichloridozinc

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    Rachid Bouhfid

    2014-03-01

    Full Text Available In the title compound, [ZnCl2(C14H12N22], the ZnII atom exhibits a distorted tetrahedral coordination geometry involving two chloride anions and two N-atom donors from 1-benzyl-1H-benzimidazole ligands. In both ligands, the benzyl and benzimidazole rings are nearly perpendicular [dihedral angles = 81.7 (2 and 81.5 (2°]. The two benzimidazole systems are essentially planar [maximum deviations = 0.015 (3 and 0.020 (2 Å] and form a dihedral angle of 78.09 (8°. In the crystal, centrosymmetrically related molecules are linked by pairs of C—H...Cl hydrogen bonds into chains parallel to the a axis.

  17. (E-4-(2,5-Dimethoxybenzylidene-2-phenyl-1,3-oxazol-5(4H-one

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    Abdullah Mohamed Asiri

    2009-08-01

    Full Text Available The central azalactone ring in the title compound, C18H15NO4, is planar (r.m.s. deviation 0.05, 0.12 Å in both independent molecules comprising the asymmetric unit. The benzylidene substituent is coplanar with this ring [dihedral angle between the planes = 1.8 (1° in the first molecule and 2.8 (1° in the second], as is the phenyl substitutent [dihedral angle between rings = 4.6 (1 and 9.7 (1°, respectively].

  18. Ethyl 1-oxo-1,2,3,4-tetrahydro-9H-carbazole-3-carboxylate

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    Tuncer Hökelek

    2009-07-01

    Full Text Available The title compound, C15H15NO3, contains a carbazole skeleton with an ethoxycarbonyl group at the 3 position. In the indole ring system, the benzene and pyrrole rings are nearly coplanar, forming a dihedral angle of 1.95 (8°. The cyclohexenone ring has an envelope conformation. In the crystal structure, pairs of strong N—H...O hydrogen bonds link the molecules into centrosymmetric dimers with R22(10 ring motifs. π–π contacts between parallel pyrrole rings [centroid–centroid distance = 3.776 (2 Å] may further stabilize the structure. A weak C—H...π interaction is also observed.

  19. Trimethyl 3,3′,3′′-(benzene-1,3,5-triyltripropynoate

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    Felix Katzsch

    2016-04-01

    Full Text Available In the title compound, C18H12O6, the alkyne bonds are distorted, featuring bond angles around the C—C[triple-bond]C—C group of 173.6 (1/179.0 (1, 178.1 (1/178.4 (1 and 174.9 (1/175.9 (1°, and the ester groups make angles of 3.5 (1, 13.8 (1 and 14.5 (1° with the central benzene ring. In the crystal, molecules are connected in layers parallel to (131 by weak C—H...O hydrogen bonds, giving rise to a system of hydrogen-bonded ring motifs with graph sets R22(14 and R44(22. The layers are linked by C—H...O and C—H...π contacts.

  20. (4′-Phenyl-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′bis(thiocyanato-κNzinc(II unknown solvate

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    An-ran Wang

    2016-11-01

    Full Text Available The title compound, [Zn(NCS2(C21H15N3], crystallizes with three independent complex molecules in the asymmetric unit. In each complex molecule, the ZnII atom is coordinated by three N atoms of a 4′-phenyl-2,2′:6′,2′′-terpyridine ligand, and by the N atoms of two NCS− anions. The ZnII atoms are therefore five-coordinate, ZnN5, with distorted square-pyramidal geometries. In the crystal, the three independent molecules are linked by a series of offset π–π interactions [intercentroid distances vary between 3.680 (5 and 3.791 (5 Å], forming columns along the a-axis direction. The columns are linked via C—H...S interactions, forming a fence-like arrangement parallel to the ab plane. A small region of disordered electron density was corrected for using the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18], but the formula mass and unit-cell characteristics were not taken into account during the refinement.

  1. Ethyl 5-cyano-4-[2-(2,4-dichlorophenoxyacetamido]-1-phenyl-1H-pyrrole-3-carboxylate

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    Jing Xu

    2009-08-01

    Full Text Available In the title compound, C22H17Cl2N3O4, the pyrrole ring and the 2,4-dichlorophenyl group form a dihedral angle of 8.14 (13°; the phenyl ring is twisted with respect to the pyrrole ring, forming a dihedral angle of 60.77 (14°. The C=O bond length is 1.213 (3 Å, indicating that the molecule is in the keto form, associated with a –CONH– group, and the amide group adopts the usual trans conformation. The molecule is stabilized by an intramolecular N—H...O hydrogen-bonding interaction. In the crystal, the stacked molecules exhibit intermolecular C—H...O and C—H...N hydrogen-bonding interactions.

  2. Dichloridobis(4-methyl-3,5-diphenyl-1H-pyrazole-κN2copper(II

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    Moayad Hossaini Sadr

    2011-12-01

    Full Text Available The asymmetric unit of the title compound, [CuCl2(C16H14N22], comprises half of the complex. The CuII atom lies on a crystallographic twofold rotation axis and shows a significantly distorted tetrahedral coordination geometry. The dihedral angle between the phenyl rings is 74.3 (2°. The crystal structure is stabilized by intermolecular π–π interactions [centroid–centroid distances = 3.635 (2–3.803 (3 Å].

  3. Are Shorter Article Titles More Attractive for Citations? Cross-sectional Study of 22 Scientific Journals

    Science.gov (United States)

    Habibzadeh, Farrokh; Yadollahie, Mahboobeh

    2010-01-01

    Aim To investigate the correlation between the length of the title of a scientific article and the number of citations it receives, in view of the common editorial call for shorter titles. Methods Title and the number of citations to all articles published in 2005 in 22 arbitrarily chosen English-language journals (n = 9031) were retrieved from citation database Scopus. The 2008 journal impact factors of these 22 journals were also retrieved from Thomson Reuters’ Journal Citation Report (JCR). Assuming the article title length as the independent variable, and the number of citations to the article as the dependent variable, a linear regression model was applied. Results The slope of the regression line for some journals (n = 6, when titles were measured in characters but 7 when titles were measured in words) was negative – none was significantly different from 0. The overall slope for all journals was 0.140 (when titles were measured in characters) and 0.778 (when titles were measured in words), significantly different from 0 (P articles with longer titles received more citations – Spearman ρ = 0.266 – when titles were measured in characters, and ρ = 0.244 when titles were measured in words (P 10 and for 2 out of 14 journals with impact factor <10 (P < 0.001, Fisher exact test). Conclusion Longer titles seem to be associated with higher citation rates. This association is more pronounced for journals with high impact factors. Editors who insist on brief and concise titles should perhaps update the guidelines for authors of their journals and have more flexibility regarding the length of the title. PMID:20401960

  4. N-(Thiazol-2-ylacetamide

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    Uzma Yunus

    2008-08-01

    Full Text Available The title compound, C5H6N2OS, was synthesized from acetyl chloride and 2-aminothiazole in dry acetone. The asymmetric unit contains two molecules. The crystal structure is stabilized by N—H...N and C—H...O hydrogen bonds.

  5. (Z-N-[3-(4-Bromobenzoyl-1,3-thiazolidin-2-ylidene]cyanamide

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    Ling Xu

    2010-12-01

    Full Text Available In the title compound, C11H8BrN3OS, the dihedral angle between the benzene and thiazolidine rings is 63.4 (2°. Intermolecular C—H...N interactions help to stabilize the crystal structure.

  6. 3′,6′-Bis(diethylamino-3H-spiro[2-benzothiophene-1,9′-xanthene]-3-thione

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    Bing-Yuan Su

    2008-11-01

    Full Text Available The title compound, C28H30N2OS2, was obtained by thionation of 3′,6′-bis(diethylamino-3H-spiro[isobenzofuran-1,9′-xanthene]-3-one with 2,4-bis(p-methoxyphenyl-1,3-dithiadiphosphetane disulfide (Lawesson's reagent. The planes of the two benzene rings of the xanthene system are inclined at a dihedral angle of 17.4 (1°, and the plane of the dithiophthalide group and the planes through the two benzene rings of the xanthene system make dihedral angles of 80.2 (1 and 82.8 (1°, respectively.

  7. 2-(6-Bromobenzo[d]thiazol-2-yl-5,5-dimethylthiazol-4(5H-one

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    Rainer Beckert

    2013-12-01

    Full Text Available The title compound, C12H9BrN2OS2, was obtained by reacting 6-bromobenzo[d]thiazole-2-carbonitrile in iso-propanol with ethyl 2-mercapto-2-methylpropanoate at reflux temperature for several hours. The resulting dimethyloxyluciferin derivative shows partial double-bond character of the carbon–carbon bond between the two heterocyclic moieties [C—C = 1.461 (3 Å]. This double bond restricts rotation around this C—C axis, therefore leading to an almost planar molecular structure [N—C—C—S torsion angle = 9.7 (3°]. The five-membered thiazoline ring is not completely planar as a result of the bulky S atom [C—S—C—C torsion angle = 5.17 (12°].

  8. 4-((E-{2-[N-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylcarboximidoyl]benzylidene}amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

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    Richard Betz

    2011-10-01

    Full Text Available The title compound, C30H28N6O2, is a symmetric diimine derived from ortho-dibenzaldehyde. Both C=N bonds are (E-configured. The terminal N-bonded phenyl groups adopt staggered conformations relative to their respective parent heterocycles, the relevant least-squares planes intersect at angles of 32.35 (11 and 38.59 (10°. In the crystal, C—H...O contacts connect the molecules into chains along the b axis and give rise to a C11(14C11(14 and a R22(12 pattern on different levels of graph-set analysis. The shortest intercentroid distance between two centroids was found at 4.2074 (11 Å between the two five-membered heterocycles.

  9. Selective incorporation of various C-22 polyunsaturated fatty acids in Ehrlich ascites tumor cells

    International Nuclear Information System (INIS)

    Masuzawa, Y.; Okano, S.; Waku, K.; Sprecher, H.; Lands, W.E.

    1986-01-01

    Three 14 C-labeled 22-carbon polyunsaturated fatty acids, 7,10,13,16-[ 14 C]docosatetraenoic acid (22:4(n-6)), 7,10,13,16,19-[ 14 C]docosapentaenoic acid (22:5(n-3)), and 4,7,10,13,16,19-[ 14 C]docosahexaenoic acid (22:6(n-3)), were compared with [ 3 H]arachidonic acid (20:4(n-6] and [14C]linoleic acid (18:2(n-6)) to characterize their incorporation into the lipids of Ehrlich ascites cells. The relatively rapid incorporation of the labeled 22-carbon acids into phosphatidic acid indicated that substantial amounts of these acids may be incorporated through the de novo pathway of phospholipid synthesis. In marked contrast to 20:4(n-6), the 22-carbon acids were incorporated much less into choline glycerophospholipids (CGP) and inositol glycerophospholipids (IGP). No selective preference was apparent for the (n-3) or (n-6) type of fatty acids. The amounts of the acids incorporated into diacylglycerophosphoethanolamine were in the order of: 22:6(n-3) greater than 20:4(n-6) much greater than 22:5(n-3) greater than or equal to 22:4(n-6) greater than 18:2(n-6), whereas for alkylacylglycerophosphoethanolamine they were in the order of: 22:4(n-6) greater than 22:6(n-3) greater than 22:5(n-3) much greater than 20:4(n-6) greater than 18:2(n-6). Of the mechanisms possibly responsible for the selective entry of 22-carbon acids into ethanolamine glycerophospholipids, the most reasonable explanation was that the cytidine-mediated ethanolamine phosphotransferase may have a unique double selectivity: for hexaenoic species of diacylglycerol and for 22-carbon polyunsaturated fatty acid-containing species of alkylacylglycerol. The relative distribution of fatty acids between newly incorporated and already maintained lipid classes suggested that IGP may function in Ehrlich cells as an intermediate pool for the retention of polyunsaturated fatty acids in glycerolipids

  10. Ethyl 2-(3,4-dimethyl-5,5-dioxo-1H,4H-benzo[e]pyrazolo[4,3-c][1,2]thiazin-1-ylacetate

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    Sana Aslam

    2012-10-01

    Full Text Available In the title molecule, C15H17N3O4S, the heterocyclic thiazine ring adopts a twist-boat conformation, which differs from that in related compounds, with adjacent S and C atoms displaced by 0.981 (4 and 0.413 (5 Å, respectively, on the same side of the mean plane formed by the remaining ring atoms. The mean plane of the benzene ring makes a dihedral angle of 23.43 (14° with the mean plane of the pyrazole ring. In the crystal, molecules are connected by weak C—H...O hydrogen bonds to form a three-dimensional network. The H atoms of the methyl group attached to the pyrazole ring were refined over six sites with equal occupancies.

  11. 2,2′-[(3aRS,7aRS-Perhydrobenzimidazole-1,3-diylbis(methylene]diphenol

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    Augusto Rivera

    2010-04-01

    Full Text Available The molecular structure of the title compound, C21H26N2O2, shows two intramolecular O—H...N hydrogen-bonding interactions. In the crystal structure, molecular chains are formed along the c axis through weak C—H...O interactions. Neighbouring chains are weakly associated along the a axis via C—H...π interactions.

  12. 2,6-Bis(9-ethyl-9H-carbazolylmethylenecyclohexanone

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    Abdullah M. Asiri

    2009-10-01

    Full Text Available The title compound, 2,6-bis(ethyl-9-ethyl-9H-carbazolylmethylenecyclohexanone has been synthesized by condensation of 9-ethylcarbazole-3-aldehyde and cyclohexanone in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H NMR, 13C NMR and EI-MS spectral analysis.

  13. (2,3,7,8,12,13,17,18-Octaethylporphyrinato-κ4Ncobalt(II–2-nitrobenzaldehyde (1/2

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    Anissa Mansour

    2012-09-01

    Full Text Available The asymmetric unit of the title compound, [Co(C36H44N4]·2C7H5NO3, is composed of one half of the complex, arranged about an inversion center, and a complete 2-nitrobenzaldehyde (NBA molecule. The structure consists of columns that contain interleaved molecules of NBA and [CoII(OEP] (OEP is 2,3,7,8,12,13,17,18-octaethylporphyrin, which are stacked along the a axis. The CoII atom is involved in a π interaction with the ring of the NBA molecule with a centroid–metal distance of 3.508 (6 Å. There is an intramolecular C—H...O hydrogen bond in the NBA molecule.

  14. A new solid solution compound with the Sr{sub 21}Mn{sub 4}Sb{sub 18} structure type. Sr{sub 13}Eu{sub 8}Cd{sub 3}Mn{sub 1}Sb{sub 18}

    Energy Technology Data Exchange (ETDEWEB)

    Kunz Wille, Elizabeth L.; Cooley, Joya A.; Fettinger, James C.; Kazem, Nasrin; Kauzlarich, Susan M. [California Univ., Davis, CA (United States). Dept. of Chemistry

    2017-09-01

    The title compound with the nominal formula, Sr{sub 13}Eu{sub 8}Cd{sub 3}Mn{sub 1}Sb{sub 18}, was synthesized by Sn-flux. Structure refinement was based on single-crystal X-ray diffractometer data. Employing the exact composition, the formula is Sr{sub 13.23}Eu{sub 7.77}Cd{sub 3.12}Mn{sub 0.88}Sb{sub 18} for the solid solution Sr{sub 21-x}Eu{sub x}Cd{sub 4-y}Mn{sub y}Sb{sub 18}. This phase adopts the Sr{sub 21}Mn{sub 4}Sb{sub 18} type structure with site preferences for both Eu and Cd. The structure crystallizes in the monoclinic system in space group C2/m and Z=4: a=18.1522(11), b=17.3096(10), c=17.7691(10) Aa, β=91.9638(8) , 6632 F{sup 2} values, 216 variables, R1=0.0254 and wR2=0.0563. Site selectivity of the elements in this new compound will be discussed in relationship with the Sr{sub 21}Mn{sub 4}Sb{sub 18} type structure and other related structure types. Temperature dependent magnetic susceptibility data reveal Curie-Weiss paramagnetism with an experimental moment of 19.3 μ{sub B}/f.u. and a Weiss constant of 0.4 K. Magnetic ordering is seen at low temperatures, with a transition temperature of 3.5 K.

  15. Bis(2,2′-bipyridine-κ2N,N′(3-methylbenzoato-κ2O,O′zinc 3-methylbenzoate–3-methylbenzoic acid–water (1/1/2

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    Qiu-qi Ye

    2012-09-01

    Full Text Available The title compound, [Zn(C8H7O2(C10H8N22](C8H7O2·C8H8O2·2H2O, is comprised of a Zn2+ cation, two 2,2′-bipydine (bipy ligands and one 3-methylbenzoate anion (L− together with one uncoordinating L− anion, one uncoordinating HL molecule and two lattice water molecules. The ZnII atom is coordinated by four N atoms of two bipy ligands and two O atoms from one L− ligand in a distorted octahedral geometry. Pairs of centrosymmetrically related complex molecules form dimers via slipped π-stacking interactions between bipy ligands with an interplanar distance of 3.470 (4 Å. The dimers are linked into supramolecular chains along [111], via C—H...O hydrogen bonds. The uncoordinated L− anions, HL molecules and water molecules are connected with each other via O—H...O hydrogen bonds, forming chains between the metal complex chains and binding them together via C—H...O contacts. The resulting layers parallel to (010 are further assembled into a three-dimensional supramolecular architecture through additional C—H...O interactions.

  16. Disease: H00865 [KEGG MEDICUS

    Lifescience Database Archive (English)

    Full Text Available H00865 Lethal congenital contractural syndrome (LCCS) Lethal congenital contractur...al syndrome (LCCS) is a heterogeneous group of disorders characterized by congenital nonprogressive joint contract...rk OS ... TITLE ... Lethal contractural syndrome type 3 (LCCS3) is caused by a mutation in PIP5K1C, which enco

  17. (E-4-Hydroxy-6-methyl-3-[1-(2-phenylhydrazinylideneethyl]-2H-pyran-2-one

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    Samra Rahmouni

    2016-05-01

    Full Text Available The title compound, C14H14N2O3, crystallized with three crystallographically independent molecules (A, B and C in the asymmetric unit. The three molecules each have an E conformation about the C=N bond but differ in the orientation of the phenyl and pyran rings. The dihedral angles between the phenyl and pyran ring planes are 14.30 (1, 28.38 (1 and 25.58 (1° in molecules A, B and C, respectively. There is an intramolecular O—H...N hydrogen bond in each molecule with an S(6 ring motif. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds, forming layers parallel to (001, enclosing R22(8 and R33(21 ring motifs. The layers are linked via C—H...π interactions, forming bilayers, which are joined by a further C—H...π interaction, forming a three-dimensional structure.

  18. Vitamin D3 analog maxacalcitol (OCT) induces hCAP-18/LL-37 production in human oral epithelial cells.

    Science.gov (United States)

    Tada, Hiroyuki; Shimizu, Takamitsu; Nagaoka, Isao; Takada, Haruhiko

    2016-01-01

    Maxacalcitol (22-oxacalcitriol: OCT) is a synthetic vitamin D3 analog with a limited calcemic effect. In this study, we investigated whether OCT increases the production of LL-37/CAP-18, a human cathelicidin antimicrobial peptide, in human gingival/oral epithelial cells. A human gingival epithelial cell line (Ca9-22) and human oral epithelial cell lines (HSC-2, HSC-3, and HSC-4) exhibited the enhanced expression of LL-37 mRNA upon stimulation with OCT as well as active metabolites of vitamins D3 and D2. Among the human epithelial cell lines, Ca9-22 exhibited the strongest response to these vitamin D-related compounds. OCT induced the higher production of CAP-18 (ng/mL order) until 6 days time-dependently in Ca9-22 cells in culture. The periodontal pathogen Porphyromonas gingivalis was killed by treatment with the LL-37 peptide. These findings suggest that OCT induces the production of hCAP-18/LL-37 in a manner similar to that induced by the active metabolite of vitamin D3.

  19. Orthorhombic polymorph of 4-[(1H-benzimidazol-1-ylmethyl]benzoic acid

    Directory of Open Access Journals (Sweden)

    Hai-Wei Kuai

    2011-11-01

    Full Text Available We reported recently the first polymorph of the title compound [Kuai & Cheng (2011a. Acta Cryst., E67, o2787]. A second polymorph of the title compound, C15H12N2O2, was unexpectedly obtained by the hydrothermal reaction of the title compound with manganese chloride in the presence of potassium hydroxide at 413 K. The benzimidazole ring system is almost planar, with a maximum deviation from the mean plane of 0.015 (2 Å. The benzimidazole and benzene rings are inclined at a dihedral angle of 79.00 (1°. In the crystal, adjacent molecules are connected through O—H...N hydrogen bonds into a one-dimensional chain along the [001] direction.

  20. 9-Ethyl-2,3-dihydro-9H-carbazol-4(1H-one

    Directory of Open Access Journals (Sweden)

    S. Sriman Narayanan

    2008-09-01

    Full Text Available In the title compound, C28H30N2O2, the cyclohexene ring system adopts a sofa conformation. The crystal structure is stabilized by C—H...O interactions between methyl H atoms of the ethyl substituents and the O atoms of carbonyl groups of adjacent molecules, and by an intermolecular carbonyl–carbonyl interactions [3.207 (2 Å

  1. Lattice potential energy and standard molar enthalpy in the formation of 1-dodecylamine hydrobromide(1-C12H25NH3·Br)(s)

    Institute of Scientific and Technical Information of China (English)

    Liu Yu-Pu; Di You-Ying; Dan Wen-Yan; He Dong-Hua; Kong Yu-Xia; Yang Wei-Wei

    2011-01-01

    This paper reports that 1-dodecylamine hydrobromide (1-C12H25NH3·Br)(s) has been synthesized using the liquid phase reaction method. The lattice potential energy of the compound 1-C12H25NH3·Br and the ionic volume and radius of the 1-C12H25NH3+ cation are obtained from the crystallographic data and other auxiliary ther-modynamic data. The constant-volume energy of combustion of 1-C12H25NH3·Br(s) is measured to be △cUm°(1-C12H25NH3·Br, s) =-(7369.03±3.28) kJ·mol-1 by means of an RBC-Ⅱ precision rotating-bomb combustion calorimeter at T=(298.15±0.001) K. The standard molar enthalpy of combustion of the compound is derived to be △cHm°(1-C12H25NH3·Br, s)=-(7384.52±3.28) kJ·mol-1 from the constant-volume energy of combustion. The standard molar enthalpy of formation of the compound is calculated to be △fHm°(1-C12H25NH3·Br, s)=-(1317.86±3.67) kJ·mol-1 from the standard molar enthalpy of combustion of the title compound and other auxiliary thermodynamic quantities through a thermochemical cycle.

  2. Crystal structures of 2-[(4,6-diaminopyrimidin-2-ylsulfanyl]-N-(naphthalen-1-ylacetamide and 2-[(4,6-diaminopyrimidin-2-ylsulfanyl]-N-(4-fluorophenylacetamide

    Directory of Open Access Journals (Sweden)

    S. Subasri

    2017-02-01

    Full Text Available The title compounds, C16H15N5OS, (I, and C12H12FN5OS, (II, are [(diaminopyrimidinesulfanyl]acetamide derivatives. In (I, the pyrimidine ring is inclined to the naphthalene ring system by 55.5 (1°, while in (II, the pyrimidine ring is inclined to the benzene ring by 58.93 (8°. In (II, there is an intramolecular N—H...N hydrogen bond and a short C—H...O contact. In the crystals of (I and (II, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with R22(8 ring motifs. In the crystal of (I, the dimers are linked by bifurcated N—H...(O,O and C—H...O hydrogen bonds, forming layers parallel to (100. In the crystal of (II, the dimers are linked by N—H...O hydrogen bonds, also forming layers parallel to (100. The layers are linked by C—H...F hydrogen bonds, forming a three-dimensional architecture.

  3. Synthesis of 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2-14C and N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-YL-2-14C)acetamide

    International Nuclear Information System (INIS)

    Fong, M.T.; Leaffer, M.A.

    1986-01-01

    We have prepared the 14 C-labeled analogs of NSC 261036, 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2- 14 C, and NSC 301467, N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-yl-2- 14 C) acetamide, for pharmacological, drug distribution, and mechanisms of action studies. The latter is an analog designed for lower toxicity and improved properties. The former is a metabolite of, and appears to be less toxic than, misonidazole. (author)

  4. Bis(2,2′-bipyridine[1,9-bis(diphenylphosphanyl-1,2,3,4,6,7,8,9-octahydropyrimido[1,2-a]pyrimidin-5-ium]ruthenium(II hexafluoridophosphate dibromide dichloromethane disolvate monohydrate

    Directory of Open Access Journals (Sweden)

    Alain Igau

    2013-12-01

    Full Text Available In the cation of the title complex, [Ru(C31H32N3P2(C10H8N22](PF6(Br2·2CH2Cl2·H2O, the ruthenium ion is coordinated in a distorted octahedral geometry by two 2,2′-bipyridine (bpy ligands and a chelating cationic N-diphenylphosphino-1,3,4,6,7,8-hexahydro-2-pyrimido[1,2-a]pyrimidine [(PPh22-hpp] ligand. The tricationic charge of the complex is balanced by two bromide and one hexafluoridophosphate counter-anions. The compound crystallized with two molecules of dichloromethane (one of which is equally disordered about a Cl atom and a water molecule. In the crystal, one of the Br anions bridges two water molecules via O—H...Br hydrogen bonds, forming a centrosymmetric diamond-shaped R42(8 motif. The cation and anions and the solvent molecules are linked via C—H...F, C—H...Br, C—H...Cl and C—H...O hydrogen bonds, forming a three-dimensional network.

  5. 10-[1,1-Dichloro-4-(trimethylsilylbut-1-en-3-yn-2-yl]-10H-phenothiazine

    Directory of Open Access Journals (Sweden)

    Satoru Umezono

    2018-02-01

    Full Text Available The title compound, C19H17Cl2NSSi, is an enamine derivative, in which the N atom adopts a shallow trigonal–pyramidal geometry [displacement from the plane of its attached C atoms = 0.1383 (18 Å]. The dihedral angle between the plane through the three amino carbon atoms and the vinyl group is 89.47 (7°. The phenothiazine unit has a butterfly structure and the central six-membered ring adopts a boat conformation. The fold angle between the benzene rings is 28.52 (7°. The crystal structure features weak Csp3—H...Cl hydrogen bonds, H...S contacts and π–π stacking interactions between phenothiazine units.

  6. Study of alkylphenols, indol and pyridinic nucleus of HPAN compounds by SPE/SI and SPE/C{sub 18}/NEC: application of SPE/Si phase to oils from the Alagoas sub-basin

    Energy Technology Data Exchange (ETDEWEB)

    Reboucas, L.M.C.; Nogueira, F.A.R.; Sabino, A.R.; Araujo, O.R.P.; Sant' Ana, A.E.G. [Universidade Federal de Alagoas (LABIS/UFAL), Maceio, AL (Brazil). Inst. de Quimica e Biotecnologia. Lab. de Analise de Biomarcadores e Semioquimicos], E-mail: lmcr@qui.ufal.br

    2008-10-15

    Alkylphenols (AP) and hydrocarbon polycyclic aromatic nitrogen (HPAN) compounds are important to study secondary migrations of petroleum. The behavior of AP and HPAN standards was investigated by solid phase extraction (SPE) on silica gel (SPE/Si) and C{sub 18}/NEC (SPE/C{sub 18}) stationary phases. The AP standards were eluted with dichloromethane (DCM) in the F2 fraction, on both SPE/Si and SPE/C{sub 18} phases. The basic and neutral HPAN compounds were eluted together with DCM, in F2 fraction, when a SPE/C18 column was used. However in the SPE/Si column the HPAN compounds were separated by their basic and neutral character in two different fractions. The neutral HPAN compounds were eluted with DCM, F2 fraction, and the HPAN basic compounds were eluted with the mixture DCM:isopropanol 5%, F3 fraction. In general, the quantity of recovered AP and HPAN compounds was higher with SPE/Si than SPE/C{sub 18}. The nine oil samples were analyzed by SPE/Si and the saturated and aromatic hydrocarbon were separated from the polar AP and HPAN. (author)

  7. Crystal structure of 3-{5-[3-(4-fluorophenyl-1-isopropyl-1H-indol-2-yl]-1H-pyrazol-1-yl}indolin-2-one ethanol monosolvate

    Directory of Open Access Journals (Sweden)

    Md. Lutfor Rahman

    2016-03-01

    Full Text Available The title indolin-2-one compound, C28H23FN4O·C2H6O, crystallizes as a 1:1 ethanol solvate. The ethanol molecule is disordered over two positions with refined site occupancies of 0.560 (14 and 0.440 (14. The pyrazole ring makes dihedral angles of 84.16 (10 and 85.33 (9° with the indolin-2-one and indole rings, respectively, whereas the dihedral angle between indolin-2-one and indole rings is 57.30 (7°. In the crystal, the components are linked by N—H...O and O—H...O hydrogen bonds, forming an inversion molecule–solvate 2:2 dimer with R44(12 ring motifs. The crystal structure is consolidated by π–π interaction between pairs of inversion-related indolin-2-one rings [interplanar spacing = 3.599 (2 Å].

  8. Crystal structure of 4-(4-chlorophenyl-6-(morpholin-4-ylpyridazin-3(2H-one

    Directory of Open Access Journals (Sweden)

    Abdullah Aydın

    2015-08-01

    Full Text Available In the title compound, C14H14ClN3O2, the morpholine ring adopts a chair conformation, with the exocyclic N—C bond in an equatorial orientation. The 1,6-dihydropyridazine ring is essentially planar, with a maximum deviation of 0.014 (1 Å, and forms a dihedral angle of 40.16 (7° with the plane of the benzene ring. In the crystal, pairs of centrosymmetrically related molecules are linked into dimers via N—H...O hydrogen bonds, forming R22(8 ring motifs. The dimers are connected via C—H...O and C—H...Cl hydrogen bonds, forming a three-dimensional network. Aromatic π–π stacking interactions [centroid–centroid distance = 3.6665 (9 Å] are also observed. Semi-empirical molecular orbital calculations were carried out using the AM1 method. The calculated dihedral angles between the pyridizine and benzene rings and between the pyridizine and morpholine (all atoms rings are 34.49 and 76.96°, respectively·The corresponding values obtained from the X-ray structure determination are 40.16 (7 and 12.97 (9°, respectively. The morpholine ring of the title compound in the calculated gas-phase seems to have a quite different orientation compared to that indicated by the X-ray structure determination.

  9. Learn Objective-C on the Mac for OS X and iOS

    CERN Document Server

    Knaster, Scott; Malik, Waqar

    2012-01-01

    Learn to write apps for some of today's hottest technologies, including the iPhone and iPad (using iOS), as well as the Mac (using OS X). It starts with Objective-C, the base language on which the native iOS software development kit (SDK) and the OS X are based. Learn Objective-C on the Mac: For OS X and iOS, Second Edition updates a best selling book and is an extensive, newly updated guide to Objective-C. Objective-C is a powerful, object-oriented extension of C, making this update the perfect follow-up to Dave Mark's bestselling Learn C on the Mac. Whether you're an experienced C programmer

  10. 10-Benzyl-10H-phenothiazine 9-oxide

    Directory of Open Access Journals (Sweden)

    Zhouqing Xu

    2009-08-01

    Full Text Available In the title compound, C19H15NOS, the butterfly angle between the mean planes defined by the S, N and phenyl C atoms of the two wings of the phenothiazine unit is 23.4 (1°. In the crystal, a supramolecular two-dimensional arrangement arises from weak intermolecular C—H...O interactions.

  11. Development of novel strategy for the synthesis of organometallic compounds usable as protein ligands: application to the human cyclophilin hCyp-18

    International Nuclear Information System (INIS)

    Clavaud, C.

    2006-02-01

    This thesis describes a new strategy for the development of bioactive organometallic compounds, basing on the combinatorial assembly of sub-chemical libraries (A and B) independent but complementary and able to coordinate a metallic heart M to form A-M-B complex potential ligands of biomolecules. The coordination of metals, well adapted to the production of molecular variety is usually used in medicinal chemistry, in diagnostic and therapeutic nuclear medicine. Among the useful elements, the rhenium and the technetium are metals of choice for the development of the assembly strategy because of their chemical and radiochemical properties and of the structure analogy of their complexes. This strategy was validated in vitro. The protein chosen for this purpose was the cyclophilin hCyp-18. (N.C.)

  12. Bis(2,2'-bipyridyl-κN,N')(carbonato-κO,O')cobalt(III) bromide trihydrate.

    Science.gov (United States)

    Ma, Peng-Tao; Wang, Yu-Xia; Zhang, Guo-Qian; Li, Ming-Xue

    2007-12-06

    The title complex, [Co(CO(3))(C(10)H(8)N(2))(2)]Br·3H(2)O, is isostructural with the chloride analogue. The six-coordinated octahedral [Co(2,2'-bipy)(2)CO(3)](+) cation (2,2'-bipy is 2,2'-bipyrid-yl), bromide ion and water mol-ecules are linked together via O-H⋯Br and O-H⋯O hydrogen bonds, generating a one-dimensional chain.

  13. Poly[[diaquabis(2,2′-bipyridine-κ2N,N′(μ3-5-hydroxyisophthalato-κ5O1,O1′:O3,O3′:O3′(μ3-5-hydroxyisophthalato-κ4O1,O1′:O3:O3′(μ2-5-hydroxyisophthalato-κ3O1,O1′:O3didysprosium(III] dihydrate

    Directory of Open Access Journals (Sweden)

    Yan-Lin Zhang

    2011-10-01

    Full Text Available The polymeric title compound, {[Dy2(C8H4O53(C10H8N22(H2O2]·2H2O}n, contains two independent DyIII ions, both of which are nine-coordinated in a distorted tricapped trigonal–prismatic geometry. One DyIII ion is coordinated by five 5-hydroxyisophthalate (hip ligands and one 2,2′-bipyridine (bpy ligand and the other by three hip ligands, one bpy ligand and two water molecules. The DyIII ions are bridged by the carboxylate groups of the hip ligands, forming a three-dimensional framework. O—H...O hydrogen bonds are present in the crystal structure.

  14. cis-Bis(O-methyl-dithio-carbonato-κ(2) S,S')bis-(tri-phenyl-phosphane-κP)ruthenium(II).

    Science.gov (United States)

    Valerio-Cárdenas, Cintya; Hernández-Ortega, Simón; Reyes-Martínez, Reyna; Morales-Morales, David

    2013-01-01

    In the title compound, [Ru(CH3OCS2)2(C18H15P)2], the Ru(II) atom is in a distorted octa-hedral coordination by two xanthate anions (CH3OCS2) and two tri-phenyl-phosphane (PPh3) ligands. Both bidentate xanthate ligands coordinate the Ru(II) atom with two slightly different Ru-S bond lengths but with virtually equal bite angles [71.57 (4) and 71.58 (3)°]. The packing of the complexes is assured by C-H⋯O and C-H⋯π inter-actions.

  15. Metabolic fate of 18F-FDG in mice bearing either SCCVII squamous cell carcinoma or C3H mammary carcinoma

    DEFF Research Database (Denmark)

    Kaarstad, Katrin; Bender, Dirk; Bentzen, Lise

    2002-01-01

    in mice. METHODS: 18F-FDG was given intravenously to mice with either SCCVII squamous cell carcinoma or C3H mammary carcinoma grown on the back. 18F-Labeled metabolites were determined by radio-high-performance liquid chromatography in tumor tissue biopsies, in a time course of 180 min (12 mice of each...... tumor type), and in liver tissue biopsies 80 min after tracer injection (2 mice of each type). RESULTS: After the tracer injection, not only 18F-FDG and 18F-FDG-6-P but also 18F-FD-PG1 and 2-18F-fluoro-2-deoxy-1,6-biphosphate were detected in both tumors, relatively more in SCCVII carcinoma than in C3H...... carcinoma. Both tumors accumulated radioactivity throughout the 180-min measurement period, 4-fold more in SCCVII carcinoma than in C3H carcinoma. At 80 min, the radioactivity was approximately 6 and 1.2 times higher in the respective tumors than in liver tissue. CONCLUSION: Our results agree...

  16. Lattice dynamics and thermophysical properties of h.c.p. Os and Ru from the quasi-harmonic approximation.

    Science.gov (United States)

    Palumbo, Mauro; Dal Corso, Andrea

    2017-10-04

    We report first-principles phonon frequencies and anharmonic thermodynamic properties of h.c.p. Os and Ru calculated within the quasi-harmonic approximation, including Grüneisen parameters, temperature-dependent lattice parameters, thermal expansion, and isobaric heat capacity. We discuss the differences between a full treatment of anisotropy and a simplified approach with a constant [Formula: see text] ratio. The results are systematically compared with the available theoretical and experimental data and an overall satisfactory agreement is obtained.

  17. Two new hydrogen bond-supported supramolecular compounds assembly from polyoxovanadate and organoamines

    International Nuclear Information System (INIS)

    Duan Weijie; Cui Xiaobing; Xu Yan; Xu Jiqing; Yu Haihui; Yi Zhihui; Cui Jiwen; Wang Tiegang

    2007-01-01

    Two novel organic-inorganic hybrid compounds based on organoamines and polyoxovanadates formulated as (H 2 dien) 4 [H 10 V 18 O 42 (PO 4 )](PO 4 ).2H 2 O (1) (dien=diethylenetriamine) and (Him) 8 [HV 18 O 42 (PO 4 )] (2) (im=imidazole) have been prepared under hydrothermal conditions by using different starting materials, and characterized by elemental analyses, IR, ESR, XPS, TGA and single-crystal X-ray diffraction analyses. Crystal data for compound 1: C 16 H 74 N 12 O 52 V 18 P 2 , Monoclinic, space group C2/c, a=23.9593(4) A, b=13.0098(2) A, c=20.1703(4) A, β=105.566(3) o , V=6056.6(19) A 3 , Z=4; for compound 2, C 24 H 41 N 16 O 46 V 18 P, Tetragonal, space group I4/mmm, a=13.5154(8) A, b=13.5154(8) A, c=19.1136 A, β=90 o , V=3491.4(3) A 3 , Z=2. Compound 1 consists of protonated diens together with polyoxovanadates [H 10 V 18 O 42 (PO 4 )] 5- . Compound 2 is composed of protonated ims and polyoxovanadates [HV 18 O 42 (PO 4 )] 8- . There are hydrogen-bonding interactions between polyoxovanadates and different organoamines in 1 and 2. Polyoxovanadates are linked through H 2 dien into a three-dimensional network via hydrogen bonds in 1, while polyoxovanadates are linked by Him into a two-dimensional layer network via hydrogen bonds in 2. The crystal packing patterns of the two compounds reveal various supramolecular frameworks. - Graphical abstract: Two new organic-inorganic hybrid compounds based on [V 18 O 42 (PO 4 )] building blocks have been hydrothermally synthesized. 1 is the first 3-D supramolecular network structure consisting of [V 18 O 42 (PO 4 )] unit, while 2 possesses 2-D layered supramolecular structure

  18. N-[5-Methyl-2-(2-nitrophenyl-4-oxo-1,3-thiazolidin-3-yl]pyridine-3-carboxamide monohydrate

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2011-02-01

    Full Text Available In the title compound, C16H14N4O4S·H2O, the benzene and pyridine rings make a dihedral angle of 85.8 (1°. Both enantiomers of the chiral title compound are statistically disordered over the same position in the unit cell. The methyl and carbonyl group attached to the stereogenic center (C5 of the thiazolidine ring were therefore refined with common site-occupation factors of 0.531 (9 and 0.469 (9, respectively, for each stereoisomer. In the crystal, intermolecular N—H...O, O—H...O and O—H...N hydrogen bonds link the molecules, forming a three-dimensional supramolecular network. The crystal structure further shows π–π stacking interactions [centroid–centroid distance = 3.5063 (13 Å] between the pyridine rings.

  19. 2-Chloroquinazolin-4(3H-one

    Directory of Open Access Journals (Sweden)

    Dong-Lei Cao

    2012-06-01

    Full Text Available In the title compound, C8H5ClN2O, the quinazoline system is approximately planar with a maximum deviation from the least-squares plane of 0.034 (2 Å. In the crystal, classical N—H...O and weak non-classical C—H...N hydrogen bonds link the molecules.

  20. Synthesis and crystal structure of trans-[Ni(pyzdcH)M 2 (H 2 O) 2 ...

    African Journals Online (AJOL)

    The determined structure of the title compound C24H20Ni2N8O20 consists of the mononuclear trans-[Ni(pyzdc)2(H2O)2], (pyzdc = pyrazine-2,3- dicarboxylate). The Ni(II) atom is hexa-coordinated by two (pyzdcH)- groups and two water molecules. The coordinated water molecules are in trans-diaxial positions and the ...

  1. Di-μ-iodido-bis{[(R-(+-2,2′-bis(diphenylphosphanyl-1,1′-binaphthyl-κ2P,P′]copper(I} 0.67-hydrate

    Directory of Open Access Journals (Sweden)

    Daniel Volz

    2012-04-01

    Full Text Available The structure of the title compound, [Cu2I2(C44H32P22]·0.67H2O, has been determined because of its interesting catalytic and optical features. The molecule, which has non-crystallographic C2-symmetry, consists of a core structure of two CuI ions, bridged by two iodide ions. Each CuI ion is also coordinated by one equivalent of the chiral bidentate (R-BINAP ligand [BINAP = 2,2′-bis(diphenylphosphanyl-1,1′-binaphthyl]. Thus, both cations show a distorted tetrahedral geometry being surrounded by two I atoms and two P atoms from the (R-BINAP ligands. The complex consists of isolated butterfly-shaped molecules featuring an angle of 146.11 (2° between adjacent CuI2 planes. The structure displays intramolecular C—H...I hydrogen bonding and contains disordered water. The absolute configuration of this chiral complex was determined by anomalous dispersion effects.

  2. 3-[4-(10H-Indolo[3,2-b]quinolin-11-ylpiperazin-1-yl]propan-1-ol

    Directory of Open Access Journals (Sweden)

    Gary S. Nichol

    2011-12-01

    Full Text Available In the title compound, C22H24N4O, the aromatic moiety is essentially planar (r.m.s. deviation of a least-squares plane fitted through all non-H atoms = 0.0386 Å and is rotated by 89.98 (4° from the piperazine ring, which adopts the expected chair conformation. The propanol chain is not fully extended away from the piperazine ring. In the crystal, there are two unique hydrogen-bonding interactions. One is an O—H...N interaction which, together with an inversion-related symmetry equivalent, forms a ring motif. The second is an N—H...N interaction which links adjacent molecules by means of a chain motif which propagates in the c-axis direction. Overall, a two-dimensional hydrogen-bonded structure is formed.

  3. Low-temperature heat capacity and standard molar enthalpy of formation of 9-fluorenemethanol (C14H12O)

    International Nuclear Information System (INIS)

    Di, You-Ying; Tan, Zhi-Cheng.; Sun, Xiao-Hong; Wang, Mei-Han; Xu, Fen; Liu, Yuan-Fa; Sun, Li-Xian; Zhang, Hong-Tao

    2004-01-01

    Low-temperature heat capacities of the 9-fluorenemethanol (C 14 H 12 O) have been precisely measured with a small sample automatic adiabatic calorimeter over the temperature range between T=78 K and T=390 K. The solid-liquid phase transition of the compound has been observed to be T fus =(376.567±0.012) K from the heat-capacity measurements. The molar enthalpy and entropy of the melting of the substance were determined to be Δ fus H m =(26.273±0.013) kJ · mol -1 and Δ fus S m =(69.770±0.035) J · K -1 · mol -1 . The experimental values of molar heat capacities in solid and liquid regions have been fitted to two polynomial equations by the least squares method. The constant-volume energy and standard molar enthalpy of combustion of the compound have been determined, Δ c U(C 14 H 12 O, s)=-(7125.56 ± 4.62) kJ · mol -1 and Δ c H m compfn (C 14 H 12 O, s)=-(7131.76 ± 4.62) kJ · mol -1 , by means of a homemade precision oxygen-bomb combustion calorimeter at T=(298.15±0.001) K. The standard molar enthalpy of formation of the compound has been derived, Δ f H m compfn (C 14 H 12 O,s)=-(92.36 ± 0.97) kJ · mol -1 , from the standard molar enthalpy of combustion of the compound in combination with other auxiliary thermodynamic quantities through a Hess thermochemical cycle

  4. Gas-phase Absorptions of {{\\rm{C}}}_{42}{{\\rm{H}}}_{18}^{+} near 8300 Å below 10 K: Astronomical Implications

    Science.gov (United States)

    Campbell, E. K.; Maier, J. P.

    2017-11-01

    The gas-phase electronic spectrum of {{{C}}}42{{{H}}}18+ ({{HBC}}+) with an origin band at 8281 \\mathringA has been measured below 10 {{K}} by photofragmentation of helium complexes ({{{C}}}42{{{H}}}18+{--}{{He}}n) in a radiofrequency trap. {{HBC}}+ is a medium-sized polycyclic aromatic hydrocarbon (PAH) cation, and using an ion trapping technique it has been possible to record a high-quality gas-phase spectrum to directly compare with astronomical observations. No diffuse interstellar bands (DIBs) have been reported at the wavelengths of the strongest absorption bands in the {{{C}}}42{{{H}}}18+ spectrum. Measurement of absolute absorption cross sections in the ion trap allows upper limits to the column density of this ion to be {10}12 {{cm}}-2, indicating that even PAH cations of this size, which are believed to be stable in the interstellar medium, should be excluded as candidates for at least the strong DIBs.

  5. Potassium (2,2'-bipyridine-κN,N')bis-(carbonato-κO,O')cobaltate(III) dihydrate.

    Science.gov (United States)

    Wang, Jian-Fei; Lin, Jian-Li

    2010-09-30

    In the title compound, K[Co(CO(3))(2)(C(10)H(8)N(2))]·2H(2)O, the Co(III) atom is coordinated by two bipyridine N atoms and four O atoms from two bidentate chelating carbonate anions, and thus adopts a distorted octa-hedral N(2)O(4) environment. The [Co(bipy)(CO(3))(2)](-) (bipy is 2,2'-bipyridine) -units are stacked along [100] via π-π stacking inter-actions, with inter-planar distances between the bipyridine rings of 3.36 (4) and 3.44 (6) Å, forming chains. Classical O-H⋯O hydrogen-bonding inter-actions link the chains, forming channels along (100) in which the K(+) ions reside and leading to a three-dimensional supra-molecular architecture.

  6. Crystal structure of (acetato-κO(ethanol-κO[(9S,17S,21S,29S-9,17,21,29-tetrahydroxy-18,30-dioxaoctacyclo[18.10.0.02,7.08,19.09,17.011,16.021,29.023,28]triaconta-1,3,5,7,11(16,12,14,19,23(28,24,26-undecaene-10,22-dione-κ3O18,O21,O22]caesium ethanol monosolvate

    Directory of Open Access Journals (Sweden)

    Ravell Bengiat

    2016-07-01

    Full Text Available The title compound, [Cs(CH3COO(C28H16O8(C2H5OH]·C2H5OH, is the product of the complexation between one vasarene analogue [1], bis ninhydrin naphthalene-1,3-diol and CsF, where the F− ion has reacted with residual acetic acid (AcOH, to form a [1]·CsOAc complex. The intermolecular interactions with the multiple oxygen-containing functional groups of the ligand, as well as O—H...O hydrogen bonds involving the ethanol solvent molecules, stabilize the complex, forming a chain along [100]. Additional parallel-displaced π–π stacking, with an interplanar distance of 3.669 (1 Å, connect several unit cells in a three-dimensional supramolecular structure, though, the larger size of AcO− (1.60 Å compared to F− (1.33 Å prevents the tight packing that was once achieved with other vasarene complexes of CsF.

  7. Synthesis, characterization and thermal decomposition of [Pd2 (C2-dmba (µ-SO4 (SO22

    Directory of Open Access Journals (Sweden)

    Caires Antonio Carlos Fávero

    1998-01-01

    Full Text Available The bridged sulphate complex [Pd2 (C²,dmba (µ-SO4 (SO22] has been obtained by reacting a saturated solution of SO2 in methanol and the cyclometallated compound [Pd(C²,N-dmba(µ-N3] 2; (dmba = N,N-dimethylbenzylamine, at room temperature for 24 h. Reaction product was characterized by elemental analysis, NMR comprising 13C{¹H} and ¹H nuclei and I.R. spectrum's measurements. Thermal behavior has been investigated and residual products identified by X-ray powder diffraction.

  8. Amyloid imaging in cognitively normal older adults: comparison between 18F-flutemetamol and 11C-Pittsburgh compound B

    International Nuclear Information System (INIS)

    Adamczuk, Katarzyna; Schaeverbeke, Jolien; Neyens, Veerle; Dupont, Patrick; Nelissen, Natalie; Vandenbulcke, Mathieu; Goffin, Karolien; Lilja, Johan; Hilven, Kelly; Laere, Koen van; Vandenberghe, Rik

    2016-01-01

    Preclinical, or asymptomatic, Alzheimer's disease (AD) refers to the presence of positive AD biomarkers in the absence of cognitive deficits. This research concept is being applied to define target populations for clinical drug development. In a prospective community-recruited cohort of cognitively intact older adults, we compared two amyloid imaging markers within subjects: 18 F-flutemetamol and 11 C-Pittsburgh compound B (PIB). In 32 community-recruited cognitively intact older adults aged between 65 and 80 years, we determined the concordance between binary classification based on 18 F-flutemetamol versus 11 C-PIB according to semiquantitative assessment (standardized uptake value ratio in composite cortical volume, SUVR comp ) and, alternatively, according to visual reads. We also determined the correlation between 18 F-flutemetamol and 11 C-PIB SUVR and evaluated how this was affected by the reference region chosen (cerebellar grey matter versus pons) and the use of partial volume correction (PVC) in this population. Binary classification based on semiquantitative assessment was concordant between 18 F-flutemetamol and 11 C-PIB in 94 % of cases. Concordance of blinded binary visual reads between tracers was 84 %. The Spearman correlation between 18 F-flutemetamol and 11 C-PIB SUVR comp with cerebellar grey matter as reference region was 0.84, with a slope of 0.98. Correlations in neocortical regions were significantly lower with the pons as reference region. PVC improved the correlation in striatum and medial temporal cortex. For the definition of preclinical AD based on 18 F-flutemetamol, concordance with 11 C-PIB was highest using semiquantitative assessment with cerebellar grey matter as reference region. (orig.)

  9. [μ-Bis(diphenylphosphanylmethane]tricarbonyl(μ-p-toluenesulfonylmethyl isocyanato(triphenylphosphaneironplatinum(Fe—Pt

    Directory of Open Access Journals (Sweden)

    Carsten Strohmann

    2012-03-01

    Full Text Available The title compound, [FePt(C9H9NO2S(C18H15P(C25H22P2(CO3], represents a rare example of an isonitrile-bridged heterobimetallic complex (here Pt and Fe and is an interesting precursor for the preparation of heterodinuclear μ-aminocarbyne complexes, since the basic imine-type N atom of the μ2-C=N–R ligand readily undergoes addition with various electrophiles to afford iminium-like salts. In the crystal, the almost symmetrically bridging μ2-C=N-R ligand (neglecting the different atomic radii of Fe and Pt is strongly bent towards the Fe(CO3 fragment, with a C=N-R angle of only 121.1 (4°.

  10. 2-(7-Methyl-1H-indol-3-ylacetonitrile

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    Yu-Hua Ge

    2012-01-01

    Full Text Available In the title compound, C11H10N2, the carbonitrile group is twisted away from the indole plane [Ccy—Cme—Car—Car = 66.6 (2°; cy = cyanide, me = methylene and ar = aromatic]. In the crystal, N—H...N hydrogen bonds link the molecules into C(7 chains propagating in the [001] direction.

  11. 3-D silver(I)-lanthanide(III) heterometallic-organic frameworks constructed from 2,2'-bipyridine-3,3'-dicarboxylic acid: synthesis, structure, photoluminescence, and their remarkable thermostability.

    Science.gov (United States)

    Zhou, Yunshan; Li, Xiaomin; Zhang, Lijuan; Guo, Yan; Shi, Zonghai

    2014-04-07

    A new family of silver(I)-lanthanide(III) heterometallic-organic frameworks having the formula [AgLn(bpdc)2] (Ln = Eu (1), Tb (2), Sm (3), Dy (4), Y (5), Yb (6), Er (7), Ho (8); H2bpdc = 2,2'-bipyridine-3,3'-dicarboxylic acid), each of which crystallizes in the monoclinic space group C2/c with Z = 4, has been hydrothermally synthesized. The compounds were characterized by means of IR, elemental analysis, thermogravimetric-differential thermal analysis, and powder X-ray diffraction (XRD), wherein compounds 1, 2, and 4-8 were structurally characterized. The powder XRD and single-crystal structures of the title compounds indicate that all the compounds are isostructural and feature a three-dimensional (3-D) open framework. In the structures of the compounds, bpdc(2-) ligands link Ln(3+) through their carboxylic groups, resulting in the formation of a one-dimensional {Ln(bpdc)2}n infinite chain along the c direction. The adjacent chains are then connected to each other through the coordination interaction between Ag(+) and the pyridyl N atoms of bpdc(2-) ligands from the chains, resulting in a 3-D (2,4,6)-connected open framework with (4(11)·6(4))(4(3)·8(2)·10)(8)2 topology. The compounds show remarkable good thermally stability up to 370 °C because neither aquo ligands nor lattice water molecules exist in the composition of the compounds. The photoluminescent properties of compounds 1 and 2 were studied in detail. The energy level of the triplet states of the ligand H2bpdc 21,505 cm(-1) (465 nm) was determined based on the 77 K emission spectrum of the compound [Gd2(bpdc)3(phen)2(H2O)2]·6H2O 9. The (5)D0 and (5)D4 emission lifetimes (1.58 and 1.76 ms) and the overall quantum yields (21% and 22%) were determined for the compounds 1 and 2, respectively.

  12. Bis(O-ethyl dithio­carbonato-κ2 S,S′)bis­(pyridine-3-carbonitrile-κN 1)nickel(II)

    Science.gov (United States)

    Kapoor, Sanjay; Kour, Ramandeep; Sachar, Renu; Kant, Rajni; Gupta, Vivek K.; Kapoor, Kamini

    2012-01-01

    The Ni2+ ion in the title complex, [Ni(C3H5OS2)2(C6H4N2)2], is in a strongly distorted octa­hedral coordination environment formed by an N2S4 donor set, with the Ni2+ ion located on a centre of inversion. In the crystal, weak C—H⋯S and C—H⋯N inter­actions are observed. PMID:22259356

  13. Estimation of lower flammability limits of C-H compounds in air at atmospheric pressure, evaluation of temperature dependence and diluent effect.

    Science.gov (United States)

    Mendiburu, Andrés Z; de Carvalho, João A; Coronado, Christian R

    2015-03-21

    Estimation of the lower flammability limits of C-H compounds at 25 °C and 1 atm; at moderate temperatures and in presence of diluent was the objective of this study. A set of 120 C-H compounds was divided into a correlation set and a prediction set of 60 compounds each. The absolute average relative error for the total set was 7.89%; for the correlation set, it was 6.09%; and for the prediction set it was 9.68%. However, it was shown that by considering different sources of experimental data the values were reduced to 6.5% for the prediction set and to 6.29% for the total set. The method showed consistency with Le Chatelier's law for binary mixtures of C-H compounds. When tested for a temperature range from 5 °C to 100 °C, the absolute average relative errors were 2.41% for methane; 4.78% for propane; 0.29% for iso-butane and 3.86% for propylene. When nitrogen was added, the absolute average relative errors were 2.48% for methane; 5.13% for propane; 0.11% for iso-butane and 0.15% for propylene. When carbon dioxide was added, the absolute relative errors were 1.80% for methane; 5.38% for propane; 0.86% for iso-butane and 1.06% for propylene. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. H2O2 and NADPH oxidases involve in regulation of 2-(2-phenylethyl)chromones accumulation during salt stress in Aquilaria sinensis calli.

    Science.gov (United States)

    Wang, Xiaohui; Dong, Xianjuan; Feng, Yingying; Liu, Xiao; Wang, Jinling; Zhang, Zhongxiu; Li, Jun; Zhao, Yunfang; Shi, Shepo; Tu, Pengfei

    2018-04-01

    2-(2-Phenylethyl)chromones are the main compounds responsible for the quality of agarwood, which is widely used in traditional medicines, incenses and perfumes. H 2 O 2 and NADPH oxidases (also known as respiratory burst oxidase homologs, Rbohs) mediate diverse physiological and biochemical processes in environmental stress responses. However, little is known about the function of H 2 O 2 and NADPH oxidases in 2-(2-phenylethyl)chromones accumulation. In this study, we found that salt stress induced a transient increase in content of H 2 O 2 and 2-(2-phenylethyl)chromones accumulation in Aquilaria sinensis calli. Exogenous H 2 O 2 remarkably decreased the production of 2-(2-phenylethyl)chromones, while dimethylthiourea (DMTU), a scavenger of H 2 O 2 , significantly increased 2-(2-phenylethyl)chromones accumulation in salt treated calli. Three new H 2 O 2 -generating genes, named AsRbohA-C, were isolated and characterized from A. sinensis. Salt stress also induced a transient increase in AsRbohA-C expression and NADPH oxidase activity. Furthermore, exogenous H 2 O 2 increased AsRbohA-C expression and NADPH oxidase activity, while DMTU inhibited AsRbohA-C expression and NADPH oxidase activity under salt stress. Moreover, diphenylene iodonium (DPI), the inhibitor of NADPH oxidases, reduced AsRbohA-C expression and NADPH oxidase activity, but significantly induced 2-(2-phenylethyl)chromones accumulation during salt stress. These results clearly demonstrated the central role of H 2 O 2 and NADPH oxidases in regulation of salt-induced 2-(2-phenylethyl)chromones accumulation in A. sinensis calli. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Crystal structure of {(R-N2-[(benzo[h]quinolin-2-ylmethyl]-N2′-[(benzo[h]quinolin-2-ylmethylidene]-1,1′-binaphthyl-2,2′-diamine-κ4N,N′,N′′,N′′′}(trifluoromethanesulfonato-κOzinc(II} trifluoromethanesulfonate dichloromethane 1.5-solvate

    Directory of Open Access Journals (Sweden)

    Shayna R. Skokan

    2017-07-01

    Full Text Available The zinc(II atom in the title compound, [Zn(C48H31N4(CF3SO3](CF3SO3·1.5CH2Cl2, adopts a distorted five-coordinate square-pyramidal geometry. It is coordinated by one trifluoromethanesulfonate ligand and four N atoms of the N2-[(benzo[h]quinolin-2-ylmethyl]-N2′-[(benzo[h]quinolin-2-ylmethylidene]-1,1′-binaphthyl-2,2′-diamine ligand. The complex is present as a single-stranded P-helimer monohelical structure incorporating π–π and/or σ–π interactions. One of the imine bonds present in the original ligand framework is reduced, leading to variations in bond lengths and torsion angles for each side of the ligand motif. The imine-bond reduction also affects the bond lengths involving the metal atom with the N-donor atoms located on the imine bond. There are two molecules of the complex in the asymmetric unit. One of the molecules exhibits positional disorder within the coordinating trifluoromethanesulfonate ion making the molecules symmetrically non-equivalent.

  16. Crystal structure of 5-[bis(methylsulfonylmethyl]-1,3-dimethyl-5-(methylsulfonylpyrimidine-2,4,6(1H,3H,5H-trione

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    Eyad Mallah

    2015-01-01

    Full Text Available In the title compound, C10H16N2O9S3, the pyrimidine ring of the 1,3-dimethyl barbituric acid moiety has an envelope conformation with the C atom carrying the methylsulfonyl and bis(methylsulfonylmethyl substituents as the flap. The dihedral angle between mean plane of the pyrimidine ring and the S/C/S plane is 72.4 (3°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure.

  17. Synthesis of novel 3-cyclohexylpropanoic acid-derived nitrogen heterocyclic compounds and their evaluation for tuberculostatic activity.

    Science.gov (United States)

    Gobis, Katarzyna; Foks, Henryk; Bojanowski, Krzysztof; Augustynowicz-Kopeć, Ewa; Napiórkowska, Agnieszka

    2012-01-01

    A series of novel 3-cyclohexylpropanoic acid derivatives and 3-cyclohexylpropanoic acid-derived nitrogen heterocyclic compounds (1-8) have been synthesized and evaluated for tuberculostatic activity. Compounds 1a, 1c, 1e and 1f bearing benzimidazole or benzimidazole-like systems showed the most potent tuberculostatic activity against Mycobacterium tuberculosis strains with MIC values ranging from 1.5 to 12.5μg/mL. More importantly 1a (6-chloro-2-(2-cyclohexylethyl)-4-nitro-1H-benzo[d]imidazole) and 1f (2-(2-cyclohexylethyl)-1H-imidazo[4,5-b]phenazine) appeared selective for M. tuberculosis as compared with eukaryotic cells (human fibroblasts), and other antimicrobial strains. These compounds may thus represent a novel, selective class of antitubercular agents. Additionally compound 1a stimulated type I collagen output by fibroblasts, in vitro. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. 1,8-Diazabicyclo[5.4.0]undec-7-en-8-ium bromido(phthalocyaninatozincate

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    Bartosz Przybył

    2014-06-01

    Full Text Available The title compound, (C9H17N2[ZnBr(C32H16N8], contains a bromido(phthalocyaninatozincate anion and a protonated 1,8-diazabicyclo[5.4.0]undece-7-ene cation, [DBUH]+. The central ZnII atom has a distorted square-pyramidal geometry, with four isoindole N atoms of the macrocycle in equatorial positions and a bromide ion in the axial position. The latter has a relatively high displacement parameter, but no evidence for disorder was obtained. The central ZnII atom is displaced by 0.488 (3 Å from the mean plane defined by the four isoindole N atoms. The [DBUH]+ cation is involved in an almost linear N—H...Br hydrogen bond. In the crystal, π–π interactions lead to a relatively short distance of 3.366 (3 Å between the phthalocyaninate rings.

  19. Crystal structure of dimethyl 4,4′-dimethoxybiphenyl-3,3′-dicarboxylate

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    Fredrik Lundvall

    2016-03-01

    Full Text Available In the title compound, C18H18O6, the benzene rings are coplanar due to the centrosymmetric nature of the molecule, with an inversion centre located at the midpoint of the C—C bond between the two rings. Consequently, the methyl carboxylate substituents are oriented in a trans fashion with regards to the bond between the benzene rings. The methyl carboxylate and methoxy substituents are rotated slightly out of plane relative to their parent benzene rings, with dihedral and torsion angles of 18.52 (8 and −5.22 (15°, respectively. The shortest O...H contact between neighbouring molecules is about 2.5 Å. Although some structure-directing contributions from C—H...O hydrogen-bonding interactions are possible, the crystal packing seems primarily directed by weak van der Waals forces.

  20. An open-framework three-dimensional indium oxalate: [In(OH)(C2O4)(H2O)]3.H2O

    International Nuclear Information System (INIS)

    Yang Sihai; Li Guobao; Tian Shujian; Liao Fuhui; Lin Jianhua

    2005-01-01

    By hydrothermal reaction of In 2 O 3 with H 2 C 2 O 4 .2H 2 O in the presence of H 3 BO 3 at 155 deg. C, an open-framework three-dimensional indium oxalate of formula [In(OH)(C 2 O 4 )(H 2 O)] 3 .H 2 O (1) has been obtained. The compound crystallizes in the trigonal system, space group R3c with a=18.668(3)A, c=7.953(2)A, V=2400.3(7)A 3 , Z=6, R 1 =0.0352 at 298K. The small pores in 1 are filled with water molecules. It loses its filled water at about 180 deg. C without the change of structure, then the bounded water at 260 deg. C, and completely decompounds at 324 deg. C. The residue is confirmed to be In 2 O 3

  1. 4,5,7,8,17-Pentahydroxy-14,18-dimethyl-6-methylene-3,10-dioxapentacyclo[9.8.0.01,7.04,19.013,18]nonadec-14-ene-9,16-dione methanol solvate dihydrate

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    Chin Hoe Teh

    2009-04-01

    Full Text Available The title quassinoid compound, C20H24O9·CH3OH·2H2O, is a natural eurycomanone isolated from the roots of Eurycoma longifolia. The molecules contain a fused five-ring system, with one tetrahydrofuran ring adopting an envelope conformation, one tetrahydropyran-2-one ring in a screw boat conformation, one cyclohexenone ring in a half-chair conformation and two cyclohexane rings in chair conformations. Intramolecular C—H...O interactions generate S(5 ring motifs and an O—H...O interaction generates an S(7 ring motif. In the crystal, molecules are linked via intermolecular O—H...O interactions along the b axis and further stacked along a axis. The absolute configuration of the title compound was inferred from previously solved structures of its analogues.

  2. Specific heat of filled skutterudite PrOs4P12

    International Nuclear Information System (INIS)

    Matsuhira, Kazuyuki; Doi, Yoshihiro; Wakeshima, Makoto; Hinatsu, Yukio; Kihou, Kunihiro; Sekine, Chihiro; Shirotani, Ichimin

    2005-01-01

    We report the specific heat of filled skutterudite compounds PrOs 4 P 12 and LaOs 4 P 12 down to 1.8K. The specific heat divided by temperature C(T)/T in PrOs 4 P 12 shows a shoulder around 13K. This shoulder is caused by a Schottky anomaly due to a crystalline electric field effect. The electronic specific heat coefficients γ of PrOs 4 P 12 and LaOs 4 P 12 are estimated to be 56.5 and 21.6mJ/K 2 mol, respectively. The value of γ in PrOs 4 P 12 is 2.6 times larger than that in LaOs 4 P 12

  3. 1-Allyl-3-amino-1H-pyrazole-4-carboxylic acid

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    Feng-Ling Yang

    2008-12-01

    Full Text Available The title compound, C7H9N3O2, was prepared by alkaline hydrolysis of ethyl 1-allyl-3-amino-1H-pyrazole-4-carboxylate. The crystal structure is stabilized by three types of intermolecular hydrogen bond (N—H...O, N—H...N and O—H...N.

  4. 4,4′-Dichloro-2,2′-[(3aR,7aR/3aS,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diylbis(methylene]diphenol

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    Michal Dušek

    2010-10-01

    Full Text Available Molecules of the the title compound, C21H24Cl2N2O2, are located on a twofold rotation axis, which passes through the C atom linking the two N atoms. Two intramolecular O—H...N hydrogen bonds were observed. In the crystal, non-classical intermolecular C—H...O hydrogen bonds link the molecules into chains along the a axis. The crystal studied was a racemic twin.

  5. Efficient method of enzymatic synthesis of nucleosides labelled with 14C and 3H

    International Nuclear Information System (INIS)

    Nejedly, Z.; Filip, J.

    1988-01-01

    The method is presented of enzymatic synthesis of nucleosides labelled with 14 C or 3 H either uniformly or specifically in the base or the deoxyribosyl or ribosyl moiety. The method is based on the ribosylation or deoxyribosylation of the nucleic acid bases (non-labelled or labelled with 14 C or 3 H) by the catalytic effect of enzymes occurring in the supernatant fractions of non-purified homogenates of Escherichia coli B. bacteria. The non-labelled and labelled nucleosides are used as donors of ribosyl or deoxyribosyl groups. The HPLC method is used for separating labelled nucleosides. The radiochemical purity of the labelled nucleosides is higher than 98%, molar activity ranges from 9.2 to 18.5 GBq.mmol -1 ( 14 C-labelled compounds) and from 0.6 to 1.9 TBq.mmol -1 (3H-labelled compounds). (author). 4 figs., 8 refs

  6. Poly[[diaquabis(μ2-4,4′-bipyridinemanganese(II] bis[2-(2-carboxyphenyldisulfanylbenzoate

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    Shao-Ming Fang

    2009-05-01

    Full Text Available The title complex, {[Mn(C10H8N22(H2O2](C14H9O4S22}n, contains an octahedrally coordinated MnII cation and 2-(2-carboxyphenyldisulfanylbenzoate anions. The MnII center is situated on a crystallographic center of inversion and is coordinated by four 4,4′-bipyridine (4,4′-bipy ligands and two water molecules. The 4,4′-bipy ligands act as bridging ligands, producing a fishing-net-like two-dimensional framework. In the crystal structure, this positively charged framework is charge balanced by 2-(2-carboxyphenyldisulfanylbenzoate anions that form a separate anionic two-dimensional framework via intermolecular O—H...O hydrogen bonds and C—H...π stacking interactions. Additional intermolecular O—H...O hydrogen bonds link the cationic and anionic frameworks to form the three-dimensional crystal structure.

  7. Triphenyl{(E-4-[4-(phenyldiazenylphenyl]-4H-1,2,4-triazol-1-yl}boron

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    Daisuke Urakami

    2009-10-01

    Full Text Available In the title compound, C32H26BN5 or [(C14H11N5B(C6H53], the B atom is approximately tetrahedrally coordinated. The diazo unit is in a trans conformation, which is generally more stable than a cis one for aromatic azo compounds. The crystal structure features very weak C—H...π interactions. The dihedral angles between the central benzene ring and the terminal rings in the heterocycle are 62.64, 73.54 and 61.60°.

  8. 4,4′-Diiodo-2,2′-[(3aR,7aR-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diylbis(methylene]diphenol

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    Augusto Rivera

    2011-09-01

    Full Text Available In the crystal structure of the title compound, C21H24I2N2O2, the two N atoms of the imidazolidine moiety are linked to the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. The cyclohexane ring adopts a chair conformation and the heterocyclic ring to which it is fused has a twisted envelope conformation.

  9. Bis(N-ethyl-N-methyldithiocarbamato-κ2S,S′diphenyltin(IV

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    Amirah Faizah Muthalib

    2010-04-01

    Full Text Available The dithiocarbamate anions in the title compound, [Sn(C6H52(C4H8NS22], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The molecule lies across a twofold rotation axis.

  10. Bis(N-isopropyl-N-methyldithiocarbamato-κ2S,S′diphenyltin(IV

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    Amirah Faizah Muthalib

    2010-04-01

    Full Text Available The dithiocarbamate anions in the title compound, [Sn(C6H52(C5H10NS22], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The molecule lies across a twofold rotation axis.

  11. 5-(2,5-Dioxooxolan-3-yl-8-methyl-3,3a,4,5-tetrahydro-1H-naphtho[1,2-c]furan-1,3-dione

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    Y. Z. Guo

    2013-02-01

    Full Text Available In the title compound, C17H14O6, the dihedral angle between the two anhydride rings is 76.01 (8°while the dihedral angles between the benzene and anhydride rings are 42.60 (7 and 68.94 (7°. The cyclohexene ring of the tetrahydronaphthalene unit exhibits an envelope conformation.

  12. Diethyl 2,2-bis(3,5-di-tert-butyl-4-hydroxybenzylmalonate

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    Tao Zeng

    2012-02-01

    Full Text Available The title molecule, C37H56O6, possesses twofold symmetry, with the twofold axis passing through the quaternary C atom. In the crystal, neighbouring molecules are linked via O—H...O hydrogen bonds involving the phenol OH group and the carbonyl O atom, forming chains propagating in [101]. Within these chains, rings are formed with an R22(20 motif. There are also C—H...O interactions present within the rings.

  13. RhII -Catalyzed β-C(sp2 )-H Alkylation of Enol Ethers, Enamides and Enecarbamates with α-Diazo Dicarbonyl Compounds.

    Science.gov (United States)

    McLarney, Brett D; Cavitt, Marchello A; Donnell, Theodore M; Musaev, Djamaladdin G; France, Stefan

    2017-01-23

    A Rh II -catalyzed method for intermolecular alkylation of the β-C(sp 2 )-H bond of enol ethers, enamides, and enecarbamates with α-diazo-1,3-dicarbonyl compounds is reported. The products are formed in up to 99 % yield and can be readily derivatized under a variety of conditions. By utilizing a combination of experimental and computational studies, the presumptive addition-elimination reaction mechanism was investigated and found to proceed under thermodynamic control at higher temperature. The acquired fundamental knowledge was translated into a strategic reaction design and yielded the first example of the β-C-H functionalizations of acyclic enol ethers using α-diazo-1,3-dicarbonyl compounds. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Crystal structure of 2-[(3aS,6R-3,3,6-trimethyl-3,3a,4,5,6,7-hexahydro-2H-indazol-2-yl]thiazol-4(5H-one

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    Abdellah N'ait Ousidi

    2016-03-01

    Full Text Available The title compound, C13H19N3OS, is a new thiazolidin-4-one derivative prepared and isolated as the pure (3aS,6R-diastereisomer from (R-thiosemicarbazone pulegone. It crystallized with two independent molecules (A and B in the asymmetric unit. The compound is composed of a hexhydroindazole ring system (viz. a five-membered dihydropyrazole ring fused to a cyclohexyl ring with a thiazole-4-one ring system attached to one of the pyrazole N atoms (at position 2. The overall geometry of the two molecules differs slightly, with the mean planes of the pyrazole and thiazole rings being inclined to one another by 10.4 (1° in molecule A and 0.9 (1° in molecule B. In the crystal, the A and B molecules are linked via C—H...O hydrogen bonds, forming slabs parallel to the ab plane. There are C—H...π interactions present within the layers, and between the layers, so forming a three-dimensional structure.

  15. In situ ligand synthesis with the UO22+ cation under hydrothermal conditions

    International Nuclear Information System (INIS)

    Frisch, Mark; Cahill, Christopher L.

    2007-01-01

    A novel uranium (VI) coordination polymer, (UO 2 ) 2 (C 2 O 4 )(C 5 H 6 NO 3 ) 2 (1), has been prepared under the hydrothermal reaction of uranium nitrate hexahydrate and L-pyroglutamic acid. Compound 1 (monoclinic, C2/c, a=22.541(6) A, b=5.7428(15) A, c=15.815(4) A, β=119.112(4) o , Z=4, R 1 =0.0237, wR 2 =0.0367) consists of uranium pentagonal bipyramids linked via L-pyroglutamate and oxalate anions to form an overall two-dimensional (2D) structure. With the absence of oxalic acid within the starting materials, the oxalate anions are hypothesized to form in situ whereby decarboxylation of L-pyroglutamic acid occurs followed by coupling of CO 2 to form the oxalate linkages as observed in the crystal structure. Addition of copper (II) to this system appears to promote oxalate formation in that synthetic moolooite (Cu(C 2 O 4 ).nH 2 O; 0≤n≤1) and a known uranyl oxalate [(UO 2 ) 2 (C 2 O 4 )(OH) 2 (H 2 O) 2 .H 2 O], co-crystallize in significant quantity. Compound 1 exhibits the characteristic uranyl emission spectrum upon either direct uranyl excitation or ligand excitation, the latter of which shows an increase in relative intensity. This subsequent increase in the intensity indicates an energy transfer from the ligand to the uranyl cations thus illustrating an example of the antenna effect in the solid state. - Graphical abstract: A novel homometallic coordination polymer (UO 2 ) 2 (C 2 O 4 )(C 5 H 6 NO 3 ) 2 , in the uranium-L-pyroglutamic acid system has been synthesized under hydrothermal conditions. The title compound consists of uranium pentagonal bipyramids bridged through both L-pyroglutamate and oxalate linkages to produce a 3D crystal structure. The oxalate anions are theorized to result from decarboxylation of L-pyroglutamic acid followed by subsequent coupling of CO 2

  16. Crystal structure of poly[[μ-1,1′-(butane-1,4-diylbis(1H-benzimidazole-κ2N3:N3′]{μ-4,4′-[1,4-phenylenebis(oxy]dibenzoato-κ4O,O′:O′′,O′′′}cobalt(II

    Directory of Open Access Journals (Sweden)

    Chen Xie

    2015-06-01

    Full Text Available In the title compound, [Co(C20H12O6(C18H18N4]n, the CoII atom, located on a twofold rotation axis, is hexacoordinated to four O from two bis-bidentate 4,4′-[phenylenebis(oxy]dibenzoate (L ligands and two N atoms from two 1,1′-(butane-1,4-diylbis(1H-benzimidazole (bbbm ligands, forming a distorted octahedral cis-N2O4 coordination environment. Polymeric zigzag chains along [102] are built up by the bridging L ligands. These chains are additionally connected by the bbbm ligands to produce a two-dimensional coordination polymer parallel too (010.

  17. C{sub 60}{sup 3-} versus C{sub 60}{sup 4-} /C{sub 60}{sup 2-} - synthesis and characterization of five salts containing discrete fullerene anions

    Energy Technology Data Exchange (ETDEWEB)

    Boeddinghaus, M. Bele; Klein, Wilhelm; Wahl, Bernhard; Faessler, Thomas F. [Department of Chemistry, Technische Universitaet Muenchen, Garching (Germany); Jakes, Peter; Eichel, Ruediger A. [Institut fuer Energie- und Klimaforschung (IEK-9), Forschungszentrum Juelich (Germany)

    2014-04-15

    Five new compounds, [Rb(18crown-6)]{sub 3}[C{sub 60}] (1), [Rb(18crown-6)]{sub 6}[C{sub 60}]{sub 2}(C{sub 3}H{sub 7}NO){sub 2}(C{sub 4}H{sub 8}O){sub 2} (2), [Rb(benzo18crown-6)]{sub 6}[C{sub 60}]{sub 2}(C{sub 2}H{sub 8}N{sub 2}){sub 5} (3), [Cs(benzo18crown-6)]{sub 3}C{sub 60}(C{sub 2}H{sub 8}N{sub 2}){sub 2} (4), and [Cs{sub 3}(benzo18crown-6){sub 5}]C{sub 60}(C{sub 2}H{sub 8}N{sub 2}){sub (4.5+x)} (5) were synthesized and characterized by single-crystal X-ray structure determination. All compounds contain discrete C{sub 60} anions, which are ordered in 1, 2, and 4, where direct cation-anion contacts occur. The unit cells of 1 and 2 contain two independent fullerides, which coordinate to the rubidium atoms either of two or of four [Rb(18crown-6)] units. Owing to the presence of differently coordinated fullerene units in compounds 1 and 2, a possible disproportionation of C{sub 60}{sup 3-} into C{sub 60}{sup 2-} and C{sub 60}{sup 4-} anions is discussed. In 3 and 4 the C{sub 60} anions are coordinated by three Rb and Cs atoms, respectively. In all compounds the average charge of the anion is -3. Magnetic data reveal a doublet spin state for 3. The EPR spectra are discussed for compounds 3 and 5. The role of a dynamic Jahn-Teller distortion is discussed, and we report the first IR spectroscopic data of fullerene trianions, which have been obtained in solution. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. Structural and spectral analyses of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide)

    Science.gov (United States)

    Yıldırım, Sema Öztürk; Büyükmumcu, Zeki; Pekdur, Özlem Savaş; Butcher, Ray J.; Doǧan, Şengül Dilem

    2018-02-01

    In this study we report structure determination of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide). 2,2'-Dithiobis(benzamide) derivatives have been reported to possess important biological properties such as antibacterial, antifungal activities and inhibition of blood platelet aggregation and redeterrmined at 100(2)K from the data published by Raftery, Lallbeeharry, Bhowon, Laulloo & Joulea [Acta Cryst. 2009, E65, o16]. 2,2'-Dithiobis(N-butyl-benzamide) has been reported to be useful as an antiseptic for cosmetics. The structural properties of the compound have been characterized by using 1H NMR and the structure were determined by single-crystal X-ray diffraction. Molecular structure crystallizes in triclinic form, space group with a = 9.6396(7) Å, b = 9.9115(7) Å, c = 12.0026(8) Å, α = 109.743(6)°, β = 103.653(6)°, γ = 104.633(6)° and V = 977.15(13) Å3. In the solid state of the molecular structure N-H…S, N-H…O and C-H…O, type interactions provide for stabilization. The geometries of the title compound have been optimized using density functional theory (DFT) method. The calculated values were found to be in agreement with the experimental data.

  19. 5,11-Ditosyl-5H,11H-dibenzo[b,f][1,5]diazocine-6,12-dione acetic acid hemisolvate

    Directory of Open Access Journals (Sweden)

    Najat Abbassi

    2013-04-01

    Full Text Available The molecular structure of the title compound, C28H22N2O6S2·0.5CH3COOH, is built up from three fused rings, two six and one eight membered. The eight-membered ring shows a boat conformation and the dihedral angle between the two benzene groups attached thereto is 66.43 (11°, resulting in a V-shaped geometry. Two tosyl substituents are bound to the N atoms. The planes through the tolyl rings are roughly perpendicular, as indicated by the dihedral angle of 82.44 (12°. In the crystal, the molecule and its inversion-related symmetry-equivalent are linked to the acetic acid solvent molecule by non-classical O—H...O and C—H...O hydrogen bonds. Two half-occupied acetic acid solvent molecules are disordered at the same site and linked by a center of symmetry.

  20. The Production of Polycyclic Aromatic Hydrocarbon Anions in Inert Gas Matrices Doped with Alkali Metals. Electronic Absorption Spectra of the Pentacene Anion (C22H14(-))

    Science.gov (United States)

    Halasinski, Thomas M.; Hudgins, Douglas M.; Salama, Farid; Allamandola, Louis J.; Mead, Susan (Technical Monitor)

    1999-01-01

    The absorption spectra of pentacene (C22H14) and its radical cation (C22H14(+)) and anion (C22H14(-)) isolated in inert-gas matrices of Ne, Ar, and Kr are reported from the ultraviolet to the near-infrared. The associated vibronic band systems and their spectroscopic assignments are discussed together with the physical and chemical conditions governing ion (and counterion) production in the solid matrix. In particular, the formation of isolated pentacene anions is found to be optimized in matrices doped with alkali metal (Na and K).

  1. Sterically crowded monomeric neutral bis(benzamidinato) compounds of aluminium, [PhC(NSiMe(3))(2)](2)AlX (X=Cl, H); X-ray crystal structure of [PhC(NSiMe(3))(2)]2AlH

    NARCIS (Netherlands)

    Duchateau, R; Meetsma, A; Teuben, JH

    1996-01-01

    AlCl3 reacts with [PhC(NSiMe(3))(2)]Li(OEt(2)) to afford the bis(N,N'-bis(trimethylsilyl)benzamidinato)aluminium chloro compound which, on treatment with KBEt(3)H, yields the structurally characterized monomeric hydride derivative, [PhC(NSiMe(3))(2)]2AlH, whose reactivity towards unsaturated

  2. (2R,3aR,4S,7R,7aS,9R,10aR,11S,14R,14aS-rel-3a,4,7,7a,10a,11,14,14a-Octahydro-4,14:7,11-diepoxy-2,9-propanonaphtho[1,2-f:5,6-f′]diisoindole-1,3,8,10-tetrone (9CI: a cyclophane derived from naphtho[1,2-c:5,6-c]difuran

    Directory of Open Access Journals (Sweden)

    Peter W. Dibble

    2008-09-01

    Full Text Available The title compound, C25H18N2O6, is a naphthalenophane styled in the manner of Warrener's alicyclic cyclophanes or molecular racks wherein a trimethylene tether is perfectly staggered between the two N atoms such that the central methylene H atoms point toward the naphthalene π-system. The dihedral angle between the mean planes of the two benzene rings is 7.61 (7°.

  3. Design, synthesis and molecular docking study of thienopyrimidin-4(3H-thiones as antifungal agents

    Directory of Open Access Journals (Sweden)

    Sanjay B. Bari

    2017-01-01

    Full Text Available In an attempt to find a new class of antimicrobial agents, a series of thienopyrimidin-4(3H-thiones 4(H1–H36 were synthesized and evaluated for in vitro antifungal activity against Candida albicans (NCIM 3471, Aspergillus niger (NCIM 545, and Penicillium chrysogenum (NCIM 709. The title compounds were synthesized by thionation of thienopyrimidin-4(3H-ones 3(H1–H36 using Lawesson’s reagent. All the compounds were characterized using elemental analytical (C, H, and N and spectral (FT-IR, 1H NMR, 13C NMR and MS data. Among the tested compounds, 5-(4-chlorophenyl-2-(pyridin-3-ylthieno[2,3-d]pyrimidine-4(3H-thione 4(H11, 2-sulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H18, and 2-(butylsulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H32 were identified as potentially excellent antifungal agents. They exhibited potent antifungal activity against C. albicans (MIC; 4 μg/mL, A. niger (MIC; 2 μg/mL, and P. chrysogenum (MIC; 2 μg/mL comparable with that of ketoconazole. The binding mode of compounds by SP docking studies shows that it fits well into the active site cavity of DHFR. Lipinski’s rule and in silico ADME pharmacokinetic parameters are within the acceptable range defined for human use thereby indicating their potential as drug-like molecules.

  4. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    Directory of Open Access Journals (Sweden)

    YuanQi Yu

    2011-10-01

    Full Text Available The asymmetric unit of the title compound, C8H9N2+·C8H5O4−, contains two independent ion pairs. In each 2-methyl-1H-benzimidazolium ion, an intramolecular O—H...O bond forms an S(7 graph-set motif. In the crystal, the components are linked by N—H...O hydrogen bonds, forming chains along [210]. Further stabilization is provided by weak C—H...O hydrogen bonds.

  5. Accurate stereochemistry for two related 22,26-epiminocholestene derivatives

    International Nuclear Information System (INIS)

    Vega-Baez, José Luis; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Montiel-Smith, Sara; Gómez-Calvario, Victor; Bernès, Sylvain

    2008-01-01

    Regioselective opening of ring E of solasodine under various conditions afforded (25R)-22,26-epimino@@cholesta-5,22(N)-di@@ene-3β,16β-diyl diacetate (previously known as 3,16-diacetyl pseudosolasodine B), C 31 H 47 NO 4 , or (22S,25R)-16β-hydr@@oxy-22,26-epimino@@cholesta-5-en-3β-yl acetate (a derivative of the naturally occurring alkaloid oblonginine), C 29 H 47 NO 3 . In both cases, the reactions are carried out with retention of chirality at the C16, C20 and C25 stereogenic centers, which are found to be S, S and R, respectively. Although pseudosolasodine was synthesized 50 years ago, these accurate assignments clarify some controversial points about the actual stereochemistry for these alkaloids. This is of particular importance in the case of oblonginine, since this compound is currently under consideration for the treatment of aphasia arising from apoplexy; the present study defines a diastereoisomerically pure compound for pharmacological studies

  6. What is the best bonding model of the (σ-H-BR) species bound to a transition metal? Bonding analysis in complexes [(H)2Cl(PMe3)2M(σ-H-BR)] (M = Fe, Ru, Os).

    Science.gov (United States)

    Pandey, Krishna K

    2012-03-21

    Density Functional Theory calculations have been performed for the σ-hydroboryl complexes of iron, ruthenium and osmium [(H)(2)Cl(PMe(3))(2)M(σ-H-BR)] (M = Fe, Ru, Os; R = OMe, NMe(2), Ph) at the BP86/TZ2P/ZORA level of theory in order to understand the interactions between metal and HBR ligands. The calculated geometries of the complexes [(H)(2)Cl(PMe(3))(2)Ru(HBNMe(2))], [(H)(2)Cl(PMe(3))(2)Os(HBR)] (R = OMe, NMe(2)) are in excellent agreement with structurally characterized complexes [(H)(2)Cl(P(i)Pr(3))(2)Os(σ-H-BNMe(2))], [(H)(2)Cl(P(i)Pr(3))(2)Os{σ-H-BOCH(2)CH(2)OB(O(2)CH(2)CH(2))}] and [(H)(2)Cl(P(i)Pr(3))(2)Os(σ-H-BNMe(2))]. The longer calculated M-B bond distance in complex [(H)(2)Cl(PMe(3))(2)M(σ-H-BNMe(2))] are due to greater B-N π bonding and as a result, a weaker M-B π-back-bonding. The B-H2 bond distances reveal that (i) iron complexes contain bis(σ-borane) ligand, (ii) ruthenium complexes contain (σ-H-BR) ligands with a stretched B-H2 bond, and (iii) osmium complexes contain hydride (H2) and (σ-H-BR) ligands. The H-BR ligands in osmium complexes are a better trans-directing ligand than the Cl ligand. Values of interaction energy, electrostatic interaction, orbital interaction, and bond dissociation energy for interactions between ionic fragments are very large and may not be consistent with M-(σ-H-BR) bonding. The EDA as well as NBO and AIM analysis suggest that the best bonding model for the M-σ-H-BR interactions in the complexes [(H)(2)Cl(PMe(3))(2)M(σ-H-BR)] is the interaction between neutral fragments [(H)(2)Cl(PMe(3))(2)M] and [σ-H-BR]. This becomes evident from the calculated values for the orbital interactions. The electron configuration of the fragments which is shown for C in Fig. 1 experiences the smallest change upon the M-σ-H-BR bond formation. Since model C also requires the least amount of electronic excitation and geometry changes of all models given by the ΔE(prep) values, it is clearly the most appropriate choice of

  7. Crystal structure of strontium osmate (8) Sr[OsO5(H2O)]x3H2O

    International Nuclear Information System (INIS)

    Nevskij, N.N; Ivanov-Ehmin, B.N.; Nevskaya, N.A.; Belov, N.V.; AN SSSR, Moscow. Inst. Kristallografii)

    1982-01-01

    Crystal structure of the Sr[OsO 5 (H 2 O)]x3H 2 O complex is studied. Rhombic P-cell has the parameters: a=6.426(1), b=7.888(1), c=14.377(5) A, Vsub(c)=729 A 3 . The R-factor equals 0.034. The coordinates of the basis atoms and isotropic temperature corrections, as well as basic interatomic distances, are determined

  8. trans-4-(Phenoxymethylcyclohexanecarboxylic acid

    Directory of Open Access Journals (Sweden)

    Hu Zheng

    2008-04-01

    Full Text Available The title compound, C14H18O3, is an important model compound in the synthesis of phenolic ethers. The cyclohexane ring adopts a chair conformation. In the crystal structure, adjacent molecules are linked by O—H...O hydrogen bonds.

  9. Quantum mechanical and spectroscopic (FT-IR, 13C, 1H NMR and UV) investigations of 2-(5-(4-Chlorophenyl)-3-(pyridin-2-yl)-4,5-dihydropyrazol-1-yl)benzo[d]thiazole by DFT method

    Science.gov (United States)

    Diwaker

    2014-07-01

    The electronic, NMR, vibrational, structural properties of a new pyrazoline derivative: 2-(5-(4-Chlorophenyl)-3-(pyridine-2-yl)-4,5-dihydropyrazol-1-yl)benzo[d]thiazole has been studied using Gaussian 09 software package. Using VEDA 4 program we have reported the PED potential energy distribution of normal mode of vibrations of the title compound. We have also reported the 1H and 13C NMR chemical shifts of the title compound using B3LYP level of theory with 6-311++G(2d,2p) basis set. Using time dependent (TD-DFT) approach electronic properties such as HOMO and LUMO energies, electronic spectrum of the title compound has been studied and reported. NBO analysis and MEP surface mapping has also been calculated and reported using ab initio methods.

  10. Bis(N-ethyl-N-methyl?dithio?carbamato-?2 S,S?)diphenyl?tin(IV)

    OpenAIRE

    Muthalib, Amirah Faizah; Baba, Ibrahim; Ng, Seik Weng

    2010-01-01

    The dithio?carbamate anions in the title compound, [Sn(C6H5)2(C4H8NS2)2], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol?ecule lies across a twofold rotation axis.

  11. Bis(N-isopropyl-N-methyl-dithio-carbamato-κS,S')diphenyl-tin(IV).

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Farina, Yang; Ng, Seik Weng

    2010-03-03

    The dithio-carbamate anions in the title compound, [Sn(C(6)H(5))(2)(C(5)H(10)NS(2))(2)], chelate to the Sn(IV) atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol-ecule lies across a twofold rotation axis.

  12. Bis(N-isopropyl-N-methyl?dithio?carbamato-?2 S,S?)diphenyl?tin(IV)

    OpenAIRE

    Muthalib, Amirah Faizah; Baba, Ibrahim; Farina, Yang; Ng, Seik Weng

    2010-01-01

    The dithio?carbamate anions in the title compound, [Sn(C6H5)2(C5H10NS2)2], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol?ecule lies across a twofold rotation axis.

  13. Bis(N-ethyl-N-methyl-dithio-carbamato-κS,S')diphenyl-tin(IV).

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Ng, Seik Weng

    2010-03-03

    The dithio-carbamate anions in the title compound, [Sn(C(6)H(5))(2)(C(4)H(8)NS(2))(2)], chelate to the Sn(IV) atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol-ecule lies across a twofold rotation axis.

  14. Ethyl 2-[1-(3-methylbutyl-4-phenyl-1H-1,2,3-triazol-5-yl]-2-oxoacetate

    Directory of Open Access Journals (Sweden)

    Muhammad Hafeez

    2013-12-01

    Full Text Available In the title compound, C17H21N3O3, the non-planar (r.m.s. deviation = 0.212 Å ethyl (oxoacetate group is oriented towards the phenyl substituent. The triazole and benzene rings are twisted with respect to each other, making a dihedral angle of 41.69 (6°. In the crystal, molecules are arranged into centrosymmetric R22(10 dimers via pairs of C—H...O interactions involving the ethyl (oxoacetate groups. In addition, the triazole rings show π–π stacking interactions, with their centroids at a distance of 3.745 (2 Å.

  15. 6-Butyl-5-(4-methoxyphenoxy-3-phenyl-3H-1,2,3-triazolo[4,5-d]pyrimidin-7(6H-one

    Directory of Open Access Journals (Sweden)

    Hong-Mei Wang

    2009-12-01

    Full Text Available The asymmetric unit of the title compound, C21H21N5O3, consists of two geometrically similar molecules. The fused rings of the triazolo[4,5-d]pyrimidine system are nearly coplanar, making dihedral angels of 1.48 (18 and 1.34 (16°, and the phenyl rings are twisted by 12.3 (1 and 8.7 (1° with respect to the triazolopyrimidine plane. The ethyl groups of the n-butyl side chains are disordered over two sites in each of the independent molecules, the ratios of occupancies being 0.60:0.40 and 0.61:0.39.

  16. Phase equilibria, phases and compounds in the Ti-C system

    International Nuclear Information System (INIS)

    Gusev, Aleksandr I

    2002-01-01

    The results of experimental and theoretical investigations of the phase equilibria in the titanium-carbon system are generalised. The generalised thermodynamic characteristics of disordered titanium carbide TiC y , are reported. Peculiarities of the crystal structures of all the known and hypothetical compounds of titanium with carbon are considered in detail. The X-ray diffraction patterns which allow identification of all these compounds are presented. The phase diagrams of the Ti-C system constructed with allowance for atomic ordering of non-stoichio metric carbide, TiC y , and for the existence of the molecular cluster-like compounds Ti 8 C 12 and Ti 13 C 22 (TiC 2 ) are discussed. The bibliography includes 142 references.

  17. Phase equilibria, phases and compounds in the Ti-C system

    International Nuclear Information System (INIS)

    Gusev, A.I.

    2002-01-01

    The results of experimental and theoretical investigations related to the phase equilibria in the titanium-carbon system are generalized. The generalized thermodynamic characteristics of the disordered titanium carbide TiC y are given. The crystal structure of all the discovered and hypothetical compounds of titanium with carbon are considered in detail. The x-ray diffraction patterns which allow one to identify all these compounds are given. The phase diagrams of the Ti-C system constructed with allowance for atomic ordering of non-stoichiometric TiC y carbide and for the existence of the compounds Ti 8 C 12 and Ti 13 C 22 (TiC 2 ) of the molecule cluster type are discussed [ru

  18. Redetermination of (2,2′-bipyridine-κ2N,N′dichloridopalladium(II dichloromethane solvate

    Directory of Open Access Journals (Sweden)

    Nam-Ho Kim

    2009-06-01

    Full Text Available In the title compound, [PdCl2(C10H8N2]·CH2Cl2, the Pd2+ ion is four-coordinated in a slightly distorted square-planar environment by two N atoms of the 2,2′-bipyridine (bipy ligand and two chloride ions. The compound displays intramolecular C—H...Cl hydrogen bonds and pairs of complex molecules are connected by intermolecular C—H...Cl hydrogen bonds. Intermolecular π–π interactions are present between the pyridine rings of the ligand, the shortest centroid–centroid distance being 4.096 (3 Å. As a result of the electronic nature of the chelate ring, it is possible to create π–π interactions to its symmetry-related counterpart [3.720 (2 Å] and also with a pyridine ring [3.570 (3 Å] of the bipy unit. The present structure is a redetermination of a previous structure [Vicente et al. (1997. Private communication (refcode PYCXMN02. CCDC, Cambridge, England]. In the new structure refinement all H atoms were located in a difference Fourier synthesis. Their coordinates were refined freely, together with isotropic displacement parameters.

  19. Synthesis, crystal structure, thermal analysis and dielectric properties of [(C{sub 4}H{sub 9}){sub 4}N]{sub 3}Bi{sub 2}Cl{sub 9} compound

    Energy Technology Data Exchange (ETDEWEB)

    Trigui, W., E-mail: walatrigui@yahoo.fr; Oueslati, A.; Chaabane, I.; Hlel, F.

    2015-07-15

    A new organic–inorganic tri-tetrabutylammonium nonachlorobibismuthate(III) compound was prepared. It was found to crystallize in the monoclinic system (P2{sub 1}/n space group) with the following lattice parameters: a=11.32(2) Å, b=22.30(3) Å, c=28.53(2) Å and β=96.52(0)°. The [Bi{sub 2}Cl{sub 9}]{sup 3−} anions are surrounded by six [(C{sub 4}H{sub 9})N]{sup +} cations, forming an octahedral configuration. These octahedra are sharing corners in order to provide the tri-dimensional network cohesion. The differential scanning calorimetry reveals four order-disorder reversible phase transitions located at 214, 238, 434 and 477 K. The Raman and infrared spectra confirm the presence of both cationic [(C{sub 4}H{sub 9})N]{sup +} and anionic [Bi{sub 2}Cl{sub 9}]{sup 3−} parts. The dielectric parameters, real and imaginary dielectric permittivity (ε′ and ε″), and dielectric loss tangent (tg δ), were measured in the frequency range of 209 kHz–5 MHz at different temperatures. The variations of dielectric dispersion (ε') and dielectric absorption (ε″) with frequency show a distribution of relaxation times, which is probably related to the change in the dynamical state of the [(C{sub 4}H{sub 9}){sub 4}N]{sup +} cations and the [Bi{sub 2}Cl{sub 9}]{sup 3−} anions. - Graphical abstract: Projection of the atomic arrangement of the [(C{sub 4}H{sub 9}){sub 4}N]{sub 3}Bi{sub 2}Cl{sub 9} compound along the b axis. - Highlights: • The structure of the (TBA){sub 3}Bi{sub 2}Cl{sub 9} compound was solved and reported. • The cristal belongs to the monoclinic system with P2{sub 1}/n space group. • DSC discloses four order–disorder reversible phases transitions. • The temperature-dependent permittivity ε' and ε″ has been investigated.

  20. N,N′-Bis(2-hydroxy-3-ethoxybenzylidenebutane-1,4-diamine

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2009-04-01

    Full Text Available The title Schiff base compound, C22H28N2O4, lies across a crystallographic inversion centre and adopts an E configuration with respect to the C=N bond. Pairs of weak intermolecular C—H...O interactions link neighbouring molecules into dimers with an R22(28 ring motif. The crystal structure is stabilized by intermolecular C—H...π interactions. An intramolecular O—H...N hydrogen bond occurs.

  1. Ethyl 27-oxo-15-oxa-2,20-diazahexacyclo[18.6.1.01,8.02,6.09,14.021,26]heptacosa-9,11,13,21,23,25-hexaene-7-carboxylate

    Directory of Open Access Journals (Sweden)

    Devadasan Velmurugan

    2013-01-01

    Full Text Available In the title compound, C27H30N2O4, the pyrrolidine ring adopts a twisted conformation. The indoline ring system is almost perpendicular to the mean plane of the pyrrolidine ring, making a dihedral angle of 81.7 (8°. In the crystal, molecules are linked into centrosymmetric dimers with graph-set motif R22(16 via pairs of C—H...O hydrogen bonds. The terminal ethyl group of the ester group is disordered over two sets of sites, with a site-occupancy ratio of 0.587 (11:0.413 (11.

  2. Rh(III)-Catalyzed C-H Activation of Benzoylacetonitriles and Tandem Cyclization with Diazo Compounds to Substituted Benzo[ de]chromenes.

    Science.gov (United States)

    Fang, Feifei; Zhang, Chunmei; Zhou, Chaofan; Li, Yazhou; Zhou, Yu; Liu, Hong

    2018-04-06

    Rh (III)-catalyzed C-H activation of benzoylacetonitriles in coupling with diazo compounds was developed to synthesize diversified substituted benzo[ de]chromenes via a formal (4 + 2) cycloaddition with a diazo compound and subsequent tandem (4 + 2) cycloaddition with another diazo compound. Intriguingly, synthesis of substituted benzo[ de]chromenes and their decarboxylation products could be realized by controlling the reaction conditions. These reactions have a broad range of substrates, moderate to good yields, and high regioselectivity.

  3. Tris(O-cyclo-hexyl dithio-carbonato-κS)anti-mony(III).

    Science.gov (United States)

    Li, Wenkuan; Yin, Handong; Wen, Liyuan; Wang, Daqi

    2008-12-10

    In the mol-ecule of the title compound, [Sb(C(7)H(11)OS(2))(3)], the anti-mony(III) is coordinated by the S atoms of three O-alkyl xanthate groups acting as monodentate ligands, forming a distorted trigonal-pyramidal coordination.

  4. Tris(O-cyclohexyl dithiocarbonato-κSantimony(III

    Directory of Open Access Journals (Sweden)

    Wenkuan Li

    2009-01-01

    Full Text Available In the molecule of the title compound, [Sb(C7H11OS23], the antimony(III is coordinated by the S atoms of three O-alkyl xanthate groups acting as monodentate ligands, forming a distorted trigonal-pyramidal coordination.

  5. SYNTHESIS AND STRUCTURAL CHARACTERISTICS OF BIS(CITRATEGERMANATES(IV (Hbipy2[Ge(HCit2]•2H2O AND [CuCl(bipy2]2[Ge(HCit2]•8H2O

    Directory of Open Access Journals (Sweden)

    Inna Seifullina

    2016-12-01

    Full Text Available The crystalline compounds (Hbipy2[Ge(HCit2]·2H2O (1 and CuCl(bipy2]2[Ge(HCit2]·8H2O (2 (where H4Cit is citric acid, bipy is 2,2ʹ-bipyridine were obtained for the fi rst time and their structures were determined by the single-crystal X-ray diffraction method. Compounds were characterized by IR spectroscopy, thermogravimetric (TGA and elemental analyses. Both compounds are formed with complex bis(citrategermanate anion and protonated 2,2’-bipyridine or [Cu(bipy2Cl]+ as cations in compounds 1 and 2, respectively.

  6. 7-Diethylamino-2-oxo-2H-chromene-3-carbohydrazide

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    Li-Jun Zhang

    2011-05-01

    Full Text Available The asymmetric unit of the title compound, C14H17N3O3, contains two independent molecules with different conformations of the ethyl groups. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into ribbons extending along the a axis.

  7. 2-Methyl-1,10b-dihydro-5H-pyrazolo[1,5-c][1,3]benzoxazin-5-one

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    Jan Světlík

    2009-05-01

    Full Text Available In the title compound, C11H10N2O2, a potential inhibitor of the cyclooxygenase-2 isoenzyme, the pyrazoline ring exists in a flat-envelope conformation while the puckering of the central oxazine ring is more severe. As a result, the molecule as a whole is non-planar. The formal sp3 pyrazoline N atom is sp2 hybridized, with the lone-pair electrons delocalized through conjugation with the carbonyl group rather than the double bond of the pyrazoline ring.

  8. 2-(2-Hydroxy-3-methoxyphenyl-1H-benzimidazol-3-ium perchlorate

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    Chuan Chen

    2012-06-01

    Full Text Available In the title molecular salt, C14H13N2O2+·ClO4−, the ring systems in the cation are almost coplanar [dihedral angle = 5.53 (13°]. Intramolecular N—H...O and O—H...O hydrogen bonds generate S(6 and S(5 rings, respectively. In the crystal, the two H atoms involved in the intramolecular hydrogen bonds also participate in intermolecular links to acceptor O atoms of the perchlorate anions. A simple intermolecular N—H...O bond also occurs. Together, these form a double-chain structure along [101].

  9. Vantagens e desvantagens das colunas C18 e C30 para a separação de carotenóides por CLAE Advantages and disadvantages of C18 and C30 columns for HPLC separation of carotenoids

    Directory of Open Access Journals (Sweden)

    Itaciara Larroza Nunes

    2006-12-01

    Full Text Available Estudos têm demonstrado uma alta associação entre ingestão ou nível plasmático de carotenóides e a diminuição do risco ou proteção contra algumas doenças. Estes fatos, bem como a elevada suscetibilidade destes compostos à luz e calor, com formação de isômeros cis, os quais apresentam menor atividade biológica, torna importante o desenvolvimento de sistemas que permitam a separação destes carotenóides em alimentos. Neste trabalho foi avaliada a separação de isômeros geométricos de licopeno, e dos isômeros de posição luteína e zeaxantina, por cromatografia líquida de alta eficiência (CLAE, utilizando colunas C18 (monomérica, 4 mm, 300 x 3,9 mm e C30 (polimérica, 3 mm, 250 x 4,6 mm e diferentes fases móveis, tanto com eluição isocrática como com gradiente. Os carotenóides foram identificados através das características espectrais e co-cromatografia com padrões. As melhores condições cromatográficas foram obtidas em coluna C30 com temperatura de 33 ºC, eluição isocrática a 1 mL/min e fase móvel com metanol (0,1% trietilamina/éter metil-terc-butílico (50:50 para separar isômeros de licopeno e (95:5 para luteína e zeaxantina. Entretanto, para análise quantitativa, é necessário verificar a repetibilidade da área dos picos na coluna C30. Além disso, a coluna C18 monomérica pode ser empregada para separar luteína e zeaxantina.Several studies have demonstrated a high association between dietary intake or plasma levels of carotenoids and the decrease of risk or the protection against some diseases. Taking this into consideration, as well as the high susceptibility of these compounds to light and heat, leading to the formation of cis isomers with lower biological activity, it is important to develop systems that allow the separation of such compounds in foods. This work evaluated the separation of the geometric isomers of lycopene and of the position isomers, lutein and zeaxanthin, by high

  10. Electrochemical Cobalt-Catalyzed C-H Activation.

    Science.gov (United States)

    Sauermann, Nicolas; Meyer, Tjark H; Ackermann, Lutz

    2018-06-19

    Carbon-heteroatom bonds represent omnipresent structural motifs of the vast majority of functionalized materials and bioactive compounds. C-H activation has emerged as arguably the most efficient strategy to construct C-Het bonds. Despite of major advances, these C-H transformations were largely dominated by precious transition metal catalysts, in combination with stoichiometric, toxic metal oxidants. Herein, we discuss the recent evolution of cobalt-catalyzed C-H activations that enable C-Het formations with electricity as the sole sustainable oxidant until May 2018. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Development and optimization of methods for the radiofluorination of aromatic compounds with specific, high fluorine-18 activity

    International Nuclear Information System (INIS)

    Franken, K.

    1987-06-01

    The positron emitter fluorine-18 (T 1/2 = 110 min) is an ideal radionuclide for analogue tracers in positron emission tomography (PET). In this study the production of the electrophilic species [ 18 F]-F 2 , [ 18 F]-CH 3 CO 2 F and to some extent [ 18 F]-XeF 2 has been optimized with respect to yield and specific activity. Selectivity and reactivity of these species have been studied in simple aromatic model compounds. Fluorine was produced via the 20 Ne(d,α) 18 F reaction. The effect of target material, dimensions, amount of carrier (F 2 ), pressure, beam current and irradiation time was studied. Reactivity of [ 18 F]-F 2 and [ 18 F]-CH 3 CO 2 F with respect to hydrogen subsitution was systematically studied in a series of benzene derivatives (C 6 H 5 X, X = CF 3 , I, Br, CL, F, H, CH 3 , OCH 3 , OH) in various solvents (CHCl 3 , CFCl 3 , CH 3 CN, CH 3 OH, CF 3 COOH). The radiochemical yield of 18 F-for-H-substitution in the aromatic ring increased with increasing acceptor number (AN) of the solvent. The electrophilic nature of both fluorination agents was confirmed by a Hammett plot. As expected, [ 18 F]-CH 3 CO 2 F showed a higher selectivity than [ 18 F]-F 2 . Direct radiofluorination with [ 18 F]-F 2 and [ 18 F]-CH 3 CO 2 F was successfully applied to the biomolecules phenylalanine, tyrosine and DOPA. As potential methods for no-carrier-added (n.c.a.) radiofluorination some less common dediazoniation reactions were also studied. (orig./RB) [de

  12. Multiple C-H Bond Activations and Ring-Opening C-S Bond Cleavage of Thiophene by Dirhenium Carbonyl Complexes.

    Science.gov (United States)

    Adams, Richard D; Dhull, Poonam; Tedder, Jonathan D

    2018-06-14

    The reaction of Re 2 (CO) 8 (μ-C 6 H 5 )(μ-H) (1) with thiophene in CH 2 Cl 2 at 40 °C yielded the new compound Re 2 (CO) 8 (μ-η 2 -SC 4 H 3 )(μ-H) (2), which contains a bridging σ-π-coordinated thienyl ligand formed by the activation of the C-H bond at the 2 position of the thiophene. Compound 2 exhibits dynamical activity on the NMR time scale involving rearrangements of the bridging thienyl ligand. The reaction of compound 2 with a second 1 equiv of 1 at 45 °C yielded the doubly metalated product [Re 2 (CO) 8 (μ-H)] 2 (μ-η 2 -2,3-μ-η 2 -4,5-C 4 H 2 S) (3), formed by the activation of the C-H bond at the 5 position of the thienyl ligand in 2. Heating 3 in a hexane solvent to reflux transformed it into the ring-opened compound Re(CO) 4 [μ-η 5 -η 2 -SCC(H)C(H)C(H)][Re(CO) 3 ][Re 2 (CO) 8 (μ-H)] (4) by the loss of one CO ligand. Compound 4 contains a doubly metalated 1-thiapentadienyl ligand formed by the cleavage of one of the C-S bonds. When heated to reflux (125 °C) in an octane solvent in the presence of H 2 O, the new compound Re(CO) 4 [η 5 -μ-η 2 -SC(H)C(H)C(H)C(H)]Re(CO) 3 (5) was obtained by cleavage of the Re 2 (CO) 8 (μ-H) group from 4 with formation of the known coproduct [Re(CO) 3 (μ 3 -OH)] 4 . All new products were characterized by single-crystal X-ray diffraction analyses.

  13. X-ray diffraction, vibrational and photoluminescence studies of the self-organized quantum well crystal H3N(CH2)6NH3PbBr4

    International Nuclear Information System (INIS)

    Dammak, T.; Fourati, N.; Boughzala, H.; Mlayah, A.; Abid, Y.

    2007-01-01

    We have prepared new semiconductor H 3 N(CH 2 ) 6 NH 3 PbBr 4 crystals which are self-assembled organic-inorganic hybrid materials. The grown crystals have been studied by X-ray diffraction, infrared absorption and Raman spectroscopy scattering. We found that the title compound, abbreviated 2C 6 PbBr 4 , crystallizes in a two-dimensional (2D) structure with a P2 1 /a space group. In the inorganic semiconductor sub-lattice, the corner sharing PbBr 6 octahedra form infinite 2D chains. The organic C 6 H 18 N 2 + ions form the insulator barriers between the inorganic semiconductor layers. Such a packing leads to a self-assembled multiple quantum well structure. Raman and infrared spectra of the title compound were recorded in the 50-500 and 400-4000 cm -1 frequency regions, respectively. The assignment of the observed Raman lines was performed by comparison with the homologous compounds. Transmission measurements on thin films of 2C 6 PbBr 4 , obtained by the spin coating method, revealed a strong absorption peak at 380 nm. Luminescence measurements showed an emission line at 402 nm associated with radiative recombinations of excitons confined within the PbBr 6 layers. The electron-hole binding energy is estimated at 180 meV

  14. Crystal structure, Hirshfeld surface analysis, quantum mechanical study and spectroscopic characterization of the non-centrosymmetric coordination compound bis(4-fluoroaniline)dichloridozincate

    Science.gov (United States)

    Ben Nasr, M.; Soudani, S.; Lefebvre, F.; Jelsch, C.; Ben Nasr, C.

    2017-06-01

    The Zn(II) complex with the monodentate ligand 4-fluoroaniline, ZnCl2(C6H4FNH2)2, has been prepared and characterized by single crystal X-ray diffraction, solid state nuclear magnetic resonance, infrared spectroscopy and differential scanning calorimetry. The Zn(II) ion is tetracoordinated by two nitrogen atoms of two monodentate 4-fluoroaniline ligands and two chlorine atoms. In the molecular arrangement, the ZnCl2(C6H4FNH2)2 entities are interconnected via Nsbnd H⋯Cl hydrogen bonds to form layers parallel to the (a, b) plane. The nature and proportion of contacts in the crystal packing were investigated through the Hirshfeld surfaces. The crystal is mainly maintained by electrostatic attractions Cl- … Hsbnd N and by extensive hydrophobic contacts as revealed by the Hirshfeld 2D fingerprint plots and statistical analysis. The13C and 19F CP-MAS NMR spectra are in agreement with the X-ray structure and confirm the phase purity of the crystalline sample. The vibrational absorption bands were identified by infrared spectroscopy. A calorimetric study shows that the title compound is stable until 262.5 °C.

  15. Di-tert-butyl 2,2′-(biphenyl-2,2′-diyldioxydiacetate

    Directory of Open Access Journals (Sweden)

    Qamar Ali

    2008-08-01

    Full Text Available The title compound, C24H30O6, does not exhibit π–π interactions due to the steric effect of the bulky tert-butyl groups present in the molecule. The presence of these groups at the 2 and 2′ positions hinders the free motion of the benzene rings relative to each other, causing them to adopt an antiperiplanar arrangement. The benzene rings are twisted by just under 50.96 (17° with respect to each other. The carbonyl groups within the molecule are directed in different directions, one towards the biphenyl group and the other away from it. The molecules are linked together by C=O...H—C hydrogen bonds.

  16. Crystal structure of cis-anti-cis-dicyclohexane-18-crown-6 acetonitrile disolvate

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    Alexander Nazarenko

    2015-07-01

    Full Text Available The title compound (systematic name: cis-anti-cis-2,5,8,15,18,21-hexaoxatricyclo[20.4.0.09,14]hexacosane acetonitrile disolvate, C20H36O6·2CH3CN, crystallizes from an acetonitrile solution of dicyclohexane-18-crown-6 on evaporation. The molecule is arranged around a center of symmetry with half the crown ether molecule and one molecule of acetonitrile symmetry independent. All O—C—C—O torsion angles are gauche while all C—O—C—C angles are trans. The sequence of torsion angles is [(tg+t(tg−t]3; the geometry of oxygen atoms is close to pseudo-D3d with three atoms below and three atoms above the mean plane, with an average deviation of ±0.16 (1 Å from the mean plane. This geometry is identical to that observed in metal ion complexes of dicyclohexane-18-crown-6 but differs significantly from the conformation of a free unsolvated molecule. Each acetonitrile molecule connects to a crown ether molecule via two of its methyl group H atoms (C—H...O. Weaker interactions exist between the third H atom of the acetonitrile methyl group and an O atom of a neighbouring crown ether molecule (C—H...O; and between the N atom of the acetonitrile molecule and a H atom of another neighbouring crown ether molecule. All these intermolecular interactions create a three-dimensional network stabilizing the disolvate.

  17. Synthesis, vibrational and optical properties of a new three-layered organic-inorganic perovskite (C4H9NH3)4Pb3I4Br6

    International Nuclear Information System (INIS)

    Dammak, T.; Elleuch, S.; Bougzhala, H.; Mlayah, A.; Chtourou, R.; Abid, Y.

    2009-01-01

    An organic-inorganic hybrid perovskite (C 4 H 9 NH 3 ) 4 Pb 3 I 4 Br 6 was synthesized and studied by X-ray diffraction, Raman and infrared spectroscopies, optical transmission and photoluminescence. The title compound, abbreviated (C 4 ) 4 Pb 3 I 4 Br 6 , crystallises in a periodic two-dimensional multilayer structure with P2 1 /a space group. The structure is built up from alternating inorganic and organic layers. Each inorganic layer consists of three sheets of PbX 6 (X=I, Br) octahedra. Raman and infrared spectra of the title compound were recorded in the 100-3500 and 400-4000 cm -1 frequency ranges, respectively. An assignment of the observed vibration modes is reported. Optical transmission measurements, performed on thin films of (C 4 ) 4 Pb 3 I 4 Br 6 , revealed two absorption bands at 474 and 508 nm. Photoluminescence measurements have shown a green emission peak at 519 nm.

  18. meso-4,4′-Dimethoxy-2,2′-{[(3aR,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-benzimidazole-1,3-diyl]bis(methylene}diphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2013-07-01

    Full Text Available The title compound, C23H30N2O4, a di-Mannich base derived from 4-methoxyphenol and cis-1,2-diaminecyclohexane, has a perhydrobenzimidazolidine nucleus, in which the cyclohexane ring adopts a chair conformation and the heterocyclic ring has a half-chair conformation with a C—N—C—C torsion angles of −48.14 (15 and −14.57 (16°. The mean plane of the heterocycle makes dihedral angles of 86.29 (6 and 78.92 (6° with the pendant benzene rings. The molecular structure of the title compound shows the presence of two interactions between the N atoms of the imidazolidine ring and the hydroxyl groups through intramolecular O—H...N hydrogen bonds with graph-set motif S(6. The unobserved lone pairs of the N atoms are presumed to be disposed in a syn conformation, being only the second example of an exception to the typical `rabbit-ears' effect in 1,2-diamines.

  19. 1-[(1-Methyl-1H-imidazol-5-ylmethyl]-1H-indole-5-carbonitrile

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    Josephus Jacobus de Jager

    2012-12-01

    Full Text Available In the title compound, C14H12N4, the dihedral angle between the indole ring system (r.m.s. deviation = 0.010 Å and the imidazole ring is 77.70 (6°. In the crystal, molecules are linked by C—H...N hydrogen bonds. One set of hydrogen bonds forms an undulating chain running parallel to the b-axis direction, while the other undulating chain is parallel to the c-axis direction. In combination, (100 sheets result.

  20. A one-dimensional polymeric cobalt(III–potassium complex with 18-crown-6, cyanide and porphyrinate ligands

    Directory of Open Access Journals (Sweden)

    Yassine Belghith

    2014-03-01

    Full Text Available The reaction of CoII(TpivPP {TpivPP is the dianion of 5,10,15,20-tetrakis[2-(2,2-dimethylpropanamidophenyl]porphyrin} with an excess of KCN salts and an excess of the 18-crown-6 in chlorobenzene leads to the polymeric title compound catena-poly[[dicyanido-2κ2C-(1,4,7,10,13,16-hexaoxacyclooctadecane-1κ6O{μ3-(2α,2β-5,10,15,20-tetrakis[2-(2,2-dimethylpropanamidophenyl]porphyrinato-1κO5:2κ4N,N′,N′′,N′′′:1′κO15}cobalt(IIIpotassium] dihydrate], {[CoK(CN2(C12H24O6(C64H64N8O4]·2H2O}n. The CoIII ion lies on an inversion center, and the asymmetric unit contains one half of a [CoIII(2α,2β-TpivPP(CN2]− ion complex and one half of a [K(18-C-6]+ counter-ion (18-C-6 is 1,4,7,10,13,16-hexaoxacyclooctadecane, where the KI ion lies on an inversion center. The CoIII ion is hexacoordinated by two C-bonded axial cyanide ligands and the four pyrrole N atoms of the porphyrin ligand. The KI ion is chelated by the six O atoms of the 18-crown-6 molecule and is further coordinated by two O atoms of pivalamido groups of the porphyrin ligands, leading to the formation of polymeric chains running along [011]. In the crystal, the polymeric chains and the lattice water molecules are linked by N—H...O and O—H...N hydrogen bonds, as well as weak C—H...O, O—H...π and C—H...π interactions into a three-dimensional supramolecular architecture.

  1. Crystal structure of chlorido(2-{[2-(phenylcarbamothioylhydrazin-1-ylidene](pyridin-2-ylmethyl}pyridin-1-iumgold(I chloride sesquihydrate

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    Claudia C. Gatto

    2015-09-01

    Full Text Available The title complex, [AuCl(C18H16N5S]Cl·1.5H2O, may be considered as a gold(I compound with the corresponding metal site coordinated by a thiosemicarbazone ligand through the S atom. The ligand adopts an E conformation and the gold(I atom displays the expected linear geometry with a Cl atom also bonded to the metal ion [Cl—Au—S = 174.23 (5°]. One of the pyridyl rings is protonated, giving the gold complex an overall positive charge. Two solvent water molecules, one of which is located on a twofold rotation axis, and a non-coordinating chloride ion complete the structural assembly. The molecular structure is stabilized by intramolecular and intermolecular N—H...Cl, N—H...N, O—H...Cl and O—H...O hydrogen bonding.

  2. {1-[(3,5-Dimethyl-4H-1,2,4-triazol-4-ylimino]ethyl}ferrocene

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    Mao-Ping Song

    2008-10-01

    Full Text Available In the title compound, [Fe(C5H5(C11H13N4], the triazolyl and Cp ring form a dihedral angle of 76.6 (3°. In the crystal structure, there are both intra- and intermolecular C—H...π interactions, forming a one-dimensional chain structure along [010].

  3. 2,7-Bis(trichloromethyl-1,8-naphthyridineThis paper is dedicated to His Majesty King Bhumibol Adulyadej of Thailand (King Rama IX for his sustainable development of the country.

    Directory of Open Access Journals (Sweden)

    Shyamaprosad Goswami

    2010-03-01

    Full Text Available The complete molecule of the title compound, C10H4Cl6N2, is generated by crystallographic twofold symmetry, with two C atoms lying on the rotation axis; the 1,8-naphthyridine ring is almost planar with an r.m.s. deviation of 0.0002 Å. In the crystal structure, the molecules are stacked in an antiparallel manner along [001]. Short Cl...Cl [3.3502 (4] and Cl...N [3.2004 (11–3.2220 (10 Å] contacts are observed in the crystal structure.

  4. 2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12H-6λ5-dibenzo[d,i][1,3,7,2]dioxazaphosphecin-6-thione

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    M. Krishnaiah

    2010-01-01

    Full Text Available In the title compound, C25H28NO2PS, the cyclodecene ring exhibits a crown conformation. The two dimethylbenzene rings which are fused symmetrically on either side of the ten-membered ring, make dihedral angles of 20.2 (1 and 18.0 (1°. The phenyl ring substituted at P is perpendicular to the heterocyclic ring, making a dihedral angle of 88.4 (1°. The crystal structure is stabilized by very weak intramolecular C—H...O hydrogen bonding.

  5. Tris[2-(2H-indazol-2-ylethyl]amine

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    Saúl Ovalle

    2012-06-01

    Full Text Available The title tertiary amine, C27H27N7, a potential tripodal ligand for coordination chemistry, crystallizes with the central N atom located on a threefold axis of a trigonal cell. The gauche conformation of the N(amime—CH2—CH2—N(indazole chain [torsion angle = −64.2 (2°] places the pendant 2H-indazole heterocycles surrounding the symmetry axis, affording a claw-like shaped molecule. Two symmetry-related indazole planes in the molecule make an acute angle of 60.39 (4°. The lone pair of the tertiary N atom is located inside the cavity, and should thus be inactive (as a ligand. In the crystal, neither significant π–π nor C—H...π interactions between molecules are found.

  6. N-(4-Nitrobenzoyl)-N'-(1,5-dimethyl-3-oxo-2-phenyl-1H-3(2H)-pyrazolyl)-thiourea hydrate: Synthesis, spectroscopic characterization, X-ray structure and DFT studies

    Science.gov (United States)

    Arslan, N. Burcu; Kazak, Canan; Aydın, Fatma

    2012-04-01

    The title molecule (C19H17N5O4S·H2O) was synthesized and characterized by IR-NMR spectroscopy, MS and single-crystal X-ray diffraction. The molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the compound in the ground state have been calculated by using the density functional theory (DFT) method with 6-31G(d) basis set, and compared with the experimental data. All the assignments of the theoretical frequencies were performed by potential energy distributions using VEDA 4 program. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and 1H and 13C NMR chemical shift values show good agreement with experimental data. To determine conformational flexibility, the molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which was varied from -180° to +180° in steps of 10°. Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and thermodynamic properties of the compound were investigated by theoretical calculations.

  7. Other compounds isolated from Simira glaziovii and the 1H and 13C NMR chemical shift assignments of new 1-epi-castanopsol

    International Nuclear Information System (INIS)

    Araujo, Marcelo F. de; Vieira, Ivo J. Curcino; Braz-Filho, Raimundo; Carvalho, Mario G. de

    2012-01-01

    A new triterpene, 1-epi-castanopsol, besides eleven known compounds: sitosterol, stigmasterol, campesterol, lupeol, lupenone, simirane B, syringaresinol, scopoletin, isofraxidin, 6,7,8-trimethoxycoumarin and harman, were isolated from the wood of Simira glaziovii. The structures of the known compounds were defined by 1D, 2D 1 H, 13 C NMR spectra data analyses and comparison with literature data. The detailed spectral data analyses allowed the definition of the structure of the new 1-epi isomer of castanopsol and performance of 1 H and 13 C NMR chemical shift assignments. (author)

  8. 2-[(2-Chlorobenzylideneamino]-4,5,6,7-tetrahydro-1-benzothiophene-3-carbonitrile

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    Abdullah M. Asiri

    2011-09-01

    Full Text Available In the title compound, C16H13ClN2S, the mean planes fitted through all non-H atoms of the heterocyclic five-membered and the benzene rings are oriented at a dihedral angle of 5.19 (7°. In the crystal, a weak C—H...π interaction occurs, along with weak π–π interactions [cenroid–centroid distance = 3.7698 (11 Å].

  9. Crystal structure of 3-methoxy-2-[5-(naphthalen-1-yl-4,5-dihydro-1H-pyrazol-3-yl]phenol

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    Dongsoo Koh

    2015-11-01

    Full Text Available In the title compound, C20H18N2O2, the central pyrazoline ring has an envelope conformation with the atom substituted by the naphthalene ring as the flap. It bridges a benzene ring and a naphthalene ring system which are almost normal to one another, making a dihedral angle of 82.03 (6 °. There is an intramolecular O—H...N hydrogen bond forming an S(6 ring motif. In the crystal, molecules are linked by pairs of N—H...π interactions, forming inversion dimers. There are also C—H...π interactions present and the dimers are linked via C—H...O hydrogen bonds, forming ribbons propagating along the a-axis direction.

  10. catena-Poly[[[dichloridozinc(II]-μ-1,4-bis(1H-benzimidazol-2-yl-κN3butane] 1,4-bis(1H-benzimidazol-2-ylbutane solvate

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    Yan-Ling Zhou

    2010-01-01

    Full Text Available In the crystal structure of the title coordination polymer/co-crystal, {[ZnCl2(C18H18N4]·C18H18N4}n, the tetrahedrally coordinated ZnII ions are linked by the N-heterocycle into a linear chain. Another N-heterocycle present is not coordinated to the metal atom but interacts with the chain through N—H...N and N—H...Cl hydrogen bonds. The butyl chain of the uncoordinated ligand is disordered over three positions in a 0.511 (4:0.289 (5:0.200 (5 ratio.

  11. 39 CFR 211.1 - Disposition of former title 39, U.S.C.

    Science.gov (United States)

    2010-07-01

    ... 39 Postal Service 1 2010-07-01 2010-07-01 false Disposition of former title 39, U.S.C. 211.1... REGULATIONS § 211.1 Disposition of former title 39, U.S.C. Except as otherwise continued in effect as postal regulations, all provisions of former title 39, U.S.C., which were continued in effect as regulations of the...

  12. Synthesis and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).

    Science.gov (United States)

    Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B

    2016-08-01

    Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms.

  13. One-azabicyclic compounds. 22. Stereochemistry and /sup 13/C NMR spectra of salts of pyrrolizidine and its homologs with protonic acids

    Energy Technology Data Exchange (ETDEWEB)

    Subbotin, O.A.; Skvortsov, I.M.

    1986-06-01

    /sup 13/C NMR spectra were obtained for pyrrolizidinium salts and their homologs and their signals were assigned. With the exception of highly strained cis-3,8-H-cis-5,8-H-3,5-dimethylpyrrolizidine (VI), all the bases studied upon their direct mixing with CF/sub 3/CO/sub 2/H form salts only with cis-fused rings in the cation. Mixtures of salts with cis- and trans-fused pyrrolizidinium fragments are formed upon the reaction of cis-3,8-H-methyl- (III) and cis-3,8-H-cis-5,8-H-3,5-dimethylpyrrolizidine (VI) under conditions close to those for kinetically-controlled amine protonation. The /sup 13/C NMR spectra of the isomeric pyrrolizidinium salts obtained as a result of the absorption of base VI by sulfuric acid were used to evaluate the conformational equilibrium in the starting compound VI. The /sup 13/C NMR chemical shifts of unsubstituted trans-fused pyrrolizidinium salts were predicted.

  14. 4-Bromo-N-(di-n-propyl-carbamothioyl)-benzamide.

    Science.gov (United States)

    Binzet, Gün; Flörke, Ulrich; Külcü, Nevzat; Arslan, Hakan

    2009-02-04

    The synthesis of the title compound, C(14)H(19)BrN(2)OS, involves the reaction of 4-bromo-benzoyl chloride with potassium thio-cyanate in acetone followed by condensation of the resulting 4-bromo-benzoyl isothio-cyanate with di-n-propyl-amine. Typical thio-urea carbonyl and thio-carbonyl double bonds, as well as shortened C-N bonds, are observed in the title compound. The short C-N bond lengths in the centre of the mol-ecule reveal the effects of resonance in this part of the mol-ecule. The asymmetric unit of the title compound contains two crystallographically independent mol-ecules, A and B. There is very little difference between the bond lengths and angles of these mol-ecules. In mol-ecule B, one di-n-propyl group is twisted in a -anti-periplanar conformation with C-C-C-H = -179.1 (3)° and the other adopts a -synclinal conformation with C-C-C-H = -56.7 (4)°; in mol-ecule A the two di-n-propyl groups are twisted in + and -anti-periplanar conformations, with C-C-C-H = -179.9 (3) and 178.2 (3)°, respectively. In the crystal, the mol-ecules are linked into dimeric pairs via pairs of N-H⋯S hydrogen bonds.

  15. Bis(2,2′-bipyridyl-κ2 N,N′)(carbonato-κ2 O,O′)cobalt(III) bromide trihydrate

    Science.gov (United States)

    Ma, Peng-Tao; Wang, Yu-Xia; Zhang, Guo-Qian; Li, Ming-Xue

    2008-01-01

    The title complex, [Co(CO3)(C10H8N2)2]Br·3H2O, is isostructural with the chloride analogue. The six-coordinated octahedral [Co(2,2′-bipy)2CO3]+ cation (2,2′-bipy is 2,2′-bipyrid­yl), bromide ion and water mol­ecules are linked together via O—H⋯Br and O—H⋯O hydrogen bonds, generating a one-dimensional chain. PMID:21200495

  16. A method for hydrogenating and carbonylizing unsaturated compounds in the presence of catalysts based on phosphine and metal complexes

    Energy Technology Data Exchange (ETDEWEB)

    Briggs, J C; Dyer, G

    1982-12-22

    The hydrogenation of unsaturated organic compounds or the attachment to them of CO is accomplished with contact with a synthesis gas in the presence of a stereospecific catalyst (Kt), a compound of a metal of the platinum group (preferably Rhodium, but also Platinum, Palladium, Ruthenium or Iridium) and an asymmetrical bis-phosphine of the formula A-(CH2)n-B, where A and B are phosphine groups. R2P and R'2P or RRhP, where R is an aryl radical, R' is aralkyl, alcarylic or alkyl radical, n = 1 to 10, or an asymmetrical monophosphine of the formula R2-R'P. The complex compound also includes Hydrogen, CO and (or) halogen (preferably Chlorine) as ligands. The physical properties of the obtained complex compounds of the carbonylchlorbisphosphines or Rh are presented: trans-(RhC1-(CO)(Ph2P(CH2)6PPh2))2; trans-(RhC1(CO)(C2H5PhP-(CH2)6PPh2))2; trans-(RhC1(CO)(cycloC6H11PhP(CH2)6-PPh2))2; trans-(RhC1(CO)(C2H5PhP(CH2)4PPh2)2; trans-(RhC1(CO)(C2H5PhP(Ch2))2 and PhC1(CO)4(p-C6H4CH2)2P(Ch2)6PPh2). The isolated complexes are light yellow crystalline substances.

  17. Characterizing the Solvated Structure of Photoexcited [Os(terpy2]2+ with X-ray Transient Absorption Spectroscopy and DFT Calculations

    Directory of Open Access Journals (Sweden)

    Xiaoyi Zhang

    2016-02-01

    Full Text Available Characterizing the geometric and electronic structures of individual photoexcited dye molecules in solution is an important step towards understanding the interfacial properties of photo-active electrodes. The broad family of “red sensitizers” based on osmium(II polypyridyl compounds often undergoes small photo-induced structural changes which are challenging to characterize. In this work, X-ray transient absorption spectroscopy with picosecond temporal resolution is employed to determine the geometric and electronic structures of the photoexcited triplet state of [Os(terpy2]2+ (terpy: 2,2′:6′,2″-terpyridine solvated in methanol. From the EXAFS analysis, the structural changes can be characterized by a slight overall expansion of the first coordination shell [OsN6]. DFT calculations supports the XTA results. They also provide additional information about the nature of the molecular orbitals that contribute to the optical spectrum (with TD-DFT and the near-edge region of the X-ray spectra.

  18. 2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide

    Directory of Open Access Journals (Sweden)

    B. Narayana

    2013-01-01

    Full Text Available In the crystal structure of the title compound, C19H17Cl2N3O2, the molecules form dimers of the R22(10 type through N—H...O hydrogen bonding. As a result of steric repulsion, the amide group is rotated with respect to both the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 80.70 (13 and 64.82 (12°, respectively. The dihedral angle between the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings is 48.45 (5° while that between the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings is 56.33 (6°.

  19. Bis(N-ethyl-N-methyl­dithio­carbamato-κ2 S,S′)diphenyl­tin(IV)

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Ng, Seik Weng

    2010-01-01

    The dithio­carbamate anions in the title compound, [Sn(C6H5)2(C4H8NS2)2], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol­ecule lies across a twofold rotation axis. PMID:21580470

  20. Bis(N-isopropyl-N-methyl­dithio­carbamato-κ2 S,S′)diphenyl­tin(IV)

    Science.gov (United States)

    Muthalib, Amirah Faizah; Baba, Ibrahim; Farina, Yang; Ng, Seik Weng

    2010-01-01

    The dithio­carbamate anions in the title compound, [Sn(C6H5)2(C5H10NS2)2], chelate to the SnIV atom, which is six-coordinated in a skew-trapezoidal-bipyramidal geometry. The mol­ecule lies across a twofold rotation axis. PMID:21580469

  1. 2-Methoxy-4-(prop-2-en-1-ylphenyl 4-methoxybenzoate

    Directory of Open Access Journals (Sweden)

    Mallikarjuna Rao Pichika

    2013-06-01

    Full Text Available In the title compound, C18H18O4, the planes of the benzene rings are twisted by 81.60 (5°. In the crystal, weak C—H...O hydrogen bonds link the molecules into supramolecular chains extending along the a axis.

  2. 2,2′-Bis{8-[(benzylaminomethylidene]-1,6-dihydroxy-5-isopropyl-3-methylnaphthalen-7(8H-one}

    Directory of Open Access Journals (Sweden)

    Shukhrat M. Hakberdiev

    2013-11-01

    Full Text Available The asymmetric unit of the title compound, C44H44N2O6, contains two independent molecules with similar conformations. The dihydronaphthalene ring systems are approximately planar [maximum deviations = 0.036 (2, 0.128 (2, 0.0.24 (2 and 0.075 (2 Å]. The dihedral angle between two dihydronaphthalene ring systems is 83.37 (4° in one molecule and 88.99 (4° in the other. The carbonyl O atom is linked with the adjacent hydroxy and imino groups via intramolecular O—H...O and N—H...O hydrogen bonds. In the crystal, molecules are linked through O—H...O hydrogen bonds into layers parallel to (001, and adjacent layers are further stacked by π–π interactions between dihydronaphthalene and phenyl rings into a three-dimensional supramolecular architecture. In the crystal, one of the isopropyl groups is disordered over two positions with an occupancy ratio of 0.684 (8:0.316 (8.

  3. Three closely related (2E,2′E-3,3′-(1,4-phenylenebis[1-(methoxyphenylprop-2-en-1-ones]: supramolecular assemblies in one dimension mediated by hydrogen bonding and C—H...π interactions

    Directory of Open Access Journals (Sweden)

    Aijia Sim

    2017-06-01

    Full Text Available In the title compounds, (2E,2′E-3,3′-(1,4-phenylenebis[1-(2-methoxyphenylprop-2-en-1-one], C26H22O4 (I, (2E,2′E-3,3′-(1,4-phenylenebis[1-(3-methoxyphenylprop-2-en-1-one], C26H22O4 (II and (2E,2′E-3,3′-(1,4-phenylenebis[1-(3,4-dimethoxyphenylprop-2-en-1-one], C28H26O6 (III, the asymmetric unit consists of a half-molecule, completed by crystallographic inversion symmetry. The dihedral angles between the central and terminal benzene rings are 56.98 (8, 7.74 (7 and 7.73 (7° for (I, (II and (III, respectively. In the crystal of (I, molecules are linked by pairs of C—H...π interactions into chains running parallel to [101]. The packing for (II and (III, features inversion dimers linked by pairs of C—H...O hydrogen bonds, forming R22(16 and R22(14 ring motifs, respectively, as parts of [201] and [101] chains, respectively.

  4. Carbonyl{3,3′-di-tert-butyl-5,5′-dimethoxy-2,2′-bis[(4,4,5,5-tetramethyl-1,3,2-dioxaphospholan-2-yloxy]biphenyl-κ2P,P′}hydrido(triphenylphosphane-κPrhodium(I diethyl ether trisolvate

    Directory of Open Access Journals (Sweden)

    Detlef Selent

    2013-01-01

    Full Text Available In the title compound, [RhH(C74H68O8P2(C18H15P(CO]·3C4H10O, the CHP3 coordination set at the RhI ion is arranged in a distorted trigonal–bipyramidal geometry with the P atoms adopting equatorial coordination sites and the C atom of the carbonyl ligand as well as the H atom adopting the axial sites. The asymmetric unit contains two very similar molecules of the rhodium complex, two half-occupied diethyl ether molecules and further diethyl ether solvent molecules which could not be modelled successfully. Therefore contributions of the latter were removed from the diffraction data using the SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  5. 2-(4-Methoxy-1H-indol-3-ylacetonitrile

    Directory of Open Access Journals (Sweden)

    Yong-Hong Lu

    2012-01-01

    Full Text Available In the title compound, C11H10N2O, the cyanide group is twisted away from the indole-ring plane [Ccy—Cme—Car—Car = 70.7 (2°; cy = cyanide, me = methylene, ar = aromatic], whereas the methoxy C atom is almost coplanar with the ring system [displacement = 0.014 (5 Å]. In the crystal, N—H...N hydrogen bonds link the molecules into C(7 chains propagating in [100].

  6. 2,2′-(Diselane-1,2-diyldinicotinamide N,N′-dimethylformamide disolvate

    Directory of Open Access Journals (Sweden)

    Aixia Feng

    2010-05-01

    Full Text Available The asymmetric unit of the title compound, C12H10N4O2Se2·2C3H7NO, contains two solvent molecules and two half molecules of the dinicotinamide, each of which sits on a center of symmetry passing through the middle of the Se—Se bond. In each molecule, the two pyridyl groups and diseleno group are approximately coplanar (r.m.s. deviations from planarity for all non-H atoms = 0.011 and 0.008 Å in the two molecules. Intermolecular N—H...O hydrogen bonds stablilize the crystal packing.

  7. (E-3-Methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone

    Directory of Open Access Journals (Sweden)

    Yordanka Ivanova

    2016-04-01

    Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone, was synthesized by Claisen-Schmidt condensation of 3-methyl-2(3H-benzothiazolone-6-carbaldehyde with 2-acetylthiophene in 94% yield. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

  8. N-[7-Ethoxy-1-(prop-2-en-1-yl-1H-indazol-4-yl]-4-methylbenzenesulfonamide

    Directory of Open Access Journals (Sweden)

    Najat Abbassi

    2011-07-01

    Full Text Available In the title compound, C19H21N3O3S, the C—SO2—NH—C torsion angle is 103.72 (11°. The almost planar indazole ring [r.m.s. deviation = 0.0202 (14 Å] is twisted away from the methylbenzene ring by 76.87 (7°. The vinyl group is disordered over two orientations with site occupancies of 0.622 (10 and 0.378 (10. The S atom has a distorted tetrahedral geometry [maximum deviation: O—S—O = 119.18 (11°]. An intramolecular C—H...O hydrogen bond occurs. In the crystal, two molecules are linked about a center of inversion by pairs of N—H...O hydrogen bonds, generating a dimer. C—H...π interactions are also observed.

  9. Novel high pressure hexagonal OsB2 by mechanochemistry

    Science.gov (United States)

    Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

    2014-07-01

    Hexagonal OsB2, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from -225 °C to 1050 °C. The hexagonal OsB2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods.

  10. (R-3-(tert-Butoxycarbonyl-5-methyl-1,2,3-oxathiazolidine 2,2-dioxide

    Directory of Open Access Journals (Sweden)

    Gerhard Laus

    2017-06-01

    Full Text Available The chiral title compound, C8H15NO5S, was obtained by cyclization of (R-1-(tert-butoxycarbonylamino-2-propanol with thionyl chloride and subsequent oxidation with sodium metaperiodate/ruthenium(IV oxide. It crystallizes with two independent molecules in the asymmetric unit. In the crystal, C—H...O interactions link the molecules into a three-dimensional network.

  11. Accurate stereochemistry for two related 22,26-epiminocholestene derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Vega-Baez, José Luis; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Montiel-Smith, Sara; Gómez-Calvario, Victor [Facultad de Ciencias Químicas, Benemérita Universidad Autónoma de Puebla, Ciudad Universitaria, San Manuel, 72000 Puebla, Pue. (Mexico); Bernès, Sylvain, E-mail: sylvain-bernes@hotmail.com [DEP Facultad de Ciencias Químicas, UANL, Guerrero y Progreso S/N, Col. Treviño, 64570 Monterrey, NL (Mexico); Facultad de Ciencias Químicas, Benemérita Universidad Autónoma de Puebla, Ciudad Universitaria, San Manuel, 72000 Puebla, Pue. (Mexico)

    2008-04-01

    Regioselective opening of ring E of solasodine under various conditions afforded (25R)-22,26-epimino@@cholesta-5,22(N)-di@@ene-3β,16β-diyl diacetate (previously known as 3,16-diacetyl pseudosolasodine B), C{sub 31}H{sub 47}NO{sub 4}, or (22S,25R)-16β-hydr@@oxy-22,26-epimino@@cholesta-5-en-3β-yl acetate (a derivative of the naturally occurring alkaloid oblonginine), C{sub 29}H{sub 47}NO{sub 3}. In both cases, the reactions are carried out with retention of chirality at the C16, C20 and C25 stereogenic centers, which are found to be S, S and R, respectively. Although pseudosolasodine was synthesized 50 years ago, these accurate assignments clarify some controversial points about the actual stereochemistry for these alkaloids. This is of particular importance in the case of oblonginine, since this compound is currently under consideration for the treatment of aphasia arising from apoplexy; the present study defines a diastereoisomerically pure compound for pharmacological studies.

  12. 2-(4-Fluoroanilino-3-(2-hydroxyethylquinazolin-4(3H-one

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The molecular and crystal structures of the title compound, C16H14FN3O2, are stabilized by intramolecular N—H...O and intermolecular O—H...O hydrogen bonds. The existence of non-classical intramolecular C—H...N hydrogen bonds provides a dihedral angle between the fluoro-substituted benzene and pyrimidinone rings of 7.9 (1°.

  13. Crystal structure of (E-N-phenyl-N′-[1-(thiophen-2-ylethylidene]formohydrazide

    Directory of Open Access Journals (Sweden)

    C. S. Dileep

    2014-09-01

    Full Text Available In the title compound, C13H12N2OS, the planes of the thiophene and phenyl rings are nearly perpendicular to each other, making a dihedral angle of 86.42 (12°. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a helical chain along the b-axis direction.

  14. Design and syntheses of hybrid metal-organic materials based on K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] metallotectons

    Science.gov (United States)

    Sun, Yayong; Zong, Yingxia; Ma, Haoran; Zhang, Ao; Liu, Kang; Wang, Debao; Wang, Wenqiang; Wang, Lei

    2016-05-01

    By using K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] (C2O42-=oxalate) metallotectons as the starting material, we have synthesized eight novel complexes with formulas [{Fe(C2O4)2(H2O)2}2]·(H-L1)2·H2O 1, [Fe(C2O4)Cl2]·(H2-L2)0.5·(L2)0.5·H2O 2, [{Fe(C2O4)1.5Cl2}2]·(H-L3)43, [Fe2(C2O4)Cl8]·(H2-L4)2·2H2O 4, K[Al(C2O4)3]·(H2-L5)·2H2O 5, K[Al(C2O4)3]·(H-L6)2·2H2O 6, K[Cr(C2O4)3]·2H2O 7, Na[Fe(C2O4)3]·(H-L6)2·2H2O 8 (with L1=4-dimethylaminopyridine, L2=2,3,5,6-tetramethylpyrazine, L3=2-aminobenzimidazole, L4=1,4-bis-(1H-imidazol-1-yl)benzene, L5=1,4-bis((2-methylimidazol-1-yl)methyl)benzene, L6=2-methylbenzimidazole). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra and thermogravimetric analyses. Compound 3 is a 2D H-bonded supramolecular architecture. Others are 3D supramolecular structures. Compound 1 shows a [Fe(C2O4)2(H2O)2]- unit and 3D antionic H-bonded framework. Compound 2 features a [Fe(C2O4)Cl2]- anion and 1D iron-oxalate-iron chain. Compound 3 features a [Fe2(C2O4)3Cl4]4- unit. Compound 4 features distinct [Fe2(C2O4)Cl8]4- units, which are mutual linked by water molecules to generated a 2D H-bonded network. Compound 5 features infinite ladder-like chains constructed by [Al(C2O4)3]3- units and K+ cations. The 1D chains are further extended into 3D antionic H-bonded framework through O-H···O H-bonds. Compounds 6-8 show 2D [KAl(C2O4)3]2- layer, [KCr(C2O4)3]2- layer and [NaFe(C2O4)3]2- layer, respectively.

  15. Converting a C-130 Hercules into a Compound Helicopter: A Conceptual Design Study

    Science.gov (United States)

    Kottapalli, Anjaney P.; Harris, Franklin D.

    2010-01-01

    This study presents the performance and weight changes for a Compound C-130 as compared to the Baseline C-130H Hercules, using NDARC as the primary analysis tool. First, the C-130H was modeled within NDARC, from which performance at various conditions and a parametric weight statement were generated. Then, the C-130H NDARC file was modified to represent the Compound C-130, which was then put through the same performance analysis as the C-130H. A parametric weight statement was also calculated for the Compound C-130, which allowed for comparison to the C-130H. As part of the modeling of the Compound C-130, a Rotor Design Spreadsheet was created that would allow the direct calculation of the weight of the main rotors being added. Using composite materials led to considerable weight savings for both the rotor system and the hub weights. These weight savings are reflected in the NDARC Technology Factors which were determined to be 0.71 and 0.5 for the rotor blades and the hub/hinge system, respectively. Such Technology Factors suggest that using composites for other components could drastically lighten the Operating Empty Weight of the aircraft. The weight statements show the weights for each of the components on each aircraft. It is quite evident that the Compound C-130 has a higher Operating Empty Weight due to the addition of the two main rotors and a drive system to connect each engine group on the wing tips. Upon further analysis, the main weight driver is the drive system. While the main rotor/hub/hinge weight increase is to be expected, the weight increase due to the transmission drive and gear boxes are cause for concern. Unless a method can be found of reducing the weight of the drive system, the weight penalty makes the Compound a C-130 an inefficient aircraft in terms of payload/fuel capacity. Possible solutions are either off-loading some of the power requirements through the drive system or using composite materials in the construction of the drive system

  16. Tris(O-cyclo­hexyl dithio­carbonato-κS)anti­mony(III)

    Science.gov (United States)

    Li, Wenkuan; Yin, Handong; Wen, Liyuan; Wang, Daqi

    2009-01-01

    In the mol­ecule of the title compound, [Sb(C7H11OS2)3], the anti­mony(III) is coordinated by the S atoms of three O-alkyl xanthate groups acting as monodentate ligands, forming a distorted trigonal-pyramidal coordination. PMID:21581504

  17. 2,2'-(Carbono-thio-yldisulfanedi-yl)bis-(2-methyl-propanoic acid).

    Science.gov (United States)

    Moreno-Fuquen, Rodolfo; Grande, Carlos; Advincula, Rigoberto C; Tenorio, Juan C; Ellena, Javier

    2013-05-01

    The mol-ecular structure of the title compound, C9H14O4S3, exhibits intra-molecular C-H⋯S hydrogen bonds. In the crystal, pairs of O-H⋯O hydrogen bonds lead to the formation of centrosymmetric dimers, which are in turn connected by weak C-H⋯O inter-actions. The combination of these inter-actions generates edge-fused R 2 (2)(8) and R 2 (2)(20) rings running along [211].

  18. N-{4-[4-(4-Fluorophenyl-1-(2-methoxyethyl-2-methylsulfanyl-1H-imidazol-5-yl]-2-pyridyl}-2-methyl-3-phenylpropionamide

    Directory of Open Access Journals (Sweden)

    Stefan Laufer

    2009-12-01

    Full Text Available In the crystal structure of the title compound, C28H29FN4O2S, the imidazole ring makes dihedral angles of 11.85 (7, 73.33 (7 and 22.83 (8° with the 4-fluorophenyl, pyridine and phenyl rings, respectively. The 4-fluorophenyl ring makes dihedral angles of 77.91 (7 and 26.93 (8° with the pyridine and phenyl rings, respectively. The phenyl and pyridine rings are nearly perpendicular, making a dihedral angle of 86.47 (9°. The crystal packing shows an intermolecular N—H...O hydrogen-bonding interaction between the N—H and carbonyl groups of the amide functions.

  19. 4,4′-Dimethoxy-2,2′-[(butane-1,4-diyldioxybis(nitrilomethylidyne]diphenol

    Directory of Open Access Journals (Sweden)

    Yin-Xia Sun

    2010-11-01

    Full Text Available The title Schiff base bisoxime compound, C20H24N2O6, lies across an inversion centre and adopts an E configuration with respect to the C=N bond. In the molecule, the oxime group is roughly coplanar with the benzene ring, forming a dihedral angle of 1.77 (2°. An intramolecular O—H...N hydrogen bond forms a six-membered ring with an S(6 motif. Weak intermolecular C—H...O hydrogen bonding is present in the crystal structure.

  20. Bis(5,5-diphenylhydantoinato-κN3(ethylenediaminezinc(II

    Directory of Open Access Journals (Sweden)

    Xilan Hu

    2009-11-01

    Full Text Available In the title compound, [Zn(C15H11N2O22(C2H8N2], the ZnII atom is coordinated in a distorted tetrahedral geometry. Intramolecular N—H...O, C—H...O and C—H...N hydrogen bonds occur. In the crystal, molecules are linked by intermolecular N—H...O hydrogen bonds, forming a three-dimensional network.

  1. Insulators containing CuCl4X22- (X=H2O, NH3) units: Origin of the orthorhombic distortion observed only for CuCl4(H2O)22-

    DEFF Research Database (Denmark)

    García-Fernández, P.; García Lastra, Juan Maria; Trueba, A.

    2012-01-01

    The origin of the difference in structure between compounds containing CuCl4X22- (X=H2O, NH3) units is analyzed by means of first-principles calculations. While NH3-containing compounds display tetragonal symmetry, H2O-containing ones display an orthorhombic distortion at low temperature where...... the equatorial Cl- ions are no longer equivalent. Our simulations of optical and vibrational transitions show good agreement with all available experimental optical absorption and Raman data. As a salient feature, the value of the force constant for the B1g mode, K(B1g), driving the orthorhombic distortion......CuCl4(H2O)2 has a local origin....

  2. Novel high pressure hexagonal OsB2 by mechanochemistry

    International Nuclear Information System (INIS)

    Xie, Zhilin; Graule, Moritz; Orlovskaya, Nina; Andrew Payzant, E.; Cullen, David A.; Blair, Richard G.

    2014-01-01

    Hexagonal OsB 2 , a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB 2 begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB 2 crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB 2 phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from −225 °C to 1050 °C. The hexagonal OsB 2 powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB 2 at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods. - Graphical abstract: High resolution transmission electron micrograph of hexagonal OsB 2 nanocrystallite with corresponding fast Fourier transform and simulated diffraction pattern. - Highlights: • Hexagonal OsB 2 has been synthesized for the first time by mechanochemical method. • Hexagonal OsB 2 crystallizes in P63/mmc space group (No. 194), a=2.916 Å and c=7.376 Å. • The hexagonal structure was confirmed by a transmission electron microscope. • No phase transformation was observed after being annealed at 1050 °C for 6 days. • 20 wt% of h-OsB 2 was transformed to o-OsB 2 after being sintered at 1500 °C for 5 min

  3. Crystal structure of bis-[(acetato-κO)(imidazolidine-2-thione-κS)bis-(tri-phenyl-phosphane-κP)silver(I)] di-μ-imidazol-idine-2-thione-κ(4) S:S-bis-[(imidazol-id-ine-2-thione-κS)bis-(tri-phenyl-phosphane-κP)silver(I)] di-acetate aceto-nitrile disolvate tetra-hydrate.

    Science.gov (United States)

    Nimthong-Roldán, Arunpatcha; Ratthiwan, Janejira; Lakmas, Sawanya; Wattanakanjana, Yupa

    2016-04-01

    In the title compound, [Ag2(C3H6N2S)4(C18H15P)2](C2H3O2)2·[Ag(C2H3O2)(C3H6N2S)(C18H15P)2]2·2C2H3N·4H2O, the Ag(I) ion in the mononuclear neutral complex exhibits a distorted tetra-hedral environment with coordination by two P atoms from tri-phenyl-phosphane (PPh3) ligands, one S atom of an imidazolidine-2-thione (etu) ligand and one O atom of an acetate anion. The binuclear cationic complex comprises two inversion-related [Ag(C3H6N2S)2(C18H15P)] units with Ag(I) ions bridged by two S atoms from etu ligands forming a four-membered Ag-S-Ag-S ring. Each Ag(I) ion is coordinated by a P atom of a PPh3 ligand, two S atoms of bridging etu ligands and the terminal S atom of an etu ligand in a distorted tetra-hedral environment. In the crystal, the mononuclear complex is linked to lattice water mol-ecules through O-H⋯O and N-H⋯O hydrogen bonds, forming a chain along [100]. In addition, the binuclear complex mol-ecules are connected to acetate anions and lattice water mol-ecules via O-H⋯O, N-H⋯O and O-H⋯S hydrogen bonds, also along [100].

  4. N-Cyclohexyl-2-(5-fluoro-1H-indol-3-yl-2-oxoacetamide

    Directory of Open Access Journals (Sweden)

    Dan-Li Tian

    2011-07-01

    Full Text Available In title compound, C16H17FN2O2, the cyclohexane ring adopts a chair conformation.. The crystal packing is stabilized by weak π–π stacking interactions [centroid–centroid distance = 3.503 (5 Å] and intermolecular C—H...O, N—H...O and N—H...F hydrogen-bond interactions.

  5. (Carbonyl-1κC)bis-[2,3(η)-cyclo-penta-dien-yl][μ(3)-(S-methyl trithio-carbonato)methylidyne-1:2:3κC,S'':C:C](triphenyl-phosphine-1κP)(μ(3)-sulfido-1:2:3κS)dicobalt(II)iron(II) trifluoro-methane-sulfonate.

    Science.gov (United States)

    Manning, Anthony R; McAdam, C John; Palmer, Anthony J; Simpson, Jim

    2008-04-10

    The asymmetric unit of the title compound, [FeCo(2)(C(5)H(5))(2)(C(3)H(3)S(3))S(C(18)H(15)P)(CO)]CF(3)SO(3), consists of a triangular irondicobalt cluster cation and a trifluoro-methane-sulfonate anion. In the cation, the FeCo(2) triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithio-carbonate residue that bridges the Fe-C bond. Each Co atom carries a cyclo-penta-dienyl ligand while the Fe atom coordinates to one carbonyl and one triphenyl-phosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C-H⋯O and C-H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) inter-actions. The structure is further stabilized by additional inter-molecular C-H⋯O, C-H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) inter-action (S⋯centroid distance = 3.385 Å), generating an extended network.

  6. (4S)-4-(3,4-Dichloro?phen?yl)-1?-methyl-4?-phenyl-3,4-dihydronaphthalene-2-spiro-3?-pyrrolidine-2?-spiro-1??-acenaphthyl?ene-1,2??(2H,1??H)-dione

    OpenAIRE

    Murugan, R.; Gunasekaran, B.; Narayanan, S. Sriman; Manivannan, V.

    2008-01-01

    In the title compound, C37H27Cl2NO2, the 3,4-dichloro?phenyl ring makes a dihedral angle of 46.66?(6)? with the phenyl ring. The mol?ecular structure is stabilized by weak intra?molecular C?H?O inter?actions and the crystal structure is stabilized by weak inter?molecular C?H?O inter?actions. The C?C?C?C?C five-membered ring is planar, while the C?C?C?C?N five-membered ring adopts a half-chair conformation.

  7. Amyloid imaging in cognitively normal older adults: comparison between {sup 18}F-flutemetamol and {sup 11}C-Pittsburgh compound B

    Energy Technology Data Exchange (ETDEWEB)

    Adamczuk, Katarzyna; Schaeverbeke, Jolien; Neyens, Veerle; Dupont, Patrick [KU Leuven, Laboratory for Cognitive Neurology, Leuven (Belgium); Leuven Institute of Neuroscience and Disease, Alzheimer Research Centre KU Leuven, Leuven (Belgium); Nelissen, Natalie [KU Leuven, Laboratory for Cognitive Neurology, Leuven (Belgium); Oxford University, Department of Psychiatry, Oxford (United Kingdom); Vandenbulcke, Mathieu [University Hospitals Leuven, Old Age Psychiatry Department, Leuven (Belgium); Goffin, Karolien [KU Leuven and University Hospitals Leuven, Nuclear Medicine and Molecular Imaging Department, Leuven (Belgium); Lilja, Johan [GE Healthcare, Uppsala (Sweden); Department of Surgical Sciences, Radiology, Uppsala University Hospital, Uppsala University, Uppsala (Sweden); Hilven, Kelly [KU Leuven, Laboratory for Neuroimmunology, Leuven (Belgium); Laere, Koen van [Leuven Institute of Neuroscience and Disease, Alzheimer Research Centre KU Leuven, Leuven (Belgium); KU Leuven and University Hospitals Leuven, Nuclear Medicine and Molecular Imaging Department, Leuven (Belgium); Vandenberghe, Rik [KU Leuven, Laboratory for Cognitive Neurology, Leuven (Belgium); Leuven Institute of Neuroscience and Disease, Alzheimer Research Centre KU Leuven, Leuven (Belgium); University Hospitals Leuven, Neurology Department, Leuven (Belgium)

    2016-01-15

    Preclinical, or asymptomatic, Alzheimer's disease (AD) refers to the presence of positive AD biomarkers in the absence of cognitive deficits. This research concept is being applied to define target populations for clinical drug development. In a prospective community-recruited cohort of cognitively intact older adults, we compared two amyloid imaging markers within subjects: {sup 18}F-flutemetamol and {sup 11}C-Pittsburgh compound B (PIB). In 32 community-recruited cognitively intact older adults aged between 65 and 80 years, we determined the concordance between binary classification based on {sup 18}F-flutemetamol versus {sup 11}C-PIB according to semiquantitative assessment (standardized uptake value ratio in composite cortical volume, SUVR{sub comp}) and, alternatively, according to visual reads. We also determined the correlation between {sup 18}F-flutemetamol and {sup 11}C-PIB SUVR and evaluated how this was affected by the reference region chosen (cerebellar grey matter versus pons) and the use of partial volume correction (PVC) in this population. Binary classification based on semiquantitative assessment was concordant between {sup 18}F-flutemetamol and {sup 11}C-PIB in 94 % of cases. Concordance of blinded binary visual reads between tracers was 84 %. The Spearman correlation between {sup 18}F-flutemetamol and {sup 11}C-PIB SUVR{sub comp} with cerebellar grey matter as reference region was 0.84, with a slope of 0.98. Correlations in neocortical regions were significantly lower with the pons as reference region. PVC improved the correlation in striatum and medial temporal cortex. For the definition of preclinical AD based on {sup 18}F-flutemetamol, concordance with {sup 11}C-PIB was highest using semiquantitative assessment with cerebellar grey matter as reference region. (orig.)

  8. 18 CFR 420.22 - Prohibition; sanctions.

    Science.gov (United States)

    2010-04-01

    ... 18 Conservation of Power and Water Resources 2 2010-04-01 2010-04-01 false Prohibition; sanctions. 420.22 Section 420.22 Conservation of Power and Water Resources DELAWARE RIVER BASIN COMMISSION... established water pricing schedules of the Commission) of any such use, withdrawal or diversion, and invoke...

  9. Di-tert-butyl 2,2′-[(biphenyl-4,4′-diyldioxy]diacetate

    Directory of Open Access Journals (Sweden)

    Qamar Ali

    2010-07-01

    Full Text Available The complete molecule of the title compound, C24H30O6, is generated by a crystallographic inversion centre. In the unique part of the molecule, the four-atom –O–CH2–C(= O–O– chain between the benzene ring and the tert-butyl group assumes a zigzag conformation [O—C—C—O torsion angle = −162.3 (1°].

  10. 2-(4-Fluorophenyl-2H-chromen-4(3H-one

    Directory of Open Access Journals (Sweden)

    Michał Wera

    2012-02-01

    Full Text Available In the crystal structure of the title compound, C15H11FO2, molecules form inversion dimers through pairs of weak C—H...O hydrogen bonds. Dimers oriented in parallel, linked by C—H...π contacts, are arranged in columns along the b axis. The fluorophenyl ring and the benzene ring of the 2H-chromen-4(3H-one unit are inclined to one another by 70.41 (16°. They are respectively parallel in a given column or almost perpendicular [oriented at an angle of 87.8 (1°] in neighbouring (inversely oriented columns, forming a herringbone pattern.

  11. Ruthenium(II carbonyl compounds with the 4′-chloro-2,2′:6′,2′′-terpyridine ligand

    Directory of Open Access Journals (Sweden)

    Rajendhraprasad Tatikonda

    2017-04-01

    Full Text Available Two ruthenium carbonyl complexes with the 4′-chloro-2,2′:6′,2′′-terpyridine ligand (tpy-Cl, C15H10ClN3, i.e. [RuCl(tpy-Cl(CO2][RuCl3(CO3] (I [systematic name: cis-dicarbonylchlorido(4′-chloro-2,2′:6′,2′′-terpyridine-κ3Nruthenium(II fac-tricarbonyltrichloridoruthenate(II], and [RuCl2(tpy-Cl(CO2] (II [cis-dicarbonyl-trans-dichlorido(4′-chloro-2,2′:6′,2′′-terpyridine-κ2N1,N1′ruthenium(II], were synthesized and characterized by single-crystal X-ray diffraction. The RuII atoms in both centrosymmetric structures (I and (II display similar, slightly distorted octahedral coordination spheres. The coordination sphere in the complex cation in compound (I is defined by three N atoms of the tridentate tpy-Cl ligand, two carbonyl carbon atoms and one chlorido ligand; the charge is balanced by an octahedral [Ru(CO3Cl3]− counter-anion. In the neutral compound (II, the tpy-Cl ligand coordinates to the metal only through two of its N atoms. The coordination sphere of the RuII atom is completed by two carbonyl and two chlorido ligands. In the crystal structures of both (I and (II, weak C—H...Cl interactions are observed.

  12. Crystal structure of 3-methyl-1-phenyl-5-(1H-pyrrol-1-yl-1H-pyrazole-4-carbaldehyde

    Directory of Open Access Journals (Sweden)

    Joel T. Mague

    2014-10-01

    Full Text Available In the title compound, C15H13N3O, the pyrrolyl and phenyl rings make dihedral angles of 58.99 (5 and 34.95 (5°, respectively, with the central pyrazole ring. In the crystal, weak, pairwise C—H...O interactions across centers of symmetry form dimers, which are further associated into corrugated sheets running approximately parallel to (100 via weak C—H...N interactions.

  13. Phosphinodi(benzylsilane) PhP{(o-C6H4CH2)SiMe2H}2: a versatile "PSi2Hx" pincer-type ligand at ruthenium.

    Science.gov (United States)

    Montiel-Palma, Virginia; Muñoz-Hernández, Miguel A; Cuevas-Chávez, Cynthia A; Vendier, Laure; Grellier, Mary; Sabo-Etienne, Sylviane

    2013-09-03

    The synthesis of the new phosphinodi(benzylsilane) compound PhP{(o-C6H4CH2)SiMe2H}2 (1) is achieved in a one-pot reaction from the corresponding phenylbis(o-tolylphosphine). Compound 1 acts as a pincer-type ligand capable of adopting different coordination modes at Ru through different extents of Si-H bond activation as demonstrated by a combination of X-ray diffraction analysis, density functional theory calculations, and multinuclear NMR spectroscopy. Reaction of 1 with RuH2(H2)2(PCy3)2 (2) yields quantitatively [RuH2{[η(2)-(HSiMe2)-CH2-o-C6H4]2PPh}(PCy3)] (3), a complex stabilized by two rare high order ε-agostic Si-H bonds and involved in terminal hydride/η(2)-Si-H exchange processes. A small free energy of reaction (ΔrG298 = +16.9 kJ mol(-1)) was computed for dihydrogen loss from 3 with concomitant formation of the 16-electron species [RuH{[η(2)-(HSiMe2)-CH2-o-C6H4]PPh[CH2-o-C6H4SiMe2]}(PCy3)] (4). Complex 4 features an unprecedented (29)Si NMR decoalescence process. The dehydrogenation process is fully reversible under standard conditions (1 bar, 298 K).

  14. Synthesis and anti-HIV activity of novel 3-substituted phenyl-6,7-dimethoxy-3a,4-dihydro-3H-indeno[1,2-c]isoxazole analogues.

    Science.gov (United States)

    Ali, Mohamed A; Ismail, Rusli; Choon, Tan S; Yoon, Yeong K; Wei, Ang C; Pandian, Suresh; Samy, Jeyabalan G; De Clercq, Eric; Pannecouque, Christophe

    2011-01-01

    A series of novel 3-(substituted phenyl)-6,7-dimethoxy-3a,4-dihydro-3H-indeno[1,2-c]isoxazole analogues were synthesized by the reaction of 5,6-dimethoxy-2-[(E)-1-phenylmethylidene]-1-indanone with hydroxylamine hydrochloride. The title compounds were tested for their in vitro anti-HIV activity. Among the compounds, (4g) showed a promising anti-HIV activity in the in vitro testing against IIIB and ROD strains. The IC50 of both IIIB and ROD were found to be 9.05 microM and > 125 microM, respectively.

  15. 4,4′-Dibromo-2,2′-{[(3aS,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylidene}diphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2011-04-01

    Full Text Available The cyclohexane ring in the title compound, C21H24Br2N2O2, adopts a chair conformation and the five-membered ring to which it is fused has a twisted envelope conformation. The asymmetric unit contains one half-molecule, which is related to the other half by a twofold rotation axis. The two N atoms of the five-membered ring are linked to the hydroxy groups by intramolecular O—H...N hydrogen bonds. In the crystal, intermolecular C—H...O and C—H...π interactions occur.

  16. 2-Aminopyrimidine-3,3,3-triphenylpropanoic acid (1/1).

    Science.gov (United States)

    Serafin, Mateusz F; Wheeler, Kraig A

    2007-11-01

    The title bimolecular compound, C(4)H(5)N(3).C(21)H(18)O(2), constructed from 2-aminopyrimidine and 3,3,3-triphenylpropanoic acid, forms a tetramolecular hydrogen-bonded motif via O-H...N, N-H...O and N-H...N contacts. This aggregate organizes to give crystal-packing motifs with hydrophilic and hydrophobic regions.

  17. 1,6-Bis[(2,2′:6′,2′′-terpyridin-4′-yloxy]hexane

    Directory of Open Access Journals (Sweden)

    Varvara I. Nikolayenko

    2012-07-01

    Full Text Available The molecule of the title compound, C36H32N6O2, lies about an inversion center, located at the mid-point of the central C—C bond of the diether bridge. The terminal pyridine rings form dihedral angles of 4.67 (7 and 26.23 (7° with the central ring. In the crystal, weak C—H...N and C—H...O interactions link the molecules into a three-dimensional network.

  18. 4-[(3-Hydroxyanilino(phenylmethylidene]-3-methyl-1-phenyl-1H-pyrazol-5(4H-one

    Directory of Open Access Journals (Sweden)

    Keraghel Saida

    2012-06-01

    Full Text Available In the title compound, C23H19N3O2, the dihedral angles formed by the pyrazolone ring with the three benzene rings are 30.91 (6, 60.96 (4 and 57.01 (4°. The ligand is in the enamine–keto form and its structure is stabilized by an intramolecular N—H...O hydrogen bond. In the crystal, O—H...N hydrogen bonds link molecules into chains parallel to [01-1].

  19. (Acetonitrile-κNchloridobis[2-(pyridin-2-ylphenyl-κ2C1,N]iridium(III

    Directory of Open Access Journals (Sweden)

    Florian Blasberg

    2011-12-01

    Full Text Available The IrIII atom of the title compound, [Ir(C11H8N2Cl(CH3CN], displays a distorted octahedral coordination. The pyridyl groups are in trans positions [N—Ir—N = 173.07 (10°], while the phenyl groups are trans with respect to the acetonitrile and chloride groups [C—Ir—N = 178.13 (11 and C—Ir—Cl = 176.22 (9°]. The pyridylphenyl groups only show a small deviation from planarity, with the dihedral angle between the planes of the two six-membered rings in each pyridylphenyl group being 5.6 (2 and 5.8 (1°. The crystal packing shows intermolecular C—H...Cl, C—H...π(acetonitrile and C—H...π(pyridylphenyl contacts.

  20. 6-Hydroxymethyl-4-methoxy-2H-pyran-2-one (Opuntiol

    Directory of Open Access Journals (Sweden)

    Muhammad Athar Abbasi

    2010-01-01

    Full Text Available The title compound, C7H8O4, isolated from Opuntia dillenii Haw (Cactaceae, is almost planar [maximum deviation of 0.027 (2 Å] except for the H atoms of the methylene and methyl groups. The crystal packing is stabilized by C—H...O and O—H...O intermolecular hydrogen bonds, resulting in the formation of a three-dimensional network.

  1. 3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H-thione

    Directory of Open Access Journals (Sweden)

    Zbigniew Karczmarzyk

    2013-02-01

    Full Text Available The title compound, C11H13N3S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2:0.23 (2 for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3 Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18 and 86.56 (49° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15° and this conformation is stabilized by an intramolecular C—H...S contact. In the crystal, pairs of N—H...S hydrogen bonds link molecules into inversion dimers. π–π interactions are observed between the triazole and benzene rings, with centroid–centroid separations of 3.547 (4 and 3.544 (12 Å for components A and B, and slippages of 0.49 (6 and 0.58 (15 Å, respectively.

  2. Ethyl 8,13-dioxa-21-azapentacyclo[18.5.1.02,7.014,19.021,25]hexacosa-2(7,3,5,14,16,18-hexaene-26-carboxylate

    Directory of Open Access Journals (Sweden)

    Devadasan Velmurugan

    2013-01-01

    Full Text Available In the title compound, C26H31NO4, the five-membered rings of the central pyrrolizine system adopt N-envelope conformations. The ethyl acetate group adopts an extended conformation. The dihedral angle between the benzene rings is 36.6 (1°. In the crystal, C—H...O hydrogen bonds form a zigzag chain running along the b-axis directions. The crystal structure is futher consolidated by C—H...π interactions.

  3. 20 CFR 410.561c - Defeat the purpose of title IV.

    Science.gov (United States)

    2010-04-01

    ... 20 Employees' Benefits 2 2010-04-01 2010-04-01 false Defeat the purpose of title IV. 410.561c Section 410.561c Employees' Benefits SOCIAL SECURITY ADMINISTRATION FEDERAL COAL MINE HEALTH AND SAFETY..., accident, and health insurance including premiums for supplementary medical insurance benefits under title...

  4. Vitamina C, carotenoides, fenólicos totais e atividade antioxidante de goiaba, manga e mamão procedentes da Ceasa do Estado de Minas Gerais = Vitamin C, carotenoids, phenolic compounds and antioxidant activity of guava, mango and papaya from Ceasa of Minas Gerais State

    Directory of Open Access Journals (Sweden)

    Daniela da Silva Oliveira

    2011-01-01

    Full Text Available Este estudo teve como objetivo analisar o conteudo de compostos antioxidantes (acido ascorbico - AA, acido desidroascorbico - ADA, vitamina C total, licopeno, £]-caroteno, £]-criptoxantina e estimativa de compostos fenolicos e avaliar a atividade antioxidante, em goiaba, manga e mamao. A analise de carotenoides e vitamina C foi realizada por Cromatografia Liquida de Alta Eficiencia (CLAE. O teor de fenolicos totais foi determinado utilizando o reagente de Folin-Ciocalteu e leitura espectrofotometrica. A atividade antioxidante foi avaliada pelo Teste do 2,2-diphenil-2-picril-hidrazil (DPPH¡E e do Poder Redutor. A Anova (ƒÑ = 0,05 foi utilizada para a analise dos dados. Os teores dos constituintes antioxidantes diferiram entre as tres frutas, mas a goiaba foi a fruta que apresentou teores mais elevados de compostos fenolicos, vitamina C total, ADA e licopeno, alem dos maiores valores para atividade antioxidante. Foi constatada forte correlacao entre os testes que avaliaram a atividade antioxidante e o teor de fenolicos totais, demonstrando serem estes os principais compostos antioxidantes a contribuirem para a atividade antioxidante das frutas analisadas, em ambos os testes. E importante incentivar a utilizacao das frutas avaliadas neste estudo, tanto em nivel domestico quanto em estabelecimentos de alimentacao coletiva para aumentar o consumo de antioxidantes naturais pela populacao.This study aimed to analyze the content of antioxidant compounds (ascorbic acid - AA, dehydroascorbic acid - DHA, total vitamin C, lycopene, £]-carotene, £]-cryptoxanthin and phenolic compounds and to evaluate the antioxidant activity in guava, mango and papaya.The analysis of carotenoids and vitamin C was performed by high performance liquid chromatography (HPLC. The content of phenolic compounds was determined using the Folin-Ciocalteu reagent and spectrophotometric reading. Antioxidant activity was evaluated by testing the 2.2-diphenyl-2-picryl

  5. Synthesis and fundamental properties of stable Ph(3)SnSiH(3) and Ph(3)SnGeH(3) hydrides: model compounds for the design of Si-Ge-Sn photonic alloys.

    Science.gov (United States)

    Tice, Jesse B; Chizmeshya, Andrew V G; Groy, Thomas L; Kouvetakis, John

    2009-07-06

    The compounds Ph(3)SnSiH(3) and Ph(3)SnGeH(3) (Ph = C(6)H(5)) have been synthesized as colorless solids containing Sn-MH(3) (M = Si, Ge) moieties that are stable in air despite the presence of multiple and highly reactive Si-H and Ge-H bonds. These molecules are of interest since they represent potential model compounds for the design of new classes of IR semiconductors in the Si-Ge-Sn system. Their unexpected stability and high solubility also makes them a safe, convenient, and potentially useful delivery source of -SiH(3) and -GeH(3) ligands in molecular synthesis. The structure and composition of both compounds has been determined by chemical analysis and a range of spectroscopic methods including multinuclear NMR. Single crystal X-ray structures were determined and indicated that both compounds condense in a Z = 2 triclinic (P1) space group with lattice parameters (a = 9.7754(4) A, b = 9.8008(4) A, c = 10.4093(5) A, alpha = 73.35(10)(o), beta = 65.39(10)(o), gamma = 73.18(10)(o)) for Ph(3)SnSiH(3) and (a = 9.7927(2) A, b = 9.8005(2) A, c = 10.4224(2) A, alpha = 74.01(3)(o), beta = 65.48(3)(o), gamma = 73.43(3)(o)) for Ph(3)SnGeH(3). First principles density functional theory simulations are used to corroborate the molecular structures of Ph(3)SnSiH(3) and Ph(3)SnGeH(3), gain valuable insight into the relative stability of the two compounds, and provide correlations between the Si-Sn and Ge-Sn bonds in the molecules and those in tetrahedral Si-Ge-Sn solids.

  6. 4,4′-Difluoro-2,2′-{[(3aRS,7aRS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylene]}diphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2011-06-01

    Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, the two N atoms of the imidazolidine moiety are linked to the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. The crystal studied was a racemic mixture of RR and SS enatiomers. The cyclohexane ring adopts a chair conformation and the imidazolidine group to which it is fused has a twisted envelope conformation.

  7. Bis[(1-methyl-1H-tetrazol-5-ylsulfanyl]methane

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    Wei Wei

    2011-04-01

    Full Text Available The molecule of the title compound, C5H8N8S2, lies on a twofold rotation axis that relates on 1-methyltetrazolyl group to the other; the five-membered rings are twisted by 53.1 (1°.

  8. Crystal structure of ethyl (4R-2-amino-7-hydroxy-4-phenyl-4H-chromene-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Joel T. Mague

    2015-07-01

    Full Text Available In the title compound, C18H17NO4, the dihedral angle between the phenyl ring and the fused six-membered ring is 77.65 (4°. The conformation of the molecule is determined in part by an intramolecular N—H...O hydrogen bond between the amino H atom and the carbonyl O atom, forming an S(6 motif. In the crystal, molecules are linked into N—H...O hydrogen-bonded inversion dimers which are then connected into chains along [001], forming a two-dimensional network parallel to (100 via O—H...O hydrogen bonds. C—H...O interactions further contribute to the crystal stability. The ethyl group is disordered over two sets of sites in a 0.801 (5:0.199 (5 ratio.

  9. (Z-3-(4-Chlorophenyl-1-(2,4-difluorophenyl-2-(1H-1,2,4-triazol-1-ylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Xin-Mei Peng

    2012-06-01

    Full Text Available The asymmetric unit of the title compound, C17H10ClF2N3O, contains three independent molecules. In each molecule, the C=C bond has a cis conformation with respect to the triazole and chlorophenyl groups. The dihedral angles formed by the triazole ring with the diflurophenyl and chlorophenyl benzene rings, respectively, are 20.10 (14 and 73.22 (15, 25.31 (15 and 84.44 (15, and 16.44 (13 and 61.72 (14° in the three molecules while the dihedral angles between the benzene rings are 66.54 (13, 85.82 (12 and 58.37 (12°.

  10. Channels with ordered water and bipyridine molecules in the porous coordination polymer {[Cu(SiF6(C10H8N22]·2C10N2H8·5H2O}n

    Directory of Open Access Journals (Sweden)

    Emmanuel Aubert

    2016-11-01

    Full Text Available The coordination polymer {[Cu(SiF6(C10H8N22]·2C10H8N2·5H2O}n, systematic name: poly[[bis(μ2-4,4′-bipyridine(μ2-hexafluoridosilicatocopper(II] 4,4′-bipyridine disolvate pentahydrate], contains pores which are filled with water and 4,4′-bipyridine molecules. As a result of the presence of these ordered species, the framework changes its symmetry from P4/mmm to P21/c. The 4,4′-bipyridine guest molecules form chains inside the 6.5 × 6.9 Å pores parallel to [100] in which the molecules interact through π–π stacking. Ordered water molecules form infinite hydrogen-bonded chains inside a second pore system (1.6 × 5.3 Å free aperture perpendicular to the 4,4′-bipyridine channels.

  11. Synthesis, single-crystal structure determination and Raman spectra of the tricyanomelaminates NaA{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O (A = Rb, Cs)

    Energy Technology Data Exchange (ETDEWEB)

    Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Baker Lab.; Schulz, Armin [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

    2016-07-01

    Transparent colorless crystals of NaA{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O (A = Rb, Cs) were obtained by blending aqueous solutions of Na{sub 3}[C{sub 6}N{sub 9}] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group P2{sub 1}/m (no. 11) with the cell parameters a = 815.56(16), b = 1637.7(4) and c = 1036.4(3) pm, and β = 110.738(12) for NaRb{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O and a = 843.32(6), b = 1708.47(11) and c = 1052.42(7) pm, and β = 112.034(2) for NaCs{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O, respectively. Raman spectra of the title compounds complement our results.

  12. 4-{[(1-Phenyl-1H-pyrazol-3-yloxy]methyl}-1,3-dioxolan-2-one

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2012-11-01

    Full Text Available The title compound was obtained by the reaction of tosylated glycerol carbonate with 1-phenyl-1H-pyrazol-3-ol in a good 71% yield. Detailed spectroscopic data (1H-NMR, 13C-NMR, 15N-NMR, IR, MS are presented.

  13. (2E-3-(3-Methoxy-1-phenyl-1H-pyrazol-4-yl-2-propenal

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2009-12-01

    Full Text Available The palladium-catalyzed reaction of 4-bromo-3-methoxy-1-phenyl-1H-pyrazole with acrolein diethyl acetal gives the title compound in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  14. Electrical properties and conduction mechanism of [C2H5NH3]2CuCl4 compound

    Science.gov (United States)

    Mohamed, C. Ben; Karoui, K.; Jomni, F.; Guidara, K.; Rhaiem, A. Ben

    2015-02-01

    The [(C2H5)NH3]2CuCl4 compound was prepared and characterized by several technique: the X-ray powder diffraction confirms the purity of the synthetized compound, the differential scanning calorimetric show several phase transitions at 236 K, 330 K, 357 K and 371 K, the dialectical properties confirms the ferroelectric-paraelectric phase transition at 238 K, which is reported by V. Kapustianyk et al. (2007) [1]. The two semi-circles observed in the complex impedance identify the presence of the grain interior and grain boundary contributions to the electrical response in this material. The equivalent circuit is modeled by a combination series of two parallel RP-CPE circuits. The temperature dependence of the alternative current conductivity (σg) and direct current conductivity (σdc) confirm the observed transitions in the calorimetric study. The (AC) electrical conduction in [(C2H5)NH3]2CuCl4 was studied by two processes that can be attributed to a hopping transport mechanism: the non-overlapping small polaron tunneling (NSPT) model in phase III and the correlated barrier hopping (CBH) model in phases I, II, IV, V and VI.

  15. Synthesis, X-ray Single Crystal Structure, Molecular Docking and DFT Computations on N-[(1E)-1-(2H-1,3-Benzodioxol-5-yl)-3-(1H-imidazol-1-yl)propylidene]-hydroxylamine: A New Potential Antifungal Agent Precursor.

    Science.gov (United States)

    Al-Wabli, Reem I; Al-Ghamdi, Alwah R; Ghabbour, Hazem A; Al-Agamy, Mohamed H; Monicka, James Clemy; Joe, Issac Hubert; Attia, Mohamed I

    2017-02-28

    Mycoses are serious health problem, especially in immunocompromised individuals. A new imidazole-bearing compound containing an oxime functionality was synthesized and characterized with different spectroscopic techniques to be used for the preparation of new antifungal agents. The stereochemistry of the oxime double bond was unequivocally determined via the single crystal X-ray technique. The title compound 4 , C 13 H 13 N₃O₃·C₃H₈O, crystallizes in the monoclinic space group P 2₁with a = 9.0963(3) Å, b = 14.7244(6) Å, c = 10.7035(4) Å, β = 94.298 (3)°, V = 1429.57(9) ų, Z = 2. The molecules were packed in the crystal structure by eight intermolecular hydrogen bond interactions. A comprehensive spectral analysis of the title molecule 4 has been performed based on the scaled quantum mechanical (SQM) force field obtained by density-functional theory (DFT) calculations. A molecular docking study illustrated the binding mode of the title compound 4 into its target protein. The preliminary antifungal activity of the title compound 4 was determined using a broth microdilution assay.

  16. 11-[(E-Benzylidene]-14-hydroxy-8-phenyl-6-thia-3,13-diazaheptacyclo[13.7.1.19,13.02,9.02,14.03,7.019,23]tetracosa-1(22,15(23,16,18,20-pentaen-10-one

    Directory of Open Access Journals (Sweden)

    Raju Suresh Kumar

    2012-07-01

    Full Text Available In the title compound, C34H28N2O2S, the piperidine ring adopts a chair conformation. One of the pyrrolidine rings adopts an envelope conformation with the methylene C atom at the flap whereas the other pyrrolidine ring and the thiazolidine ring adopt half-chair conformations. The mean plane of the dihydroacenaphthylene ring system [maximum deviation = 0.067 (1 Å] makes dihedral angles of 28.31 (5 and 31.32 (6° with the two terminal benzene rings. An intramolecular O—H...N hydrogen bond forms an S(5 ring motif. In the crystal, molecules are linked by C—H...O and C—H...S hydrogen bonds into layers lying parallel to the ac plane.

  17. Crystal structure of 4-(1H-indol-3-yl-2-(4-methoxyphenyl-6-phenylpyridine-3-carbonitrile

    Directory of Open Access Journals (Sweden)

    R. Vishnupriya

    2014-10-01

    Full Text Available In the title compound, C27H19N3O, the dihedral angles between the plane of the pyridine ring and those of the indole (r.m.s. deviation = 0.018 Å, phenyl and methoxybenzene substituents are 33.60 (6, 25.28 (7 and 49.31 (7°, respectively. The N atom of the carbonitrile group is significantly displaced [0.288 (2 Å] from the plane of the pyridine ring, perhaps due to steric crowding. In the crystal, inversion dimers linked by pairs of N—H...Nn (n = nitrile hydrogen bonds generate R22(16 loops. Aromatic π–π stacking [centroid–centroid separation = 3.6906 (7 Å] and very weak C—H...π interactions are also observed".

  18. 2,3-[(3,6-Dioxaoctane-1,8-diylbis(sulfanediylmethylene]-6,7-bis(methylsulfanyl-1,4,5,8-tetrathiafulvalene

    Directory of Open Access Journals (Sweden)

    Rui-Bin Hou

    2009-11-01

    Full Text Available In the title molecule, C16H22S8O2, two S atoms, two O atoms and ten C atoms form a 14-membered ring with a boat conformation. In the crystal, C—H...O hydrogen bonds link the molecules into dimers which are further connected into a chain along the a axis by C—H...S hydrogen bonds.

  19. Radiosynthesis and pre-clinical evaluation of [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Graham [Comprehensive Cancer Imaging Centre, Faculty of Medicine, Imperial College London, Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Zhao Yongjun [MDx Discovery (part of GE Healthcare) at Hammersmith Imanet, Ltd., Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Leyton, Julius [Comprehensive Cancer Imaging Centre, Faculty of Medicine, Imperial College London, Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Shan Bo [MDx Discovery (part of GE Healthcare) at Hammersmith Imanet, Ltd., Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Nguyen, Quang-de; Perumal, Meg [Comprehensive Cancer Imaging Centre, Faculty of Medicine, Imperial College London, Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Turton, David [GE-Imanet, Hammersmith Hospital, Du Cane Road, London, W12 0NN (United Kingdom); Arstad, Erik; Luthra, Sajinder K.; Robins, Edward G. [MDx Discovery (part of GE Healthcare) at Hammersmith Imanet, Ltd., Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom); Aboagye, Eric O., E-mail: eric.aboagye@imperial.ac.u [Comprehensive Cancer Imaging Centre, Faculty of Medicine, Imperial College London, Hammersmith Hospital, Du Cane Road, London W12 0NN (United Kingdom)

    2011-01-15

    Introduction: Choline radiotracers are widely used for clinical PET diagnosis in oncology. [{sup 11}C]Choline finds particular utility in the imaging of brain and prostate tumor metabolic status, where 2-[{sup 18}F]fluoro-2-deoxy-D-glucose ('FDG') shows high background uptake. More recently we have extended the clinical utility of [{sup 11}C]choline to breast cancer where radiotracer uptake correlates with tumor aggressiveness (grade). In the present study, a new choline analog, [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline, was synthesized and evaluated as a potential PET imaging probe. Methods: [{sup 18}F]Fluorocholine, [{sup 18}F]fluoro-[1-{sup 2}H{sub 2}]choline and [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline were synthesized by alkylation of the relevant precursor with [{sup 18}F]fluorobromomethane or [{sup 18}F]fluoromethyl tosylate. Radiosynthesis of [{sup 18}F]fluoromethyl tosylate required extensive modification of the existing method. [{sup 18}F]Fluorocholine and [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline were then subjected to in vitro oxidative stability analysis in a chemical oxidation model using potassium permanganate and an enzymatic model using choline oxidase. The two radiotracers, together with the corresponding di-deuterated compound, [{sup 18}F]fluoro-[1-{sup 2}H{sub 2}]choline, were then evaluated in vivo in a time-course biodistribution study in HCT-116 tumor-bearing mice. Results: Alkylation with [{sup 18}F]fluoromethyl tosylate proved to be the most reliable radiosynthetic route. Stability models indicate that [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline possesses increased chemical and enzymatic (choline oxidase) oxidative stability relative to [{sup 18}F]fluorocholine. The distribution of the three radiotracers, [{sup 18}F]fluorocholine, [{sup 18}F]fluoro-[1-{sup 2}H{sub 2}]choline and [{sup 18}F]fluoro-[1,2-{sup 2}H{sub 4}]choline, showed a similar uptake profile in most organs. Crucially, tumor uptake of [{sup 18}F

  20. Crystal structures of hibiscus acid and hibiscus acid dimethyl ester isolated from Hibiscus sabdariffa (Malvaceae)

    OpenAIRE

    Zheoat, Ahmed M.; Gray, Alexander I.; Igoli, John O.; Kennedy, Alan R.; Ferro, Valerie A.

    2017-01-01

    The biologically active title compounds have been isolated from Hibiscus sabdariffa plants, hibiscus acid as a dimethyl sulfoxide monosolvate [systematic name: (2S,3R)-3-hy?droxy-5-oxo-2,3,4,5-tetra?hydro?furan-2,3-di?carb?oxy?lic acid dimethyl sulfoxide monosolvate], C6H6O7?C2H6OS, (I), and hibiscus acid dimethyl ester [systematic name: dimethyl (2S,3R)-3-hy?droxy-5-oxo-2,3,4,5-tetra?hydro?furan-2,3-di?carboxyl?ate], C8H10O7, (II). Compound (I) forms a layered structure with alternating laye...

  1. (5S-4-(2,2-Dimethylpropyl-5-isopropyl-1,3,4-oxadiazinan-2-one

    Directory of Open Access Journals (Sweden)

    Kate L. Edler

    2010-12-01

    Full Text Available The title compound, C11H22N2O2, has one chiral center and packs in the monoclinic space group P21. The asymmetric unit has five crystallographically independent molecules, four of which engage in intermolecular N—H...O hydrogen bonding.

  2. (E-3-Hydroxy-13-methyl-16-[4-(methylsulfanylbenzylidene]-7,8,9,11,12,13,15,16-octahydro-6H-cyclopenta[a]phenanthren-17(14H-one

    Directory of Open Access Journals (Sweden)

    R. Murugan

    2009-01-01

    Full Text Available In the title compound, C26H28O2S, the dihedral angles between the mean plane of the five membered ring and the 4-(methylsulfanylbenzylidine ring in the two crystallographically independent molecules are 34.05 (10 and 40.53 (15°. The packing is stabilized by intermolecular O—H...O and C—H...O interactions.

  3. 9-Ethyl-3,6-diformyl-9H-carbazole

    Directory of Open Access Journals (Sweden)

    Jun Jie Wang

    2008-07-01

    Full Text Available The structure of the title compound, C16H13NO2, was determined as a part of a project on the synthesis of new compounds which can make two-photon absorptions. In the crystal structure, both aldehyde groups are located within the carbazole plane. One of these groups is disordered and was refined using a split model with site-occupation factors for each position of 0.5.

  4. Crystal structure of 2-amino-N-(2-fluorophenyl-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide

    Directory of Open Access Journals (Sweden)

    K. Chandra Kumar

    2015-11-01

    Full Text Available In the title compound, C15H15FN2OS, the dihedral angle between the planes of the benzothiophene ring system and the fluorobenzene ring is 3.74 (14°. The six-membered ring of the benzothiophene moiety adopts a half-chair conformation. The molecular conformation is consolidated by intramolecular N—H...F and N—H...O hydrogen bonds. In the crystal, molecules are linked by N—H...O hydrogen bonds, generating C(6 [001] chains.

  5. 1-Chloro-3-(6-nitro-1H-indazol-1-ylpropan-2-ol

    Directory of Open Access Journals (Sweden)

    Mohamed Mokhtar Mohamed Abdelahi

    2017-05-01

    Full Text Available In the title compound, C10H10ClN3O3, the side chain is oriented nearly perpendicular to the mean plane of the indazole ring system. In the crystal, complementary sets of O—H...N and C—H...O hydrogen bonds form chains of molecules stacked along the a-axis direction

  6. 1,1′-Bicyclohexyl-1,1′-diyl 2,2′-bipyridine-3,3′-dicarboxylate

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2012-06-01

    Full Text Available The title compound, C24H26N2O4, lies about a crystallographic twofold rotation axis. The cyclohexane rings adopts a chair conformation. The two pyridine rings form a dihedral angle of 41.02 (4°. In the crystal, molecules are linked via C—H...O and C—H...N hydrogen bonds into a layer parallel to the bc plane.

  7. New Approaches for the Synthesis, Cytotoxicity and Toxicity of Heterocyclic Compounds Derived from 2-Cyanomethylbenzo[c]imidazole.

    Science.gov (United States)

    Mohareb, Rafat M; Mohamed, Abeer A; Abdallah, Amira E M

    2016-01-01

    The reaction of ethyl cyanoacetate with o-phenylenediamine gave the 2-cyanomethylbenzo[c]imidazole (1). The latter compound was used as the key starting material to synthesise biologically active heterocyclic derivatives. Thus, the reaction of 1 with cyclohexanone and either of benzaldehyde, 4-methoxybenzaldehyde or 4-chlorobenzaldehyde gave the annulated derivatives 2a-c, respectively. The antitumor evaluations of the newly synthesized products against the three cancer cell lines MCF-7 (breast adeno-carcinoma), NCI-H460 (non-small cell lung cancer) and SF-268 (CNS cancer) showed that compounds 2b, 6, 11b, 11c, 12b, 16a, 16b and 18a exhibited optimal cytotoxic effect against cancer cell lines, with IC50 values in the nM range. Bioactive compounds are often toxic to shrimp larvae. Thus, in order to monitor these chemicals in vivo lethality to shrimp larvae (Artemia salina), Brine-Shrimp Lethality Assay was used. Compounds 11b, 12b and 16b showed no toxicity against the tested organisms.

  8. C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

    Energy Technology Data Exchange (ETDEWEB)

    Audí-Miró, Carme, E-mail: carmeaudi@ub.edu [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Cretnik, Stefan [Institute of Groundwater Ecology, Helmholtz Zentrum München-National Research Center for Environmental Health, Ingolstädter Landstrasse 1, D-85764 Neuherberg (Germany); Torrentó, Clara; Rosell, Mònica [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Shouakar-Stash, Orfan [Department of Earth & Environmental Sciences, 200 University Ave. W, N2L 3G1 Waterloo, Ontario (Canada); Otero, Neus [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Palau, Jordi [Université de Neuchâtel, CHYN - Centre d' Hydrogéologie, Rue Emile-Argand 11, CH-2000 Neuchâtel (Switzerland); and others

    2015-12-15

    Highlights: • {sup 13}C to evaluate natural chlorinated ethenes biodegradation. • {sup 13}C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • {sup 13}C-{sup 37}Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • {sup 13}C-{sup 37}Cl-{sup 2}H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using {sup 13}C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element {sup 13}C-{sup 37}Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using {sup 13}C-{sup 37}Cl-{sup 2}H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the {sup 13}C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element {sup 13}C-{sup 37}Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. {sup 2}H combined with {sup 13}C and {sup 37}Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ{sup 2}H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

  9. C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

    International Nuclear Information System (INIS)

    Audí-Miró, Carme; Cretnik, Stefan; Torrentó, Clara; Rosell, Mònica; Shouakar-Stash, Orfan; Otero, Neus; Palau, Jordi

    2015-01-01

    Highlights: • 13 C to evaluate natural chlorinated ethenes biodegradation. • 13 C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • 13 C- 37 Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • 13 C- 37 Cl- 2 H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using 13 C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element 13 C- 37 Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using 13 C- 37 Cl- 2 H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the 13 C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element 13 C- 37 Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. 2 H combined with 13 C and 37 Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ 2 H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

  10. Novel high pressure hexagonal OsB{sub 2} by mechanochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Zhilin; Graule, Moritz [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Orlovskaya, Nina, E-mail: Nina.Orlovskaya@ucf.edu [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Andrew Payzant, E. [Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, 1 Bethel Valley Road, Oak Ridge, TN 37831 (United States); Cullen, David A. [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Blair, Richard G. [Department of Chemistry, University of Central Florida, Orlando, FL 32816 (United States)

    2014-07-01

    Hexagonal OsB{sub 2}, a theoretically predicted high-pressure phase, has been synthesized for the first time by a mechanochemical method, i.e., high energy ball milling. X-ray diffraction indicated that formation of hexagonal OsB{sub 2} begins after 2.5 h of milling, and the reaction reaches equilibrium after 18 h of milling. Rietveld refinement of the powder data indicated that hexagonal OsB{sub 2} crystallizes in the P63/mmc space group (No. 194) with lattice parameters of a=2.916 Å and c=7.376 Å. Transmission electron microscopy confirmed the appearance of the hexagonal OsB{sub 2} phase after high energy ball milling. in situ X-ray diffraction experiments showed that the phase is stable from −225 °C to 1050 °C. The hexagonal OsB{sub 2} powder was annealed at 1050 °C for 6 days in vacuo to improve crystallinity and remove strain induced during the mechanochemical synthesis. The structure partially converted to the orthorhombic phase (20 wt%) after fast current assisted sintering of hexagonal OsB{sub 2} at 1500 °C for 5 min. Mechanochemical approaches to the synthesis of hard boride materials allow new phases to be produced that cannot be prepared using conventional methods. - Graphical abstract: High resolution transmission electron micrograph of hexagonal OsB{sub 2} nanocrystallite with corresponding fast Fourier transform and simulated diffraction pattern. - Highlights: • Hexagonal OsB{sub 2} has been synthesized for the first time by mechanochemical method. • Hexagonal OsB{sub 2} crystallizes in P63/mmc space group (No. 194), a=2.916 Å and c=7.376 Å. • The hexagonal structure was confirmed by a transmission electron microscope. • No phase transformation was observed after being annealed at 1050 °C for 6 days. • 20 wt% of h-OsB{sub 2} was transformed to o-OsB{sub 2} after being sintered at 1500 °C for 5 min.

  11. System of Sr(NO2)2-Sr(OH)2-H2O at 25 deg C

    International Nuclear Information System (INIS)

    Popova, T.B.; Berdyukova, V.A.; Khutsistova, F.M.

    1990-01-01

    Sr(NO 2 ) 2 -Sr(OH) 2 -H 2 O system was investigated by the methods of solubility, density, viscosity, electric conductivity and refractometry. It was established that its compoments form the compound 4Sr(NO 2 ) 2 xSr(OH) 2 x8H 2 O. The compound was separated from solution; its density, decomposition temperature were determined; IR spectra and X-ray patterns of prepared and initial compounds were obtained

  12. 9-Butyl-9H-carbazole

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The title compound, C16H17N, is a carbazole derivative that has been designed and synthesized as a potential organic electronic device, such as an OLED. The tricyclic aromatic ring system is essentially planar, the two outer rings making a dihedral angle of 4.8 (1°. No classical hydrogen bonds are observed in the crystal structure.

  13. A Facile Synthesis of Pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidine and Pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazine Bearing a Thiophene Moiety

    Directory of Open Access Journals (Sweden)

    Tilal Elsaman

    2013-01-01

    Full Text Available Pyridinone derivative 8 was synthesized and transformed into the respective chloropyridine 9, which was allowed to react with hydrazine hydrate to afford pyrazolo[3,4-b]pyridin-3-amine derivative 11. Compound 11 was used as a key intermediate for a facile synthesis of the title compounds 14, 15, 17, 21a,b, and 24a–c where the reaction of 11 with some 1,3-dielecrophiles resulted in the formation of pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidines 14, 15, and 17, whereas diazotization of compound 11 gave the respective diazonium salt 18 which was coupled with some active methylene-containing compounds to give the corresponding hydrazones 19a,b and 22a–c. Cyclization of the latter hydrazones yielded the pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazines 21a,b and 24a–c, respectively.

  14. Interconversion of η3-H2SiRR' σ-complexes and 16-electron silylene complexes via reversible H-H or C-H elimination.

    Science.gov (United States)

    Lipke, Mark C; Neumeyer, Felix; Tilley, T Don

    2014-04-23

    Solid samples of η(3)-silane complexes [PhBP(Ph)3]RuH(η(3)-H2SiRR') (R,R' = Et2, 1a; PhMe, 1b; Ph2, 1c, MeMes, 1d) decompose when exposed to dynamic vacuum. Gas-phase H2/D2 exchange between isolated, solid samples of 1c-d3 and 1c indicate that a reversible elimination of H2 is the first step in the irreversible decomposition. An efficient solution-phase trap for hydrogen, the 16-electron ruthenium benzyl complex [PhBP(Ph)3]Ru[η(3)-CH2(3,5-Me2C6H3)] (3) reacts quantitatively with H2 in benzene via elimination of mesitylene to form the η(5)-cyclohexadienyl complex [PhBP(Ph)3]Ru(η(5)-C6H7) (4). This H2 trapping reaction was utilized to drive forward and quantify the elimination of H2 from 1b,d in solution, which resulted in the decomposition of 1b,d to form 4 and several organosilicon products that could not be identified. Reaction of {[PhBP(Ph)3]Ru(μ-Cl)}2 (2) with (THF)2Li(SiHMes2) forms a new η(3)-H2Si species [PhBP(Ph)3]Ru[CH2(2-(η(3)-H2SiMes)-3,5-Me2C6H2)] (5) which reacts with H2 to form the η(3)-H2SiMes2 complex [PhBP(Ph)3]RuH(η(3)-H2SiMes2) (1e). Complex 1e was identified by NMR spectroscopy prior to its decomposition by elimination of Mes2SiH2 to form 4. DFT calculations indicate that an isomer of 5, the 16-electron silylene complex [PhBP(Ph)3]Ru(μ-H)(═SiMes2), is only 2 kcal/mol higher in energy than 5. Treatment of 5 with XylNC (Xyl = 2,6-dimethylphenyl) resulted in trapping of [PhBP(Ph)3]Ru(μ-H)(═SiMes2) to form the 18-electron silylene complex [PhBP(Ph)3]Ru(CNXyl)(μ-H)(═SiMes2) (6). A closely related germylene complex [PhBP(Ph)3]Ru[CN(2,6-diphenyl-4-MeC6H2)](H)(═GeH(t)Bu) (8) was prepared from reaction of (t)BuGeH3 with the benzyl complex [PhBP(Ph)3]Ru[CN(2,6-diphenyl-4-MeC6H2)][η(1)-CH2(3,5-Me2C6H3)] (7). Single crystal XRD analysis indicated that unlike for 6, the hydride ligand in 8 is a terminal hydride that does not engage in 3c-2e Ru-H → Ge bonding. Complex 1b is an effective precatalyst for the catalytic Ge-H dehydrocoupling

  15. Synthesis of n.c.a. 18F-fluorinated NMDA- and D4-receptor ligands via [18F]fluorobenzenes

    International Nuclear Information System (INIS)

    Ludwig, T.

    2005-11-01

    In this thesis new strategies were developed and evaluated for the no-carrier-added (n.c.a.) 18 F-labelling of receptor ligands as radiodiagnostics for characterization of brain receptors using positron-emission-tomography (PET). Special emphasis was placed on the synthesis of n.c.a. (±)-3-(4-hydroxy-4-(4-[ 18 F]fluorophenyl)-piperidin-l-yl)chroman-4,7-diol, a ligand with high affinity for the NR2B subtype of NMDA receptors and n.c.a. (3-(4-[ 18 F]fluorphenoxy)propyl)-(2-(4-tolylphenoxy)ethyl)amine ([ 18 F]FPTEA) a dopamine D 4 receptor ligand. In order to synthesize n.c.a. (±)-3-(4-hydroxy-4-(4-[ 18 F]fluorophenyl)-piperidin-l-yl)chroman-4,7-diol the 18 F-fluoroarylation method via metallorganic intermediates was modified and improved. The suitability of the organometallic 18 F-fluoroarylation agents was proven with several model compounds. High radiochemical yields of 20-30% were obtained also with piperidinone-derivatives. The preparation of a suitable precursor for the synthesis of the NMDA receptor ligand, however, could not be achieved by synthesis of appropriate 1,3-dioxolane protected piperidinone derivatives. Further, the synthesis of n.c.a. ([ 18 F]fluoroaryloxy)alkylamines via n.c.a. 4-[ 18 F]fluorophenol was developed and evaluated. The synthesis of n.c.a. [ 18 F]fluoroarylethers with corresponding model compounds was optimized and led to a radiochemical yield of 25-60%, depending on the alkylhalide used. The preparation of n.c.a. 1-(3-bromopropoxy)-4-[ 18 F]fluorobenzene proved advantageous in comparison to direct use of 4-[ 18 ]fluorophenol for coupling with a corresponding N-protected precursor for the synthesis of n.c.a. [ 18 F]FPTEA. With regard to the radiochemical yields and the loss of activity during the synthesis and isolation of n.c.a. 4-[ 18 F]fluorophenol and n.c.a. 1-(3-bromopropoxy)-4-[ 18 F]fluorobenzene, [ 18 F]FPTEA was obtained by reaction with 2-(4-tolyloxy)ethylamine in radiochemical yields of about 25-30% in ethanol or 2-butanone

  16. Molecular and crystal structure of gossypol tetramethyl ether with an unknown solvate

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    Muhabbat Honkeldieva

    2015-02-01

    Full Text Available The title compound, C34H38O8 (systematic name: 5,5′-diisopropyl-2,2′,3,3′-tetramethoxy-7,7′-dimethyl-2H,2′H-8,8′-bi[naphtho[1,8-bc]furan]-4,4′-diol, has been obtained from a gossypol solution in a mixture of dimethyl sulfate and methanol. The molecule is situated on a twofold rotation axis, so the asymmetric unit contains one half-molecule. In the molecule, the hydroxy groups are involved in intramolecular O—H...O hydrogen bonds, and the two naphthyl fragments are inclined each to other by 83.8 (1°. In the crystal, weak C—H...O and C—H...π interactions consolidate the packing, which exhibits channels with an approximate diameter of 6 Å extending along the c-axis direction. These channels are filled with highly disordered solvent molecules, so their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE option in PLATON [Spek, A. L. (2015. Acta Cryst. C71, 9–18].

  17. Dibromido[1,1′-dibutyl-2,2′-(pentane-1,1-diyldi-1H-benzimidazole]copper(II

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    Robert T. Stibrany

    2010-07-01

    Full Text Available In the title compound, [CuBr2(C27H36N4], the CuII ion exhibits a distorted tetrahedral coordination geometry provided by two bromide ions and by chelation of two imine N-atom donors from a bis(benzimidazole ligand. Chelation results in a six-membered boat-shaped ring which links the benzimidazole groups. Each bis(benzimidazole fragment contains three n-butyl substituents, two of which have the expected trans conformation; the third exhibits the higher-energy cis conformation, an orientation consistent with several short intramolecular C—H...Br interactions. Essentially planar (r.m.s. deviations of 0.0101 and 0.0183 Å benzimidazole groups are oriented so as to give the bis(benzimidazole fragment a V-shaped appearance in profile with the cis and trans n-butyl groups directed to opposite sides of the planes. In the crystal, columns of molecules along the b-axis direction form layers parallel to the (202 planes. Within a given column, the molecules are linked by C—H...Br hydrogen bonds. The molecules in adjacent columns are also linked by intermolecular C—H...π interactions, forming a three-dimensional network.

  18. Structural investigation of 18-crown-6 complexes of Tri organotin carboxylate by 1H, 13C, 19F and 119Sn nuclear magnetic resonance spectroscopy

    International Nuclear Information System (INIS)

    Foladi, S.; Yousefi, M.; Mohammadpour Ammini, M. M.

    2002-01-01

    Single crystal structure determination of several 18-crown 6 complexes of orga nation derivatives reveals formation of aqua complex through hydrogen bonding to 18-crown-6, which is an important feature in their structure. In the majority of those studies, mono- and dichloro organotin have been used for complexation of them with crown ethers. In the present work, several 18-crown 6 complexes of tri organotin acetate[(C 6 H 5 ) 3 SnOCOCX 3 ] 2 , 18 C6 ], X=F, Cl, and H, have been prepared. The Lewis acidity of tin moiety in tri organotin carboxylate have been tailored by replacing hydrogen atoms of acetate group with chlorine and fluorine and influence of them in the formation of aqua complex with 18 C6 have been studied by infrared. 1 H, 13 C, 19 F and 119 Sn nuclear magnetic resonance spectroscopes. The effects of coordinating and non-coordinating solvent in status of structure in solution have been explored

  19. Development of novel strategy for the synthesis of organometallic compounds usable as protein ligands: application to the human cyclophilin hCyp-18; Developpement de ligands de proteines par assemblage combinatoire autour d'un coeur de rhenium{sup V}: application a la cyclophiline hCyp-18

    Energy Technology Data Exchange (ETDEWEB)

    Clavaud, C

    2006-02-15

    This thesis describes a new strategy for the development of bioactive organometallic compounds, basing on the combinatorial assembly of sub-chemical libraries (A and B) independent but complementary and able to coordinate a metallic heart M to form A-M-B complex potential ligands of biomolecules. The coordination of metals, well adapted to the production of molecular variety is usually used in medicinal chemistry, in diagnostic and therapeutic nuclear medicine. Among the useful elements, the rhenium and the technetium are metals of choice for the development of the assembly strategy because of their chemical and radiochemical properties and of the structure analogy of their complexes. This strategy was validated in vitro. The protein chosen for this purpose was the cyclophilin hCyp-18. (N.C.)

  20. 1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one

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    Hualing Zhu

    2011-07-01

    Full Text Available In the title compound, C21H21N3O2, an intramolecular N—H...O interaction generates an S(6 ring, which stablizes the enamine–keto tautomer. The S(6 ring makes dihedral angles of 33.07 (7, 56.50 (8 and 38.59 (8°, respectively, with the benzoylacetone benzene ring and the antipyrine pyrazole and benzene rings.

  1. 4-(2,3-Dihydroxybenzylideneamino-3-methyl-1H-1,2,4-triazol-5(4H-one

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    Şamil Işık

    2009-12-01

    Full Text Available All the non-H atoms of the title compound, C10H10N4O3, are almost coplanar, the maximum deviation from planarity being 0.065 (3 Å. The dihedral angle between the aromatic rings is 1.66 (6°. The molecule adopts the enol–imine tautomeric form with an intramolecular hydrogen-bonding interaction between the Schiff base N atom and the hydroxy group. In the crystal, intermolecular N—H...O and O—H...O hydrogen bonds link the molecules into a three-dimensional network.

  2. (E-2,2′-[3-(2-Nitrophenylprop-2-ene-1,1-diyl]bis(3-hydroxycyclohex-2-en-1-one

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    Joo Hwan Cha

    2012-01-01

    Full Text Available In the title compound, C21H21NO6, each of the cyclohexenone rings adopts a half-chair conformation. Each of the pairs of hydroxy and carbonyl O atoms are oriented to allow for the formation of intramolecular O—H...O hydrogen bonds, which are typical of xanthene derivatives.

  3. 1-Propyl-1H-indole-2,3-dione

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    Fatima Zahrae Qachchachi

    2016-04-01

    Full Text Available In the title compound, C11H11NO2, the 1H-indole-2,3-dione unit is essentially planar, with an r.m.s. deviation of 0.0387 (13 Å. This plane makes a dihedral angle of 72.19 (17° with the plane of the propyl substituent. In the crystal, chains propagating along the b axis are formed through C—H...O hydrogen bonds.

  4. 3-Ethyl-5-(4-methoxyphenoxy-2-(pyridin-4-yl-3H-imidazo[4,5-b]pyridine

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    S. Ranjith

    2011-07-01

    Full Text Available In the title compound, C20H18N4O2, the imidazopyridine fused ring system is almost perpendicular to the benzene ring [dihedral angle = 87.6 (5°]. The pyridine ring makes a dihedral angle of 35.5 (5° with the mean plane of the imidazopyridine fragment. The crystal structure is stabilized by an aromatic π–π stacking interaction between the phenyl rings of neighbouring molecules [centroid–centroid distance = 3.772 (2 Å, interplanar distance = 3.546 (2 Å and slippage = 1.286 (2 Å].

  5. 1-Methyl-4-phenyl-1H-pyrazolo[3,4-d]pyrimidine

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    Mohamed El Hafi

    2017-09-01

    Full Text Available In the crystal, molecules of the title compound, C12H10N4, stack in a head-to-tail manner along the b direction through π–π stacking interactions between both portions of the pyrazolopyrimidine ring system.

  6. Thio-phene-2-carbonyl azide.

    Science.gov (United States)

    Hsu, Gene C; Singer, Laci M; Cordes, David B; Findlater, Michael

    2013-01-01

    The title compound, C5H3N3OS, is almost planar (r.m.s. deviation for the ten non-H atoms = 0.018 Å) and forms an extended layer structure in the (100) plane, held together via hydrogen-bonding inter-actions between adjacent mol-ecules. Of particular note is the occurrence of RC-H⋯N(-)=N(+)=NR inter-actions between an aromatic C-H group and an azide moiety which, in conjunction with a complementary C-H⋯O=C inter-action, forms a nine-membered ring.

  7. Neuroprotective Properties of Compounds Extracted from Dianthus superbus L. against Glutamate-induced Cell Death in HT22 Cells.

    Science.gov (United States)

    Yun, Bo-Ra; Yang, Hye Jin; Weon, Jin Bae; Lee, Jiwoo; Eom, Min Rye; Ma, Choong Je

    2016-01-01

    Dianthus superbus L. has been used in Chinese herbal medicine as a diuretic and anti-inflammatory agent. In this study, we isolated ten bioactive compounds from D. superbus and evaluated their neuroprotective activity against glutamate-induced cell death in the hippocampal neuronal HT22 cells. New compound, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1) and, nine known compounds, diosmetin-7-O (2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), 4-hydroxy-3-methoxy-pentyl ester benzenepropanoic acid (3), vanillic acid (4), 4-hydroxy-benzeneacetic acid (5), 4-methoxybenzeneacetic acid (6), (E)-4-methoxycinnamic acid (7), 3-methoxy-4-hydroxyphenylethanol (8), hydroferulic acid (9), and methyl hydroferulate (10), were isolated by bioactivity-guided separation. Structures of the isolated compounds were identified on the basis of (1)H nuclear magnetic resonance (NMR), (13)C NMR, and two-dimensional NMR spectra, while their neuroprotective properties were evaluated by performing the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. D. superbus extract had a neuroprotective effect and isolated 10 compounds. Among the compounds, compounds 5 and 6 effectively protected HT22 cells against glutamate toxicity. In conclusion, the extract of D. superbus and compounds isolated from it exhibited neuroprotective properties, suggesting therapeutic potential for applications in neurotoxic diseases. D. superbus extract significantly protected on glutamate-induced cell death in HT22 cellsNew compound, (E)-methyl-4-hydroxy-4-(8a-methyl-3-oxodecahydronaphthalen-4a-yl) (1) and, nine known compounds, diosmetin-7-O(2'',6''-di-O-α-L-rhamnopyranosyl)-β-D-glucopyranoside (2), 4-hydroxy-3-methoxy-pentyl ester benzenepropanoic acid (3), vanillic acid (4), 4-hydroxy-benzeneacetic acid (5), 4-methoxybenzeneacetic acid (6), (E)-4-methoxycinnamic acid (7), 3-methoxy-4-hydroxyphenylethanol (8), hydroferulic acid (9), and methyl hydroferulate (10

  8. Synthesis of Donor/Acceptor-Substituted Diazo Compounds in Flow and Their Application in Enantioselective Dirhodium-Catalyzed Cyclopropanation and C-H Functionalization.

    Science.gov (United States)

    Rackl, Daniel; Yoo, Chun-Jae; Jones, Christopher W; Davies, Huw M L

    2017-06-16

    A tandem reaction system has been developed for the preparation of donor/acceptor-substituted diazo compounds in continuous flow coupled to dirhodium-catalyzed C-H functionalization or cyclopropanation. Hydrazones were oxidized in flow by solid-supported N-iodo-p-toluenesulfonamide potassium salt (PS-SO 2 NIK) to generate the diazo compounds, which were then purified by passing through a column of molecular sieves/sodium thiosulfate.

  9. Observation/confirmation of hindered E2 strength in {sup 18}C/{sup 16}C

    Energy Technology Data Exchange (ETDEWEB)

    Ong, H.J. [Osaka University, RCNP, Ibaraki, Osaka (Japan); Imai, N. [KEK, Tsukuba, Ibaraki (Japan); Suzuki, D.; Iwasaki, H.; Onishi, T.K.; Suzuki, M.K.; Nakao, T.; Ichikawa, Y. [University of Tokyo, Department of Physics, Bunkyo,Tokyo (Japan); Sakurai, H.; Takeuchi, S.; Kondo, Y.; Aoi, N.; Baba, H.; Bishop, S.; Ishihara, M.; Kubo, T.; Motobayashi, T.; Yanagisawa, Y. [RIKEN, RIKEN Nishina Center, Wako, Saitama (Japan); Ota, S. [University of Tokyo, RIKEN Campus, CNS, Wako, Saitama (Japan); Togano, Y.; Kurita, K. [Rikkyo University, Department of Physics, Toshima, Tokyo (Japan); Nakamura, T.; Okumura, T. [Tokyo Institute of Technology, Department of Physics, Meguro, Tokyo (Japan)

    2009-12-15

    We have measured the lifetime of the first excited 2{sup +} state in {sup 18}C using an upgraded recoil shadow method to determine the electric quadrupole transition. The measured mean lifetime is 18.9{+-}0.9 (stat){+-}4.4 (syst) ps, corresponding to B(E2;2{sub 1} {sup +}{yields} 0{sup +} {sub gs}) = 4.3{+-}0.2{+-}1.0 e{sup 2}fm{sup 4}, or about 1.5 Weisskopf units. The mean lifetime of the first 2{sup +} state in {sup 16}C was remeasured to be 18.3{+-}1.4{+-}4.8 ps, about four times shorter than the value reported previously. The discrepancy is explained by incorporating the {gamma} -ray angular distribution obtained in this work into the previous measurement. The observed transition strengths in {sup 16,18}C are hindered compared to the empirical values, indicating that the anomalous E2 strength observed in {sup 16}C persists in {sup 18}C. (orig.)

  10. 2-[1-(1-Naphthyl-1H-1,2,3-triazol-4-yl]pyridine

    Directory of Open Access Journals (Sweden)

    Ulrich S. Schubert

    2009-05-01

    Full Text Available In the crystal structure of the title compound, C17H12N4, the angle between the naphthalene and 1H-1,2,3-triazole ring systems is 71.02 (4° and that between the pyridine and triazole rings is 8.30 (9°.

  11. Investigation of the alpha cluster states in 22Ne through the transfer induced breakup reaction 12C (18O, 18O + α)8Be at E(18O) 94.5 MeV

    International Nuclear Information System (INIS)

    Adhikari, S.; Basu, C.; Mitra, A.K.; Behera, B.R.; Ray, S.; Kumar, Suresh; Chatterjee, A.

    2008-01-01

    The nucleus 22 Ne like 18 O and 20 Ne has been sparsely investigated experimentally for an 18 O + α cluster structure. Only one experiment has reported the 22 Ne alpha cluster states using the same reaction but a much higher energy. One other experiment also reported the states with a different target and the results of these experiments are different. Therefore the 22 Ne structure has been analyzed in this work

  12. 5′′-(4-Nitrobenzylidene-7′-(4-nitrophenyl-1′′-methyl-1′,3′,5′,6′,7′,7a′-hexahydrodispiro[acenaphthylene-1,5′-pyrrolo[1,2-c][1,3]thiazole-6′,3′′-piperidine]-2,4′′(1H-dione including an unknown solvate

    Directory of Open Access Journals (Sweden)

    P. L. Nilantha Lakshman

    2013-08-01

    Full Text Available The title compound, C35H28N4O6S, crystallizes with two molecules in the asymmetric unit. In both molecules, the piperidine ring adopts a shallow-chair conformation, the thiazole ring adopts a twisted conformation about the Cm—N bond (m = methine and the pyrrole ring adopts an envelope conformation with the C atom shared with the thiazole ring as the flap. In the crystal, inversion dimers linked by pairs of C—H...O interactions generate R22(34 loops for one of the asymmetric molecules. Further C—H...O links also involving the other molecule lead to a three-dimesional network. The contribution of the highly disordered solvent to the scattering was removed with SQUEEZE option of PLATON [Spek (2009. Acta Cryst. D65, 148–155]. The solvent contribution is not included in the reported molecular weight and density.

  13. 5-(4-Fluorophenyl-2,2,6-trimethyl-4H-1,3-dioxin-4-one

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    Julio Zukerman-Schpector

    2009-07-01

    Full Text Available The 1,3-dioxine ring in the title compound, C13H13FO3, is in a half-boat conformation with the methyl-bonded C atom 0.612 (2 Å out of the plane defined by the remaining five atoms.

  14. Quinoline-2-sulfonamide

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    Joachim Kusz

    2013-08-01

    Full Text Available In the title compound, C9H8N2O2S, the sulfamoyl –NH2 group is involved in intermolecular hydrogen bonding with the sulfonamide O and quinoline N atoms. In the crystal, molecules are linked into dimers via pairs of N—H...N hydrogen bonds, forming an R22(10 motif. The dimers are further assembled into chains parallel to the b axis through N—H...O hydrogen bonds, generating a C(4 motif. The crystal packing is additionally stabilized by intermolecular C—H...O interactions. The crystal studied was a non-merohedral twin with a domain ratio of 0.938 (2:0.062 (2. Density functional theory (DFT calculations, at the B3LYP/6–31 G(d,p level of theory, were used to optimize the molecular structure and to determine interaction energies for the title compound. The resulting interaction energy is ∼4.4 kcal mol−1 per bridge for the C(4 chain and ∼5.9 kcal mol−1 per bridge for the R22(10 motif.

  15. N-[5-Methyl-2-(2-nitro-phen-yl)-4-oxo-1,3-thia-zolidin-3-yl]pyridine-3-carboxamide monohydrate.

    Science.gov (United States)

    Akkurt, Mehmet; Celik, Ismail; Demir, Hale; Ozkırımlı, Sumru; Büyükgüngör, Orhan

    2011-01-08

    In the title compound, C(16)H(14)N(4)O(4)S·H(2)O, the benzene and pyridine rings make a dihedral angle of 85.8 (1)°. Both enanti-omers of the chiral title compound are statistically disordered over the same position in the unit cell. The methyl and carbonyl group attached to the stereogenic center (C(5) of the thia-zolidine ring) were therefore refined with common site-occupation factors of 0.531 (9) and 0.469 (9), respectively, for each stereoisomer. In the crystal, inter-molecular N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds link the mol-ecules, forming a three-dimensional supra-molecular network. The crystal structure further shows π-π stacking inter-actions [centroid-centroid distance = 3.5063 (13) Å] between the pyridine rings.

  16. Gaseous byproducts from high-temperature thermal conversion elemental analysis of nitrogen- and sulfur-bearing compounds with considerations for δ2H and δ18O analyses.

    Science.gov (United States)

    Hunsinger, Glendon B; Tipple, Christopher A; Stern, Libby A

    2013-07-30

    High-temperature, conversion-reduction (HTC) systems convert hydrogen and oxygen in materials into H2 and CO for δ(2)H and δ(18)O measurements by isotope ratio mass spectrometry. HTC of nitrogen- and sulfur-bearing materials produces unintended byproduct gases that could affect isotope analyses by: (1) allowing isotope exchange reactions downstream of the HTC reactor, (2) creating isobaric or co-elution interferences, and (3) causing deterioration of the chromatography. This study characterizes these HTC byproducts. A HTC system (ThermoFinnigan TC/EA) was directly connected to a gas chromatograph/quadrupole mass spectrometer in scan mode (m/z 8 to 88) to identify the volatile products generated by HTC at conversion temperatures of 1350 °C and 1450 °C for a range of nitrogen- and sulfur-bearing solids [keratin powder, horse hair, caffeine, ammonium nitrate, potassium nitrate, ammonium sulfate, urea, and three nitrated organic explosives (PETN, RDX, and TNT)]. The prominent HTC byproduct gases include carbon dioxide, hydrogen cyanide, methane, acetylene, and water for all nitrogen-bearing compounds, as well as carbon disulfide, carbonyl sulfide, and hydrogen sulfide for sulfur-bearing compounds. The 1450 °C reactor temperature reduced the abundance of most byproduct gases, but increased the significant byproduct, hydrogen cyanide. Inclusion of a post-reactor chemical trap containing Ascarite II and Sicapent, in series, eliminated the majority of byproducts. This study identified numerous gaseous HTC byproducts. The potential adverse effects of these gases on isotope ratio analyses are unknown but may be mitigated by higher HTC reactor temperatures and purifying the products with a purge-and-trap system or with chemical traps. Published in 2013. This article is a U.S. Government work and is in the public domain in the USA.

  17. Solid-state synthesis, structure and properties of a novel open-framework cadmium selenite bromide: [Cd10(SeO3)8Br4]·HBr·H2O

    International Nuclear Information System (INIS)

    Chen, Wen-Tong; Wang, Ming-Sheng; Wang, Guan-E; Chen, Hui-Fen; Guo, Guo-Cong

    2013-01-01

    A novel open-framework cadmium selenite bromide, [Cd 10 (SeO 3 ) 8 Br 4 ]·HBr·H 2 O (1), has been obtained by a solid-state reaction at 450 °C, and the structure has been determined by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in Pbcm of the orthorhombic system: a=10.882(3), b=16.275(5), c=18.728(6) Å, V=3317(2) Å 3 , R1/wR2=0.0411/0.0659. Compound 1 is characteristic of a novel 3-D open-framework structure, composing ∞ 2 [CdSeO 3 ] layers and the pillars of edge-shared CdO 3 Br 2 square pyramids. The lattice water molecules and the HBr molecules locate in the voids of the framework. Optical absorption spectrum of 1 reveals the presence of an optical gap of 1.65 eV. Solid-state photoluminescent study indicates that compound 1 exhibits strong violet emission. TG–DSC measurement shows that compound 1 is thermally stable up to 200 °C. - Graphical abstract: A metal selenite halide has been synthesized and features a 3-D open-framework structure, composing edge-shared CdO 8 decahedra and pillars of edge-sharing pentahedra. UV–vis, TG–DSC and luminescent measurements are also reported. Highlights: • This paper reports a novel cadmium selenite bromide obtained by an intermediate-temperature solid-state reaction. • The title compound is characteristic of a novel 3-D open-framework structure, composing ∞ 2 [CdSeO 3 ] layers and the pillars of edge-shared CdO 3 Br 2 square pyramids. • The title compound is thermally stable up to 200 °C. • The title compound has an optical gap of 1.65 eV and exhibits strong violet emission

  18. 1-Methyl-3-(2-methylphenyl-4-phenyl-1H-pyrazolo[3,4-d]pyrimidine

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    Mohamed El Hafi

    2017-10-01

    Full Text Available In the title compound, C19H16N4, the pyrazolopyrimidine unit is slightly twisted. A combination of π-stacking and offset π-stacking interactions forms columns along the b-axis direction.

  19. 1,1′-Binaphthyl-2,2′-dicarboxylic acid–urea (1/1

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    Edwin Weber

    2008-10-01

    Full Text Available In the title co-crystal, C22H14O4·CH4N2O, the 1,1′-binaphthyl-2,2′-dicarboxylic acid (BNDA and urea molecules are connected via a system of hydrogen bonds into a chiral two-dimensional polymeric structure parallel to the (001 plane. As the crystal is centrosymmetric, it consists of alternately stacked BNDA–urea layers of opposite chirality. The urea H atoms trans to the C=O group are bonded in a chelating mode [R12(6] to the carbonyl O atom from one of the carboxylic acid groups which, in turn, acts as the donor of an O—H...O hydrogen bond to another urea molecule. The [010] chains thus formed are further connected via an R22(8 hydrogen-bond motif formed between urea and the second carboxylic acid group of BNDA.

  20. Immunological response induced by cryoablation against murine H22 hepatoma cell line in vivo.

    Science.gov (United States)

    Yang, Xueling; Li, Xiaoli; Guo, Zhi; Si, Tongguo; Yu, Haipeng; Xing, Wenge

    2018-02-01

    To describe immunological consequences induced by cryoablation against H22 cells in vivo. Adult BALB/c mice underwent subcutaneous implantation of H22 cells. All of them were assigned into three groups randomly: group A (false surgery), group B (cryoablation) and group C (cryoablation plus Freund's adjuvant). Animals were sacrificed 1, 2 and 3 weeks after treatment. Serum IFN-γ and IL-4, Th1/Th2 in spleens and cytotoxicity were detected. Compared with that of group A, (1) INF-γ of group B was higher, but IL-4 was lower; cryoablation plus Freund's adjuvant enhanced these effects. (2) Th1/Th2 rose significantly in both group B and group C. (3) Strong cytolytic activity against H22 cells of group B and group C was found on day 7, 14 and 21. Our study showed a marked shift toward Th1 and IFN-γ expression after cryoablation, with an immuno-stimulatory effect against murine H22 hepatoma Cell. Copyright © 2017. Published by Elsevier Inc.