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Sample records for title compound c7h7no3

  1. Investigation of ZnI2-KI-C3H7NO system by ultrasonic method

    International Nuclear Information System (INIS)

    Shevchenko, V.M.; Surovtsev, V.I.; Gorenbejn, E.Ya.

    1975-01-01

    Applicability of the ultrasonic impulses for the research of complex formation in the solutions was demonstrated using ZnI 2 -KI-C 3 H 7 NO system as an example. Changing the solvent structure during complexing was studied. It was determined that ion solvation numbers reflect electrostriction influence of ions on the surrounding solvent moleculas. The maximum effect on dimethylformamide (C 3 H 7 NO) was made by the complex compound KZnI 3 acting as destrictor and the sound speed decrease was the highest in its solution. Possibility of using adiabatic compressibility of the solutions for complexing studies is analysed

  2. 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.

  3. The Co-III-C bond in (1-thia-4,7-diazacyclodecyl-kappa N-3(4),N-7,C-10)(1,4,7-triazacyclononane-kappa N-3(1),N-4,N-7)-cobalt(III) dithionate hydrate

    DEFF Research Database (Denmark)

    Harris, Pernille; Kofod, P.; Song, Y.S.

    2003-01-01

    In the title compound, [Co(C6H15N3)(C7H15N2S)]S2O6.H2O, the Co-C bond distance is 1.9930 (13) Angstrom, which is shorter than for related compounds with the linear 1,6-diamino-3-thiahexan-4-ide anion in place of the macrocyclic 1-thia-4,7-diazacyclodecan-8-ide anion. The coordinated carbanion pro...... produces an elongation of 0.102 (7) Angstrom of the Co-N bond to the 1,4,7-triazacyclononane N atom in the trans position. This relatively small trans influence is presumably a result of the triamine ligand forming strong bonds to the Co-III atom....

  4. (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.

  5. 2,2,7-Trichloro-3,4-dihydronaphthalen-1(2H-one

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    Ben Capuano

    2009-09-01

    Full Text Available The title compound, C10H7Cl3O, obtained as a major byproduct from a classical Schmidt reaction. The cyclohexyl ring is distorted from a classical chair conformation, as observed for monocyclic analogues, presumably due to conjugation of the planar annulated benzo ring and the ketone group (r.m.s. deviation 0.024 Å. There are no significant intermolecular interactions.

  6. 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.

  7. NQRS Data for C7H8Cl3Osb (Subst. No. 1005)

    Science.gov (United States)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C7H8Cl3OSb (Subst. No. 1005)

  8. 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.

  9. Nqrs Data for C6H7F7N2OSb2 (Subst. No. 0880)

    Science.gov (United States)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C6H7F7N2OSb2 (Subst. No. 0880)

  10. (1S,3S,8R,9S,10R-9,10-Epoxy-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodecane

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    Abdoullah Bimoussa

    2014-04-01

    Full Text Available The title compound, C16H26O, was synthesized by treating (1S,3S,8R-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodec-9-ene with metachloroperbenzoic acid. The molecule is built up from two fused six- and seven-membered rings. The six-membered ring has a half-chair conformation, whereas the seven-membered ring displays a boat conformation. In the crystal, there are no significant intermolecular interactions present.

  11. 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

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    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.

  12. 7-Chloro-4-oxo-4H-chromene-3-carbaldehyde

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    Yoshinobu Ishikawa

    2014-08-01

    Full Text Available In the title compound, C10H5ClO3, a chlorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. deviation = 0.0592 Å for all non-H atoms, with the largest deviation from the least-squares plane [0.1792 (19 Å] being for the chromone-ring carbonyl O atom. In the crystal, molecules are linked through C—H...O hydrogen bonds to form tetrads, which are assembled by stacking interactions [centroid–centroid distance between the pyran rings = 3.823 (3 Å] and van der Waals contacts between the Cl atoms [Cl...Cl = 3.4483 (16 Å and C—Cl...Cl = 171.73 (7°] into a three-dimensional architecture.

  13. 7,7′-(3,3′-Dibenzyl-3H,3H-4,4′-bi-1,2,3-triazole-5,5′-diylbis(4-methyl-2H-chromen-2-one

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    Michael J. Ferguson

    2008-10-01

    Full Text Available The title compound, a bis-5,5′-triazole, C38H28N6O4, was observed as a side-product from the Sharpless–Meldal click reaction of the corresponding coumarin alkyne and benzylazide. Although the compound was present as a minor component, it crystallized in preference to the major product. The two triazole rings are almost orthogonal to each other [dihedral angle = 83.8 (1°]. However the 4 and 4′ coumarin systems are close to coplanar with their respective triazole rings [23.6 (1 and 15.1 (1°]. Each of the benzene rings packs approximately face-to-face with the opposing coumarin ring systems, with interplanar angles of 7.7 (1 and 25.3 (1° and distances of 3.567 (2 and 3.929 (2 Å between the respective centroids of the opposing rings.

  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. (3R,4R,4aS,7aR,12bS-3-Cyclopropylmethyl-4a,9-dihydroxy-3-methyl-7-oxo-2,3,4,4a,5,6,7,7a-octahydro-1H-4,12-methanobenzofuro[3,2-e]isoquinolin-3-ium bromide

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    Xiangfeng Chen

    2012-02-01

    Full Text Available The title compound, C21H26NO4+·Br−, also known as R-methylnaltrexone (MNTX bromide, is a selective peripherally acting μ-opioid receptor antagonist with a oroxymorphone skeleton, synthesized by hydroxyl protection, N-methylation, deprotection and anion exchange of naltrexone. It comprises a five-ring system A/B/C/D/E. Rings C and E adopt distorted chair conformations, whereas ring D is in half-chair conformation. The C/E ring junctions are trans fused. The dihedral angle between rings D and E is 82.3 (1°, while the dihedral angles between the planes of rings C and A, and rings D and E are respectively 81.7 (1, 75.9 (1 and 12.2 (1°. In the crystal, molecules are linked by O—H...Br hydrogen bonds.

  16. 5′-Methylsulfanyl-4′-oxo-7′-phenyl-3′,4′-dihydro-1′H-spiro[cyclohexane-1,2′-quinazoline]-8′-carbonitrile dimethylformamide monosolvate

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    Xuan Liu

    2011-08-01

    Full Text Available In the title compound, C21H21N3OS·C3H7NO, the carbonitrile molecule is built up of two fused six-membered rings and one six-membered ring linked through a spiro C atom. The 1,3-diaza ring adopts an envelope conformation and the cyclohexane ring adopts a chair conformation. The dihedral angle between the aromatic rings is 46.7 (3°. In the crystal, the components are linked by N—H...O hydrogen bonds.

  17. Crystal structure of 1-isopropyl-4,7-dimethyl-3-nitronaphthalene

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    Ahmed Benharref

    2015-09-01

    Full Text Available The title compound, C15H17NO2, was synthesized from a mixture of α-himachalene (2-methylene-6,6,9-trimethylbicyclo[5.4.01,7]undec-8-ene and β-himachalene (2,6,6,9-tetramethylbicyclo[5.4.01,7]undeca-1,8-diene, which were isolated from an oil of the Atlas cedar (Cedrus Atlantica. The naphthalene ring system makes dihedral angles of 68.6 (2 and 44.3 (2°, respectively, with its attached isopropyl C/C/C plane and the nitro group. In the crystal, molecules held together by a C—H...O interaction, forming a chain along [-101].

  18. Tris(dibenzoylmethanido-κ2O,O′[(6S,8S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-κ2N,N′]gadolinium(III

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    Xi-Li Li

    2009-09-01

    Full Text Available In the title compound, [Gd(C15H11O23(C17H18N2], the GdIII atom is coordinated by six O atoms from three β-diketonate ligands and two N atoms from a chiral ligand LS,S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline, in a coordination geometry best described as distorted square-antiprismatic.

  19. Crystal structure of tetraaquabis(1,3-dimethyl-2,6-dioxo-7H-purin-7-ido-κN7cobalt(II

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    Hicham El Hamdani

    2017-09-01

    Full Text Available The title complex, [Co(C7H7N4O22(H2O4], comprises mononuclear molecules consisting of a CoII ion, two deprotonated theophylline ligands (systematic name: 1,3-dimethyl-7H-purine-2,6-dione and four coordinating water molecules. The CoII atom lies on an inversion centre and has a slightly distorted octahedral coordination environment, with two N atoms of two trans-oriented theophylline ligands and the O atoms of four water molecules. An intramolecular hydrogen bond stabilizes this conformation. A three-dimensional supramolecular network structure is formed by intermolecular O—H...O and O—H...N hydrogen bonds.

  20. 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.

  1. Synthesis, spectroscopic, structural and thermal characterizations of [(C7H6NO42TeBr6·4H2O

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    S. Smaoui

    2018-02-01

    Full Text Available Tellurium (IV complexes with pyridine-2,6-dicarboxylate ligand were synthesized by slow evaporation from aqueous solutions yielding a new compound: [(C7H6NO42TeBr6·4H2O]. The structure of this compound was solved and refined by single-crystal X-ray diffraction. The compound is centrosymmetric P21/c (N°: 14 with the parameters a = 8.875(5 Å, b = 15.174(5 Å, c = 10.199(5 Å, β = 94.271° (5 and Z = 2. The structure consists of isolated H2O, isolated [TeBr6]2− octahedral anions and (pyridine-2,6-dicarboxylate [C7H6NO4]+ cations. The stability of the structure was ensured by ionic and hydrogen bonding contacts (N–H⋯Br and O–H⋯Br and Van-Der Walls interaction. The thermal decomposition of the compound was studied by thermogravimetric analysis (TGA and differential scanning calorimetry (DSC. The FTIR and Raman spectroscopy at different temperatures confirm the existence of vibrational modes that correspond to the organic, inorganic and water molecular groups. Additionally, the UV–Vis diffuse reflectance spectrum was recorded in order to investigate the band gap nature. The measurements show that this compound exhibits a semiconducting behavior with an optical band gap of 2.66 eV.

  2. Photodissociation of C3H5Br and C4H7Br at 234 nm

    International Nuclear Information System (INIS)

    Kim, Hyun Kook; Paul, Dababrata; Hong, Ki Ryong; Cho, Ha Na; Kim, Tae Kyu; Lee, Kyoung Seok

    2012-01-01

    The photodissociation dynamics of cyclopropyl bromide (C-3H 5 Br) and cyclobutyl bromide (C 4 H 7 Br) at 234 nm was investigated. A two-dimensional photofragment ion-imaging technique coupled with a [2+1] resonance enhanced multiphoton ionization scheme was utilized to obtain speed and angular distributions of the nascent Br( 2 P 3/2 ) and Br*( 2 P 1/2 ) atoms. The recoil anisotropies for the Br and Br* channels were measured to be βBr = 0.92 ± 0.03 and βBr* = 1.52 ± 0.04 for C 3 H 5 Br and βBr = 1.10 ± 0.03 and βBr* = 1.49 ± 0.05 for C 4 H 7 Br. The relative quantum yield for Br was found to be ΦBr = 0.13 ± 0.03 and for C 3 H 5 Br and C 4 H 7 Br, respectively. The soft radical limit of the impulsive model adequately modeled the related energy partitioning. The nonadiabatic transition probability from the 3A' and 4A' potential energy surfaces was estimated and discussed

  3. 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.

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

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    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

  5. Thermal decomposition of heavy rare-earth butanoates, Ln(C3H7CO2)3 (Ln = Er, Tm, Yb and Lu) in argon

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Yue, Zhao; Tang, Xiao

    2016-01-01

    was observed in all four compounds, but its course depends on the rare-earth element. Decomposition to sesquioxides proceeds via the formation of dioxymonocarbonates (Ln2O2CO3) and release of 4-heptanone (C3H7COC3H7) as well as carbon dioxide (CO2) without evidence for an intermediate oxobutanoate stage...... of Ln2O2CO3 and Ln2O3. The stability of this intermediate state seems to decrease with the mass of the rare-earth elements. Complete conversion to Ln2O3 is reached at about 1100 °C. The overall thermal decomposition behaviour of the title compounds is different from previous reports for other rare....... During the decomposition of Ln2O2CO3 into the respective sesquioxides (Ln2O3), an intermediate plateau extending from approximately 550 to 850 °C appears in the TG traces. The overall composition during this stage corresponds approximately to Ln2O2.8(CO3)0.2, but the state is more probably a mixture...

  6. Rhodium(III)- and iridium(III)-catalyzed C7 alkylation of indolines with diazo compounds.

    Science.gov (United States)

    Ai, Wen; Yang, Xueyan; Wu, Yunxiang; Wang, Xuan; Li, Yuanchao; Yang, Yaxi; Zhou, Bing

    2014-12-22

    A Rh(III)-catalyzed procedure for the C7-selective C-H alkylation of various indolines with α-diazo compounds at room temperature is reported. The advantages of this process are: 1) simple, mild, and pH-neutral reaction conditions, 2) broad substrate scope, 3) complete regioselectivity, 4) no need for an external oxidant, and 5) N2 as the sole byproduct. Furthermore, alkylation and bis-alkylation of carbazoles at the C1 and C8 positions have also been developed. More significantly, for the first time, a successful Ir(III)-catalyzed intermolecular insertion of arene C-H bonds into α-diazo compounds is reported. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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    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.

  8. (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

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    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°.

  9. B7-H3 is a potent inhibitor of human T cell activation: No evidence for B7-H3 and TREML2 interaction

    Science.gov (United States)

    Leitner, Judith; Klauser, Christoph; Pickl, Winfried F.; Stöckl, Johannes; Majdic, Otto; Bardet, Anaïs F.; Kreil, David P.; Dong, Chen; Yamazaki, Tomohide; Zlabinger, Gerhard; Pfistershammer, Katharina; Steinberger, Peter

    2010-01-01

    B7-H3 belongs to the B7 superfamily, a group of molecules that costimulate or down-modulate T cell responses. Although it was shown that B7-H3 can inhibit T cell responses, several studies - most of them performed in murine systems - found B7-H3 to act in a costimulatory manner. In this study we have specifically addressed a potential functional dualism of human B7-H3 by assessing the effect of this molecule under varying experimental conditions as well as on different T cell subsets. We show that B7-H3 does not costimulate human T cells. In presence of strong activating signals, B7-H3 potently and consistently down-modulated human T cell responses. This inhibitory effect was evident when analyzing proliferation and cytokine production and affected naïve as well as pre-activated T cells. We furthermore demonstrate that B7-H3 - T cell interaction is characterized by an early suppression of IL-2 and that T cell inhibition can be reverted by exogenous IL-2. Since TREML2 has been recently described as costimulatory receptor of murine B7-H3 we have extensively analysed interaction of human B7-H3 with TREML2 (TLT2). In these experiments we found no evidence for such an interaction. Furthermore our data do not point to a role for murine TREML2 as a receptor for murine B7-H3. PMID:19544488

  10. 2-(5-Fluoro-3-isopropylsulfanyl-7-methyl-1-benzofuran-2-ylacetic acid

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    Hong Dae Choi

    2012-04-01

    Full Text Available The title compound, C14H15FO3S, was prepared by alkaline hydrolysis of ethyl 2-(5-fluoro-3-isopropylsulfanyl-7-methyl-1-benzofuran-2-ylacetate. In the crystal, molecules are linked via pairs of O—H...O hydrogen bonds, forming inversion dimers. These dimers are connected by weak C—H...O hydrogen bonds.

  11. 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.

  12. 5,7,12,14-Tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-diol dimethylformamide disolvate

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    Mohammad Nozari

    2016-07-01

    Full Text Available The crystal lattice of the title compound, C34H22O2·2C3H7NO, at 173 K has monoclinic (P21/n symmetry. Molecules are located on crystallographic centers of symmetry and have approximate non-crystallographic mmm symmetry, indicating that in solution the chemical and spectroscopic behavior would be that of a D2h molecule. The compound has applications in gas-separation membranes fabricated from polymers of intrinsic microporosity (PIM. The compound is the product of reduction of the corresponding quinone by Na2S2O4 in DMF/NaHCO3.

  13. 5,7-Dibromo-8-methoxyquinoline

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    Ísmail Çelik

    2017-05-01

    Full Text Available In the title compound, C10H7Br2NO, the methoxy C atom deviates from the quinoline ring system (r.m.s deviation = 0.003 Å by 1.204 (4 Å. In the crystal, C—H...O hydrogen bonds link the molecules into infinite chains along the b-axis direction. Aromatic π–π stacking interactions [centroid-to-centroid distance = 3.7659 (19 Å] are also observed.

  14. Nqrs Data for C6H7F4N2OSb (Subst. No. 0879)

    Science.gov (United States)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C6H7F4N2OSb (Subst. No. 0879)

  15. rac-Ethyl 2-hydroxy-2,7,7-trimethyl-4-(4-nitrophenyl-5-oxo-3,4,5,6,7,8-hexahydro-2H-chromene-3-carboxylate

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    Konstantin A. Potekhin

    2013-01-01

    Full Text Available The title molecule, C21H25NO7, has four stereogenic centres and crystallized as a racemate. It consists of enantiomeric pairs with the relative configuration rac-(1R*,2S*,3R*. The cyclohexenone ring adopts an envelope conformation; the dimethyl-substituted C atom lies 0.640 (1 Å out of the mean plane formed by the rest of the ring atoms (r.m.s. deviation = 0.016 Å. The oxacyclohexene ring adopts a half-chair conformation, the hydroxy- and carboxyl-substituted C atoms lying −0.336 (1 and 0.419 (1 Å, respectively, out of the mean plane formed by the rest of the ring atoms (r.m.s. deviation = 0.002 Å. In the crystal, O—H...O hydrogen bonds link the molecules into a chain along the c-axis direction.

  16. 2-(5,7-Dimethyl-3-methylsulfanyl-1-benzofuran-2-ylacetic acid

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    Hong Dae Choi

    2008-08-01

    Full Text Available The title compound, C13H14O3S, was prepared by alkaline hydrolysis of ethyl 2-(5,7-dimethyl-3-methylsulfanyl-1-benzofuran-2-ylacetate. In the crystal structure, the carboxyl groups are involved in intermolecular O—H...O hydrogen bonds, which link the molecules into centrosymmetric dimers. These dimers are further packed into stacks along the a axis by weak C—H...π interactions.

  17. Ethyl (E)-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylidene)acetate

    OpenAIRE

    Oulemda Bassou; Hakima Chicha; Latifa Bouissane; El Mostapha Rakib; Mohamed Saadi; Lahcen El Ammari

    2017-01-01

    In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å), with the largest deviation from the mean plane being 0.012 (1) Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7)° between them. Two intramolecular hydrogen bonds, completing S(6) ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hy...

  18. (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

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    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.

  19. Crystal structure of 2-(1,3,7,9-tetramethyl-2,4,6,8-tetraoxo-1,2,3,4,6,7,8,9-octahydropyrido[2,3-d:6,5-d′]dipyrimidin-5-ylbenzamide dimethylformamide hemisolvate

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    Armen Ayvazyan

    2014-10-01

    Full Text Available The title compound, C20H18N6O5·0.5C3H7NO, crystallized as a dimethylformamide (DMF solvate. In the main molecule, the dihedral angle between the pyridodipyrimidine fused-ring system and the benzamide substituent is 82.26 (11°. In the crystal, the benzamide molecules are linked by N—H...O hydrogen bonds to generate tetramers with an approximate square-prismatic shape, which appears to correlate with the tetragonal crystal symmetry. The DMF molecule is disordered about a crystallographic twofold axis and accepts a C—H...O interaction from the benzamide molecule.

  20. 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.

  1. 7-epi-griffonilide, a new lactone from Bauhinia pentandra: complete "1H and "1"3C chemical shift assignments

    International Nuclear Information System (INIS)

    Almeida, Macia C.S. de; Souza, Luciana G.S.; Ferreira, Daniele A.; Pinto, Francisco C.L.; Santiago, Gilvandete M.P.; Monte, Francisco J.Q.; Lemos, Telma L.G.; Oliveira, Debora R. de; Braz-Filho, Raimundo

    2017-01-01

    A new lactone, 7-epi-griffonilide (1), and six known compounds, 2, 3a - 3c, 4a and 4b, were isolated from the leaves of Bauhinia pentandra (Fabaceae). The structures elucidation of 1 and 2 were based on detailed 2D NMR techniques and spectral comparison with related compounds, leading to complete assignment of the "1H and "1"3C NMR spectra. (author)

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

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    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. (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.

  4. Systems Li2B4O7 (Na2B4O7, K2B4O7)-N2H3H4OH-H2O at 25 deg C

    International Nuclear Information System (INIS)

    Skvortsov, V.G.; Sadetdinov, Sh.V.; Akimov, V.M.; Mitrasov, Yu.N.; Petrova, O.V.; Klopov, Yu.N.

    1994-01-01

    Phase equilibriums in the Li 2 B 4 O 7 (Na 2 B 4 O 7 , K 2 B 4 O 7 )-N 2 H 3 H 4 OH-H 2 O systems were investigated by methods of isothermal solubility, refractometry and PH-metry at 25 deg C for the first time. Lithium and sodium tetraborates was established to form phases of changed composition mM 2 B 4 O 7 ·nN 2 H 3 C 2 H 4 OH·XH 2 O, where M=Li, Na with hydrazine ethanol. K 2 B 4 O 7 ·4H 2 O precipitates in solid phase in the case of potassium salt. Formation of isomorphous mixtures was supported by X-ray diffraction and IR spectroscopy methods

  5. Crystal structures of 2-methoxyisoindoline-1,3-dione, 1,3-dioxoisoindolin-2-yl methyl carbonate and 1,3-dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-2-yl methyl carbonate: three anticonvulsant compounds

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    Fortune Ezemobi

    2014-12-01

    Full Text Available The title compounds, C9H7NO3, (1, C10H7NO5, (2, and C14H9NO5, (3, are three potentially anticonvulsant compounds. Compounds (1 and (2 are isoindoline derivatives and (3 is an isoquinoline derivative. Compounds (2 and (3 crystallize with two independent molecules (A and B in their asymmetric units. In all three cases, the isoindoline and benzoisoquinoline moieties are planar [r.m.s. deviations are 0.021 Å for (1, 0.04 and 0.018 Å for (2, and 0.033 and 0.041 Å for (3]. The substituents attached to the N atom are almost perpendicular to the mean planes of the heterocycles, with dihedral angles of 89.7 (3° for the N—O—Cmethyl group in (1, 71.01 (4 and 80.00 (4° for the N—O—C(=OO—Cmethyl groups in (2, and 75.62 (14 and 74.13 (4° for the same groups in (3. In the crystal of (1, there are unusual intermolecular C=O...C contacts of 2.794 (1 and 2.873 (1 Å present in molecules A and B, respectively. There are also C—H...O hydrogen bonds and π–π interactions [inter-centroid distance = 3.407 (3 Å] present, forming slabs lying parallel to (001. In the crystal of (2, the A and B molecules are linked by C—H...O hydrogen bonds, forming slabs parallel to (10-1, which are in turn linked via a number of π–π interactions [the most significant centroid–centroid distances are 3.4202 (7 and 3.5445 (7 Å], forming a three-dimensional structure. In the crystal of (3, the A and B molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure, which is consolidated by π–π interactions [the most significant inter-centroid distances are 3.575 (3 and 3.578 (3 Å].

  6. 4-(4-Bromophenyl-7,7-dimethyl-2-methylamino-3-nitro-7,8-dihydro-4H-chromen-5(6H-one including an unknown solvate

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    S. Antony Inglebert

    2014-05-01

    Full Text Available In the title compound, C18H19BrN2O4, the chromene unit is not quite planar (r.m.s. deviation = 0.199 Å, with the methyl C atoms lying 0.027 (4 and 1.929 (4 Å from the mean plane of the chromene unit. The six-membered carbocyclic ring of the chromene moiety adopts an envelope conformation, with the dimethyl-substituted C atom as the flap. The methylamine and nitro groups are slightly twisted from the chromene moiety, with C—N—C—O and O—N—C—C torsion angles of 2.7 (4 and −0.4 (4°, respectively. The dihedral angle between the mean plane of the chromene unit and the benzene ring is 85.61 (13°. An intramolecular N—H...O hydrogen bond generates an S(6 ring motif, which stabilizes the molecular conformation. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming hexagonal rings lying parallel to the ab plane. A region of disordered electron density, most probably disordered ethanol solvent molecules, occupying voids of ca 432 Å3 for an electron count of 158, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement.

  7. 5-Fluoro-6′H,7H,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.

  8. Synthesis, characterization, DNA-binding, and DNA-photocleavage properties of [Co(bpy)2(7-NO2-dppz)]3+, [Co(dmb)2(7-NO2-dppz)]3+, and [Co(phen)2(7-NO2-dppz)]3+ complexes: (7-nitro-dppz = 7-nitro dipyrido[3,2-a:2'-3'-c]phenazine; bpy = 2,2'-bipyridine; dmb = 4,4'-dimethyl-2,2'-bipyridine; phen = 1,10-phenanthroline) and their toxicity on different microorganisms.

    Science.gov (United States)

    Reddy, Kotha Laxma; Reddy, Y Harish Kumar; Kumar, K Ashwini; Vidhisha, S; Satyanarayana, S

    2009-03-01

    The polypyridyl ligand 7-Nitro dipyrido[3,2-a:2'-3'-c]phenazine (7-Nitro-dppz) and its complexes [Co(bpy)(2)(7-NO(2)-dppz)](3+)(1) (bpy = 2,2'-bipyridine), [Co(dmb)(2)(7-NO(2)-dppz)](3+)(2), (dmb = 4,4'-dimethyl-2,2'-bipyridine), and [Co(phen)(2)(7-NO(2)-dppz)](3+)(3) (phen = 1,10-phenanthroline) were synthesized and characterized by UV/VIS, IR, elemental analysis, (1)H and (13)C-NMR, and mass spectra. The binding properties of the three complexes to CT-DNA were investigated by different spectroscopic methods and viscosity measurements and DNA cleavage assay. The experimental results suggest that these complexes bind to CT-DNA through an intercalative mode. Also, the three complexes promote the photocleavage of plasmid pBR-322 DNA under irradiation. Toxicological effects of the selected complexes were estimated with different microorganisms.

  9. 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].

  10. 2-Hydroxy-1,6,7,8-tetramethoxy-3-methylanthraquinone

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    Shu-Juan Yu

    2008-02-01

    Full Text Available The title compound, C19H18O7, also known as chrysoobtusin, was isolated from Cassia tora L. (Leguminosae. The anthraquinone ring system is almost planar, the dihedral angle between the two benzene rings being 4.27 (4°. The structure is stabilized by intra- and intermolecular O—H...O and C—H...O hydrogen bonds, and by weak π–π stacking interactions along the b axis, with a centroid–centroid distance between related benzene rings of 3.800 (4 Å.

  11. Crystal structure, quantum mechanical investigation, IR and NMR spectroscopy of two new organic salts: (C8H12NO)·[NO3] (I) and (C8H14N4)·[ClO4]2 (II)

    Science.gov (United States)

    Bayar, I.; Khedhiri, L.; Soudani, S.; Lefebvre, F.; Pereira da Silva, P. S.; Ben Nasr, C.

    2018-06-01

    Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C8H12NO)·[NO3] (I), and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C8H14N4)·[ClO4]2(II), have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a = 15.7908 (7), b = 6.8032 (3), c = 8.7091 (4) Å, V = 935.60 (7) Å3 with Z = 4. Full-matrix least-squares refinement converged at R = 0.038 and wR(F2) = 0.115. Compound (II) belongs to the monoclinic system, space group P21/c with the following parameters: a = 10.798(2), b = 7.330(1), c = 21.186(2) Å, β = 120.641 (4)°, V = 1442.7 (3) Å3and Z = 4. The structure was refined to R = 0.044, wR(F2) = 0.132. In the structures of (I) and (II), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. 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.

  12. (5S,6R-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2H-cyclopenta[b]pyran-7-one

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    Winai Ieawsuwan

    2011-10-01

    Full Text Available The title compound, C15H15BrO2, was synthesized by a Brønsted acid-catalysed domino electrocyclization-halogenation reaction. The five-membered ring is essentially planar (r.m.s. deviation 0.006 Å and forms a dihedral angle of 72.7 (3° with the attached phenyl ring. The six-membered heterocycle adopts a half-chair conformation. The crystal packing is stabilized by a C—H...O contact.

  13. 3′,7′,7′-Trimethyl-1′-phenyl-5′,6′,7′,8′-tetrahydrospiro[indoline-3,4′-(1H,4H-pyrazolo[3,4-b]chromene]-2,5′-dione

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    Li-Qin Zhao

    2010-12-01

    Full Text Available The title spirooxindole compound, C26H23N3O3, was prepared by the reaction of isatin, 3-methyl-1-phenyl-2-pyrazolin-5-one and 5,5-dimethylcyclohexane-1,3-dione in an ethanol solution. The fused cyclohexene ring adopts an envelope conformation. The dihedral angle between the aromatic and pyrazoline rings is 23.70 (8°. An intramolecular C—H...O interaction occurs. The crystal structure is stabilized by N—H...N hydrogen-bonding interactions, leading to a zigzag chain along the b axis.

  14. Ethyl (E-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylideneacetate

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    Oulemda Bassou

    2017-02-01

    Full Text Available In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å, with the largest deviation from the mean plane being 0.012 (1 Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7° between them. Two intramolecular hydrogen bonds, completing S(6 ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hydrogen bonds involving the same acceptor atom, forming chains propagating along the c-axis direction and enclosing R21(6 ring motifs. The chains are linked via offset π–π interactions [intercentroid distance = 3.622 (1 Å], involving inversion-related oxopyrano[4,3-b]pyran-4-yl ring systems, forming slabs parallel to the bc plane.

  15. Photodissociation of C{sub 3}H{sub 5}Br and C{sub 4}H{sub 7}Br at 234 nm

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hyun Kook; Paul, Dababrata; Hong, Ki Ryong; Cho, Ha Na; Kim, Tae Kyu [Pusan National University, Busan (Korea, Republic of); Lee, Kyoung Seok [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2012-01-15

    The photodissociation dynamics of cyclopropyl bromide (C-3H{sub 5}Br) and cyclobutyl bromide (C{sub 4}H{sub 7}Br) at 234 nm was investigated. A two-dimensional photofragment ion-imaging technique coupled with a [2+1] resonance enhanced multiphoton ionization scheme was utilized to obtain speed and angular distributions of the nascent Br({sup 2}P{sub 3/2}) and Br*({sup 2}P{sub 1/2}) atoms. The recoil anisotropies for the Br and Br* channels were measured to be βBr = 0.92 ± 0.03 and βBr* = 1.52 ± 0.04 for C{sub 3}H{sub 5}Br and βBr = 1.10 ± 0.03 and βBr* = 1.49 ± 0.05 for C{sub 4}H{sub 7}Br. The relative quantum yield for Br was found to be ΦBr = 0.13 ± 0.03 and for C{sub 3}H{sub 5}Br and C{sub 4}H{sub 7}Br, respectively. The soft radical limit of the impulsive model adequately modeled the related energy partitioning. The nonadiabatic transition probability from the 3A' and 4A' potential energy surfaces was estimated and discussed.

  16. 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

  17. 2′-Hydroxymethyl-1′-(4-methylphenyl-2′-nitro-1′,2′,5′,6′,7′,7a′-hexahydrospiro[indoline-3,3′-pyrrolizin]-2-one

    Directory of Open Access Journals (Sweden)

    S. Sathya

    2012-02-01

    Full Text Available In the title compound, C22H23N3O4, the tolyl ring is almost perpendicular [83.86 (7°] to the best plane through the eight atoms of the pyrrolizidine ring system. The molecular conformation is stabilized by an intramolecular O—H...O hydrogen bond. The crystal packing features inversion dimers with R22(8 motifs linked by pairs of N—H...O hydrogen bonds.

  18. Solvothermal synthesis, crystal structure, and second-order nonlinear optical properties of a new noncentrosymmetric gallium-organic framework material, [N(C3H7)4]3Ga3[C6H3(CO2)3]4

    Science.gov (United States)

    Lee, Dong Woo; Jo, Vinna; Ok, Kang Min

    2012-10-01

    A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C3H7)4]3Ga3[C6H3(CO2)3]4 (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO3)3·xH2O, 1,3,5-C6H3(CO2H)3, N(C3H7)4Cl, HNO3, and HCON(CH3)2 at 180 °C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO4 tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of α-SiO2 and the material is phase-matchable (type-1).

  19. 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.

  20. (1S,3R,8S,9R,10S-2,2-Dichloro-3,7,7,10-tetramethyl-9,10-epoxytricyclo[6.4.0.01,3]dodecane

    Directory of Open Access Journals (Sweden)

    Moha Berraho

    2010-12-01

    Full Text Available The title compound, C16H24Cl2O, was synthesized from β-himachalene (3,5,5,9-tetramethyl-2,4a,5,6,7,8-hexahydro-1H-benzocycloheptene, which was isolated from the essential oil of the Atlas cedar (cedrus atlantica. The molecule forms an extended sheet of two fused rings which exhibit different conformations. The six-membered ring has a half-chair conformation, while the seven-membered ring displays a chair conformation; the dihedral angle between the two rings is 38.2 (1°.

  1. Copper(II) perrhenate Cu(C{sub 3}H{sub 7}OH){sub 2}(ReO{sub 4}){sub 2}: Synthesis from isopropanol and CuReO{sub 4}, structure and properties

    Energy Technology Data Exchange (ETDEWEB)

    Mikhailova, D., E-mail: d.mikhailova@ifw-dresden.de [Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-Helmholtz-Platz 1, D-76434 Eggenstein-Leopoldshafen (Germany); Institute for Complex Materials, IFW Dresden, Helmholtzstrasse 20, D-01069 Dresden (Germany); Max Planck Institute for Chemical Physics of Solids, Nöthnitzer Str. 40, D-01187 Dresden (Germany); Engel, J.M. [Materials Science, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt (Germany); Schmidt, M. [Max Planck Institute for Chemical Physics of Solids, Nöthnitzer Str. 40, D-01187 Dresden (Germany); Tsirlin, A.A. [National Institute of Chemical Physics and Biophysics, Akadeemia tee 23, 12618 Tallinn (Estonia); Ehrenberg, H. [Karlsruhe Institute of Technology (KIT), Institute for Applied Materials (IAM), Hermann-von-Helmholtz-Platz 1, D-76434 Eggenstein-Leopoldshafen (Germany); Materials Science, Technische Universität Darmstadt, Alarich-Weiss-Str. 2, D-64287 Darmstadt (Germany)

    2015-12-15

    The crystal structure of Cu{sup +}Re{sup 7+}O{sub 4} is capable of a quasi-reversible incorporation of C{sub 3}H{sub 7}OH molecules. A room-temperature reaction between CuReO{sub 4} and C{sub 3}H{sub 7}OH under oxidizing conditions leads to the formation of a novel metal-organic hybrid compound Cu{sup 2+}(C{sub 3}H{sub 7}OH){sub 2}(ReO{sub 4}){sub 2}. Upon heating under reducing conditions, this compound transforms back into CuReO{sub 4}, albeit with ReO{sub 2} and metallic Cu as by-products. The crystal structure of Cu(C{sub 3}H{sub 7}OH){sub 2}(ReO{sub 4}){sub 2} solved from single-crystal X-ray diffraction (Pbca, a=10.005(3) Å, b=7.833(2) Å, and c=19.180(5) Å) reveals layers of corner-sharing CuO{sub 6}-octahedra and ReO{sub 4}-tetrahedra, whereas isopropyl groups are attached to both sides of these layers, thus providing additional connections within the layers through hydrogen bonds. Cu(C{sub 3}H{sub 7}OH){sub 2}(ReO{sub 4}){sub 2} is paramagnetic down to 4 K because the spatial arrangement of the Cu{sup 2+} half-filled orbitals prevents magnetic superexchange. The paramagnetic effective moment of 2.0(1) μ{sub B} is slightly above the spin-only value and typical for Cu{sup 2+} ions. - Highlights: • Novel Cu(C{sub 3}H{sub 7}OH){sub 2}(ReO{sub 4}){sub 2} compound has a sequence of inorganic and organic layers. • Hydrogen bonds provide an additional bonding Isopropanol molecules serve as a reducing agent during decomposition. • No direct Cu-O-Re-O-Cu connections via d{sub x2-y2} orbital of Cu{sup 2+} explain paramagnetism. • Hydrogen bonds provide an additional bonding. • Isopropanol molecules serve as a reducing agent during decomposition.

  2. Synthesis, crystal structure and Raman spectrum of Ba{sub 7}[BO{sub 3}]{sub 3}Br(O{sub 1.33}F{sub 1.33})

    Energy Technology Data Exchange (ETDEWEB)

    Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Dept. of Chemistry and Chemical Biology; Schulz, Armin [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

    2017-05-01

    In addition to amorphous material and Ba{sub 7}[BO{sub 3}]{sub 4-x}F{sub 2-3x}, air and moisture sensitive single crystals of Ba{sub 7}[BO{sub 3}]{sub 3}Br(O{sub 1.33}F{sub 1.33}) were formed from H{sub 3}BO{sub 3}, Ba(OH){sub 2}, BaF{sub 2} and BaBr{sub 2} . H{sub 2}O in alumina crucibles open to the atmosphere at 1300 K for 13 h. Ba{sub 7}[BO{sub 3}]{sub 3}Br(O{sub 1.33}F{sub 1.33}) crystallizes in the hexagonal space group P6{sub 3}mc (no. 186, Z=2) with the lattice parameters a=1118.1(2) and c=723.93(13) pm. The Raman spectrum of the title compounds was also acquired and is compared to literature data.

  3. Diethyl 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 heterocyclic ring in the title compound, C27H34N2O6, has an envelope conformation on one of the bridgehead C atoms [Q(2 = 0.4487 (19 Å and ϕ = 291.3 (2°]. Two strong intramolecular O—H...N hydrogen bonds stabilize the molecular conformation. The benzoate groups differ in the relative orientations of the ethyl groups, as quantified by the values of the C—O—C—C torsion angles of −86.5 (2 and −178.97 (17°. The carbonyl groups are nearly coplanar with the benzene rings, forming C—C—C—O torsion angles of 0.9 (3 and 3.4 (3°. The crystal structure is stabilized by weak intermolecular C—H...O interactions.

  4. A novel fluffy nanostructured 3D network of Ni(C7H4O5) for supercapacitors

    International Nuclear Information System (INIS)

    Chen, Qiulin; Lei, Shuijin; Chen, Lianfu; Deng, Peiqin; Xiao, Yanhe; Cheng, Baochang

    2017-01-01

    Highlights: • The fluffy 3D network of Ni(C 7 H 4 O 5 ) complex is firstly prepared on Ni foam. • The fluffy 3D network shows high areal capacitance and excellent cycle stability. • The fluffy network has large superior pseudocapacitive performance than the powder. • An asymmetric supercapacitor with high capacitance and energy density is assembled. - Abstract: Supercapacitors have raised considerable research interest in recent years due to their extensive potential application in next-generation energy storage. It is always of great importance to develop new electrode materials for supercapacitors so far. In this research, nickel gallate complex (Ni(C 7 H 4 O 5 )) nanostructures are successfully grown on nickel foam by a facile hydrothermal route, which can be directly used as the electrodes for supercapacitors. X-ray diffraction patterns show that the sample is amorphous. The scanning electron microscopy images reveal that the products consist of novel fluffy 3D network with a mass of fibers. The electrochemical measurements demonstrate that the prepared Ni(C 7 H 4 O 5 ) electrode possesses the specific capacitance of 3.688 F cm −2 (1229.3 F g −1 ) at a current density of 9 mA cm −2 (3 A g −1 ). It presents an excellent cycling stability with a capacitance retention of 87.9% after 5000 cycles even at a very high current density of 40 mA cm −2 . An asymmetric supercapacitor device is assembled using the Ni(C 7 H 4 O 5 ) sample as positive electrode and activated carbon as negative one. A high gravimetric capacitance of 71.4 F g −1 at a current density of 0.5 A g −1 can be achieved. The fabricated device delivers the highest energy density of 23.8 W h kg −1 at a power density of 388.2 W kg −1 with a voltage window of 1.55 V. This strategy should be extended to other organometallic compounds for supercapacitors.

  5. High-pressure synthesis of the first ternary melilite-type compound Sc{sub 1.67}B{sub 3}O{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Schmitt, Martin K.; Huppertz, Hubert [Institut fuer Allgemeine, Anorganische und Theoretische Chemie, Universitaet Innsbruck (Austria); Ploner, Kevin [Institut fuer Physikalische Chemie, Universitaet Innsbruck (Austria); Hejny, Clivia [Institut fuer Mineralogie und Petrographie, Universitaet Innsbruck (Austria)

    2017-12-13

    Sc{sub 1.67}B{sub 3}O{sub 7} was synthesized in a high-pressure/high-temperature experiment at 3.5 GPa/1200 C employing a Walker-type multianvil module. The compound was characterized with X-ray diffraction and vibrational spectroscopy. It crystallizes in the tetragonal, acentric space group P42{sub 1}m (no. 113) with the lattice parameters a = 6.6597(4) and c = 4.4364(3) Aa. Sc{sub 1.67}B{sub 3}O{sub 7} is the first ternary compound adopting the melilite-type structure and therefore the simplest representative of this manifold structure family. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  6. Formation of closo-rhodacarboranes with the η2,η3-(CH2=CHC5H6) ligand in the reaction of μ-dichloro-bis[(η4-norbornadiene)rhodium] with nido-dicarbaundecaborates [K][nido-7-R1-8-R2-7,8-C2B9H10

    International Nuclear Information System (INIS)

    Safronov, A.V.; Sokolova, M.N.; Vorontsov, E.V.; Petrovskij, P.V.; Barakovskaya, I.G.; Chizhevskij, I.T.

    2004-01-01

    New closo-(η 2 ,η 3 -(4-vinylcyclopentene-3-yl)rhodacarboranes were prepared by reaction of the complex [(η 4 -C 7 H 8 )RhCl] 2 (C 7 H 8 -norbornadiene) with salts of substituted nido-dicarbaundecaborates [K][nido-7-R 1 -8-R 2 -7,8-C 2 B 9 H 10 ] (R 1 =R 2 =H (a); R = R 2 =Me (b); R 1 , R 2 =1',2'-(CH 2 ) 2 C 6 H 4 (c); R 1 =Me, R 2 =Ph (d) in CH 2 Cl 2 . The structure of the compounds prepared in solution was studied by the method of multinuclear NMR spectroscopy. A probable mechanism of the norbornadiene ligand regrouping was suggested [ru

  7. Synthesis of binuclear rhodacarboranes from dianions 1,4- and 1,3-C6H4(CH2-9-C2H2B9H9-7,8-nido)22- and (Ph3P)3RhCl

    International Nuclear Information System (INIS)

    Zakharkin, L.I.; Zhigareva, G.G.

    1996-01-01

    Dianions 1,4 and 1,3-C 6 H 4 (CH 2 -9-C 2 H 2 B 9 H 9 -7,8-nido) 2 2- obtained from nido 7,8-dicarbollide-ion and 1,4-bis(bromomethyl) and 1,3-bis(bromomethyl)benzenes react with (Ph 3 P) 3 RhCl to give binuclear rhodacarboranes, 1,4- and 1,3-[3,3-(Ph 3 P) 2 -3-H-3,1,2-RhC 2 B 9 H 10 -4-CH 2 ] 2 C 6 H 6 with chemical reaction yield 85% and 87% respectively. 7 refs., 1 fig., 1 tab

  8. 2,5-Bis[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctylsulfanyl]-1,3,4-thiadiazole

    Directory of Open Access Journals (Sweden)

    Gabriel Partl

    2017-02-01

    Full Text Available The title compound, C18H8F26N2S3, was obtained by double S-perfluorohexylethylation of dipotassium 1,3,4-thiadiazole-2,5-dithiolate in methanol. The molecule exhibits twofold rotational symmetry, with the S atom lying on the rotation axis. The fluorocarbon chains adopt helical conformations and the F atoms of the two terminal C atoms are disordered over two sets of sites. No directional intermolecular interactions occur in the crystal.

  9. 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

    Directory of Open Access Journals (Sweden)

    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.

  10. 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

  11. (1R,3R,4R,6S-4-(7-Methoxy-2-oxo-2H-chromen-6-yl-1-methyl-3,6-dioxabicyclo[3.1.0]hexan-2-yl acetate

    Directory of Open Access Journals (Sweden)

    Wong Phakhodee

    2012-12-01

    Full Text Available In the title compound, C17H16O7, which was isolated from the leaves of Micromelum integerrimum, the furan ring adopts an envelope conformation with the O atom as the flap. An intramolecular C—H...O hydrogen bond occurs. The carbonyl O atom is disordered in a 0.57 (8:0.43 (8 ratio. In the crystal, molecules are linked by weak C—H...O hydrogen bonds into a C(10 chain along [010].

  12. 6,7-Dichloro-3-(2,4-dichlorobenzylquinoxalin-2(1H-one

    Directory of Open Access Journals (Sweden)

    Jinpeng Zhang

    2012-08-01

    Full Text Available In the title compound, C15H8Cl4N2O, the quinoxaline ring system is almost planar, with a dihedral angle between the benzene and pyrazine rings of 3.1 (2°. The 2,4-dichlorophenyl ring is approximately perpendicular to the pyrazine ring, with a dihedral angle of 86.47 (13° between them. The crystal packing features intermolecular N—H...O hydrogen bonds and π–π stacking interactions, with centroid–centroid distances in the range 3.699 (3–4.054 (3 Å.

  13. Identification of hepatic metabolites of two highly carcinogenic polycyclic aza-aromatic compounds, 7,9-dimethylbenz[c]acridine and 7,10-dimethylbenz[c]acridine.

    Science.gov (United States)

    Ye, Y; Duke, C C; Holder, G M

    1995-03-01

    The hepatic microsomal metabolites of the highly carcinogenic dimethylbenzacridines, 7,9-dimethylbenz[c]acridine (7,9-DMBAC), and 7,10-dimethylbenz[c]acridine (7,10-DMBAC) were obtained with preparations from 3-methylcholanthrene-pretreated rats. Metabolites were separated by reversed-phase HPLC and characterized using UV spectral data and chemical ionization-mass spectrometry after trimethylsilylation and GC. Comparisons with products formed in the presence of the epoxide hydrolase inhibitor, 1,1,1-trichloropropane 2,3-oxide and with those formed from the three synthetic alcohol derivatives of each parent compound, aided the assignment of firm or tentative structures to 16 products from 7,9-DMBAC found in 22 reversed-phase chromatographic peaks, and for 17 products of 7,10-DMBAC found in 19 chromatographic peaks. The more abundant metabolites were derived from oxidation of the methyl groups. Other metabolites were dihydrodiols, epoxides, phenols and secondary metabolites. The 9-methyl group prevented dihydrodiol formation at the 8,9-position from 7,9-DMBAC, and for each carcinogen, the 3,4-dihydrodiol was formed. As well, 3,4-dihydrodiols of methyl oxidized compounds were found.

  14. 5-(2,5-Dioxooxolan-3-yl-8-methyl-3,3a,4,5-tetrahydro-1H-naphtho[1,2-c]furan-1,3-dione

    Directory of Open Access Journals (Sweden)

    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.

  15. 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°.

  16. 6-Chloro-7-fluoro-4-oxo-4H-chromene-3-carbaldehyde

    Directory of Open Access Journals (Sweden)

    Yoshinobu Ishikawa

    2014-07-01

    Full Text Available In the title compound, C10H4ClFO3, a chlorinated and fluorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. = 0.0336 Å for the non-H atoms, with the largest deviation from the least-squares plane [0.062 (2 Å] being for a benzene-ring C atom. In the crystal, molecules are linked through stacking interactions [centroid–centroid distance between the benzene and pyran rings = 3.958 (3 Å and interplanar distance = 3.259 (3 Å], C—H...O hydrogen bonds, and short C...O contacts [2.879 (3 Å]. Unsymmetrical halogen–halogen interactions between the Cl and F atoms [Cl...F = 3.049 (3 Å, C—Cl...F = 148.10 (9° and C—F...Cl = 162.06 (13°] are also formed, giving a meandering two-dimensional network along the a axis.

  17. Ethyl 3-[7-ethoxy-6-(4-methoxybenzenesulfonamido-2H-indazol-2-yl]propanoate

    Directory of Open Access Journals (Sweden)

    Najat Abbassi

    2012-04-01

    Full Text Available In the title compound, C21H25N3O6S, the dihedral angle between the methoxybenzene and indazole rings is 74.96 (5°. The crystal packing is stabilized by an N—H...O hydrogen bond into a two-dimensional network. In addition, C—H...π interactions and a π–π contact, with a centroid–centroid distance of 3.5333 (6 Å, are observed. The crystal packing is stabilized by N—H...O and C—H...O hydrogen bonds.

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

    Directory of Open Access Journals (Sweden)

    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].

  19. 1-Allyl-3-amino-1H-pyrazole-4-carboxylic acid

    Directory of Open Access Journals (Sweden)

    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.

  20. 9-{[4-(Dimethylaminobenzyl]amino}-5-(4-hydroxy-3,5-dimethoxyphenyl-5,5a,8a,9-tetrahydrofuro[3′,4′:6,7]naphtho[2,3-d][1,3]dioxol-6(8H-one methanol monosolvate

    Directory of Open Access Journals (Sweden)

    Hong Chen

    2011-11-01

    Full Text Available In the title compound, C30H32N2O7·CH4O, the tetrahydrofuran ring and the six-membered ring fused to it both display envelope conformations, with the ring C atom opposite the carbonyl group and the adjacent bridgehead C atom as the flaps, respectively. In the crystal structure, intermolecular O—H...O hydrogen bonds link all moieties into ribbons along [010]. Weak intermolecular C—H...O interactions consolidate the crystal packing further.

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

    Directory of Open Access Journals (Sweden)

    Peng Zhang

    2008-02-01

    Full Text Available In the title heterotrinuclear coordination compound, [CaCu2(C9H4NO52(C3H4N22(H2O37H2O, 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.

  2. EPR and optical absorption studies of VO2+ doped L-alanine (C3H7NO2) single crystals

    International Nuclear Information System (INIS)

    Biyik, Recep

    2009-01-01

    VO 2+ doped L-alanine (C 3 H 7 NO 2 ) single crystals and powders are examined by electron paramagnetic resonance (EPR) and optical absorption spectroscopy. Three magnetically different sites are resolved from angular variations of L-alanine single crystal EPR spectra. In some specific orientations each VO 2+ line splits into three superhyperfine lines with intensities of 1:2:1 and maximum splitting value of 2.23 mT. The local symmetries of VO 2+ complex sites are nearly axial. The optical absorption spectra show three bands. Spin Hamiltonian parameters are measured and molecular orbital coefficients are calculated by correlating EPR and optical absorption data for the central vanadyl ion.

  3. Cationic polyhydrido cluster complexes. Crystal and molecular structures of (Ir3(Ph2P(CH2)3PPh2)3(H)7(CO))2+ and (Ir3(Ph2P(CH2)2(2-py))3(H)7)2+

    International Nuclear Information System (INIS)

    Hsienhau Wang; Casalnuovo, A.L.; Johnson, B.J.; Mueting, A.M.; Pignolet, L.H.

    1988-01-01

    Two new cationic polyhydrido cluster complexes of iridium have been synthesized and characterized by single-crystal x-ray diffraction and by ir and 1 H and 31 P NMR spectroscopy (Ir 3 (dppp) 3 (H) 7 (CO)) 2+ (2) and (Ir3 (PN) 3 (H) 7)2+ (5), where dppp = 1,3-bis(diphenylphosphino)propane and PN = 1-(2-pyridyl)-2-(diphenylphosphino)ethane, were synthesized by the reaction of CO with (Ir 3 (dppp) 3 (H) 7 ) 2+ (1) in CH 2 Cl 2 solution and H 2 with (Ir(PN)(COD)) + (4) in CH 3 OH solution, respectively. Crystal structures for both compounds is reported. The hydride positions were not located in the crystal structure analyses but were deduced from structural and 1 H NMR data. The molecular structure of 2 consists of a bilateral triangle of three iridium atoms with a carbonyl at the vertex and a chelating dppp ligand on each iridium atom. 1 H NMR data with use of acetone-d 6 as solvent showed that 2 possesses four doubly bridging hydrides and three terminal hydrides, yielding C 1 symmetry. The molecular structure of 5 consists of an approximately equilateral triangle of three iridium atoms (average Ir-Ir distance 2.746 (1) angstrom) with one PN ligand chelated to each iridium atom. 1 H NMR analysis, with use of CD 2 Cl 2 as solvent, showed that 5 has one triply bridging hydride and six terminal hydrides, giving C 3 symmetry. (Ir 3 (dppp) 3 (H) 7 (CH 3 C 6 H 4 NC)) 2+ (3) a complex structurally analogous to 2, was synthesized from 1 and p-tolyl isocyanide in CH 2 Cl 2 solution and characterized by ir and 1 H and 31 P NMR spectroscopy. 44 refs., 3 figs., 3 tabs

  4. 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)

  5. Bile acid metabolism in cirrhosis. VIII. Quantitative evaluation of bile acid synthesis from [7 beta-3H]7 alpha-hydroxycholesterol and [G-3H]26-hydroxycholesterol

    International Nuclear Information System (INIS)

    Goldman, M.; Vlahcevic, Z.R.; Schwartz, C.C.; Gustafsson, J.; Swell, L.

    1982-01-01

    In order to evaluate more definitively the observed aberrations in the synthesis of cholic and chenodeoxycholic acids in patients with advanced cirrhosis, two bile acid biosynthesis pathways were examined by determining the efficiency of conversion of [ 3 H]7 alpha-hydroxycholesterol and [ 3 H] 26-hydroxycholesterol to primary bile acids. Bile acid kinetics were determined by administration of [ 14 C]cholic and [ 14 C]chenodeoxycholic acids. Cholic acid synthesis in cirrhotic patients was markedly depressed (170 vs 927 μmoles per day)( while chenodeoxycholic acid synthesis was reduced to a much lesser degree (227 vs 550 μmoles per day). The administration of [ 3 H]7 alpha-hydroxycholesterol allowed for an evaluation of the major pathway of bile acid synthesis via the 7 alpha-hydroxylation of cholesterol. This compound was efficiently incorporated into primary bile acids by the two normal subjects (88 and 100%) and two cirrhotic patients (77 and 91%). However, the recovery of the label in cholic acid was slightly less in cirrhotic patients than in normal subjects. [ 3 H]26-hydroxycholesterol was administered to ascertain the contribution of the 26-hydroxylation pathway to bile acid synthesis. All study subjects showed poor conversion (9 to 22%) of this intermediate into bile acids. The results of this study suggest that a major block in the bile acid synthesis pathway in cirrhosis is at the level of 7 alpha-hydroxylation of cholesterol (impairment of 7 alpha-hydroxylase) and/or in the feedback triggering mechanism regulating bile acid synthesis. The data also suggest that the 26-hydroxylation pathway in normal subjects and patients with cirrhosis is a minor contributor to synthesis of the primary bile acids. Therefore, the relative sparing of chenodeoxycholic acid synthesis observed in cirrhotic patients is not due to preferential synthesis of this bile acid via the 26-hydroxylation pathway

  6. Clean to dirty limit and T c suppression in NdFeAsO0.7F0.3 studied by H c2 analysis

    Science.gov (United States)

    Pallecchi, I.; Tarantini, C.; Shen, Y.; Singh, R. K.; Newman, N.; Cheng, P.; Jia, Y.; Wen, H.-H.; Putti, M.

    2018-07-01

    In this work, we investigate the temperature dependence of the upper critical field, dH c2/dT, in an increasingly disordered NdFeAsO0.7F0.3 (NdFeAs(O,F)) single crystal that has been progressively irradiated up to a 5.25 × 1016 cm- 2 total α-particle dose. For the H∣∣ab-plane, dH c2/dT does not vary remarkably with irradiation, while for the H∣∣c-axis it increases sharply after the first irradiation of 3.60 × 1015 cm-2 and then more gradually with further irradiation doses. Focusing on the H∣∣c-axis, we develop a phenomenological analysis of the H c2 slope which allows us to inspect the crossover from the clean to the dirty regime. From the H c2 slope normalized to the critical temperature and to its clean limit value, we extract the ratio of the coherence length ξ BCS to the mean free path {\\ell } and we find that when T c is reduced by a factor of four from its pristine value, ξ BCS/{\\ell } becomes as large as ˜7 and {\\ell } reaches values of ˜1.8 nm, indicating that NdFeAs(O,F) is well into the dirty regime. Our analysis of the H c2 slope also allows us to compare the pair-breaking effectiveness of scattering in different superconductors, showing similarity between unconventional NdFeAs(O,F) and moderate-T c phonon-mediated devices, such as MgB2 and A15 compounds, but much a stronger difference with YBa2Cu3O7-δ . This work thus shows that dH c2/dT is a reliable parameter, providing an alternative to residual resistivity, for investigating the pair-breaking mechanism induced by impurity scattering in superconductors.

  7. Two ternary mixed-anion chlorides with divalent europium: Eu{sub 2}H{sub 3}Cl and Eu{sub 7}F{sub 12}Cl{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Reckeweg, Olaf [Baker Laboratory, Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853-1301 (United States); Institut fuer Anorganische Chemie, Universitaet Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart (Germany); DiSalvo, Francis J. [Baker Laboratory, Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853-1301 (United States); Wolf, Sarah; Schleid, Thomas [Institut fuer Anorganische Chemie, Universitaet Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart (Germany)

    2014-06-15

    Dark ruby-red, transparent, triangular plate-shaped single crystals of Eu{sub 2}H{sub 3}Cl and colorless, transparent, needle-shaped single crystals of Eu{sub 7}F{sub 12}Cl{sub 2} were obtained by solid-state reactions of Eu, NaH, NaCl, and Na (2:4:1:2 molar ratio) or Eu, EuCl{sub 3}, and LiF (1:1:4 molar ratio), respectively, in silica-jacketed tantalum ampoules at 900 C for 13 h. Eu{sub 2}H{sub 3}Cl crystallizes isotypically to Ba{sub 2}H{sub 3}X (X = Cl, Br, I) in the trigonal space group P anti 3m1 (no. 164) with lattice parameters a = 409.67(4) and c = 696.18(7) pm, whereas Eu{sub 7}F{sub 12}Cl{sub 2} crystallizes isotypically to Ba{sub 7}F{sub 12}Cl{sub 2} or Sr{sub 7}H{sub 12}Cl{sub 2} in the hexagonal space group P anti 6 (no. 174) with lattice parameters a = 1002.31(5) and c = 392.54(2) pm. Both compounds contain Eu{sup 2+} cations with coordination numbers as high as nine (Eu{sub 7}F{sub 12}Cl{sub 2}) and ten (Eu{sub 2}H{sub 3}Cl) with respect to the halide anions (F{sup -} or H{sup -} and Cl{sup -}). The structural results are corroborated by EUTAX and MAPLE calculations on both ternary mixed-anion europium(II) chlorides in comparison to these for related binary and ternary compounds with divalent europium. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. Ethyl 3-hydroxy-13-methyl-4′-phenyl-2′-(3,4,5-trimethoxyphenyl-6,7,8,9,11,12,13,14,15,16-decahydrospiro[cyclopenta[a]phenanthrene-16,3′-pyrrolidine]-5′-carboxylate

    Directory of Open Access Journals (Sweden)

    R. Murugan

    2008-11-01

    Full Text Available In the title compound, C39H45NO7,the pyrrolidine ring is connected to an estrone group, a trimethoxy benzene and a phenyl ring. The pyrrolidine ring exhibits a twist conformation and the other five-membered ring an envelope conformation. Molecules are linked by N—H...O hydrogen bonds, C—H...π interactions and C—H...O hydrogen bonds.

  9. 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

    Directory of Open Access Journals (Sweden)

    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.

  10. 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.

  11. Inactivation of Listeria monocytogenes, Escherichia coli O157:H7, and Salmonella typhimurium with compounds available in households.

    Science.gov (United States)

    Yang, Hua; Kendall, Patricia A; Medeiros, Lydia; Sofos, John N

    2009-06-01

    Solutions of selected household products were tested for their effectiveness against Listeria monocytogenes, Escherichia coli O157:H7, and Salmonella Typhimurium. Hydrogen peroxide (1.5 and 3%), vinegar (2.5 and 5% acetic acid), baking soda (11, 33, and 50% sodium bicarbonate), household bleach (0.0314, 0.0933, and 0.670% sodium hypochlorite), 5% acetic acid (prepared from glacial acetic acid), and 5% citric acid solutions were tested against the three pathogens individually (five-strain composites of each, 10(8) CFU/ml) by using a modified AOAC International suspension test at initial temperatures of 25 and 55degrees C for 1 and 10 min. All bleach solutions (pH 8.36 to 10.14) produced a >5-log reduction of all pathogens tested after 1 min at 25 degrees C, whereas all baking soda solutions (pH 7.32 to 7.55) were ineffective (5-log reduction of both Salmonella Typhimurium and E. coli O157:H7, whereas undiluted vinegar (pH 2.58) had a similar effect only against Salmonella Typhimurium. Compared with 1 min at 25 degrees C, greater reductions of L. monocytogenes (P 3% hydrogen peroxide > undiluted vinegar and 5% acetic acid > 5% citric acid > baking soda (50% sodium bicarbonate). The sensitivity of the tested pathogens to all tested household compounds followed the sequence of Salmonella Typhimurium > E. coli O157: H7 > L. monocytogenes.

  12. Targeting B7x and B7-H3 as New Immunotherapies for Prostate Cancer

    Science.gov (United States)

    2016-09-01

    activated and express receptors for B7x and B7-H3 and human prostate cancer cells express B7x or B7-H3. FACS showed the approach how we identified human...Immunomodu- latory pathways include members of the TNF receptor family and their ligands which have been studied as targets for cancer immunotherapy. These...urothelial bladder cancer patients resulting in an FDA breakthrough designation [50], and MSB0010718C which exhibits antitumor activ- ity by blocking PD-L1

  13. 3H-1,2-Benzodithiole-3-thione

    Directory of Open Access Journals (Sweden)

    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.

  14. 7-epi-griffonilide, a new lactone from Bauhinia pentandra: complete 1H and 13C chemical shift assignments.

    Science.gov (United States)

    Almeida, Macia C S DE; Souza, Luciana G S; Ferreira, Daniele A; Pinto, Francisco C L; Oliveira, Débora R DE; Santiago, Gilvandete M P; Monte, Francisco J Q; Braz-Filho, Raimundo; Lemos, Telma L G DE

    2017-01-01

    A new lactone, 7-epi-griffonilide (1), and six known compounds, 2, 3a - 3c, 4a and 4b, were isolated from the leaves of Bauhinia pentandra (Fabaceae). The structures elucidation of 1 and 2 were based on detailed 2D NMR techniques and spectral comparison with related compounds, leading to complete assignment of the 1H and 13C NMR spectra.

  15. 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

    Directory of Open Access Journals (Sweden)

    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.

  16. 2-Oxo-2H-chromen-7-yl 4-tert-butylbenzoate

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    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.

  17. rac-Dimethyl 2-(tert-butylamino-5-oxo-4,5-dihydropyrano[3,2-c]chromene-3,4-dicarboxylate

    Directory of Open Access Journals (Sweden)

    S. Antony Inglebert

    2011-11-01

    Full Text Available The title compound, C20H21NO7, is asymmetric with a chiral centre located in the pyran ring and crystallizes as a racemate. The molecular framework is somewhat bent; the coumarin moiety and the pyran ring are inclined by 7.85 (5°. The molecular structure is characterized by an intramolecular N—H...O hydrogen bond, which generates an S(6 ring motif, and the crystal packing is stabilized by intermolecular C—H...O hydrogen bonds. The 3-carboxylate O atom is involved in both of them, having a bifurcated character.

  18. 1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one

    Directory of Open Access Journals (Sweden)

    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.

  19. (2,7-Dimethoxynaphthalen-1-yl(phenylmethanone

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    Noriyuki Yonezawa

    2010-10-01

    Full Text Available The asymmetric unit of the title compound, C19H16O3, contains three independent conformers. Each of the three conformers has essentially the same feature of non-coplanar aromatic rings whereby the aroyl group at the 1-position of the naphthalene ring is twisted in a perpendicular manner to the naphthalene ring. The dihedral angles between the benzene ring planes and the naphthalene ring systems are 75.34 (7, 86.47 (7 and 76.55 (6° in the three conformers. The crystal structure is stabilized by intermolecular C—H...O hydrogen bonds.

  20. 1-[(2E-3-Phenylprop-2-en-1-yl]-1H-indole-2,3-dione

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    Fatima Zahrae Qachchachi

    2016-04-01

    Full Text Available In the title compound, C17H13NO2, the indole ring is essentially planar (r.m.s. deviation = 0.027 Å and is oriented at an angle of 69.33 (7° with respect to the phenyl ring. In the crystal, C—H...O hydrogen bonds link the molecules, forming zigzag chains propagating along the a-axis direction. Within the chains there are π–π stacking interactions [centroid–centroid distances = 3.7163 (8 and 3.7162 (8 Å] involving isatin groups of neighbouring molecules.

  1. Molecular and crystal structure of nido-9-C5H5N-11-I-7,8-C2B9H10: supramolecular architecture via hydrogen bonding X-H...I (X = B, C)

    International Nuclear Information System (INIS)

    Polyanskaya, T.M.

    2006-01-01

    A monocrystal X-ray diffraction study of a new iodine-containing cluster compound 9-(pyridine)-11-iodo-decahydro-7,8-dicarba-nido-undecaborane [9-C 5 H 5 N-11-I-7,8-C 2 B 9 H 10 ] has been performed. Crystal data: C 7 H 15 B 9 NI, M = 337.39, monoclinic, space group P2 1 /c, unit cell parameters: a=9.348(1) A, b=11.159(1) A, c=13.442(2) A, β=98.13(1) deg, V=1388.1(5) A 3 , Z=4, d calc = 1.614 g/cm 3 , T = 295 K, F(000)=648, μ=2.276 mm -1 . The structure was solved by a direct method and refined in the full-matrix anisotropic approximation (isotropic for hydrogen atoms) to final agreement factors R 1 = 0.0254, wR 2 = 0.0454 for 2437 I hkl >2σ I from 3590 measured I hkl (an Enraf-Nonius CAD-4 diffractometer, λMoK α , graphite monochromator, θ/2θ-scanning). The molecules are joined into a supramolecular assembly by hydrogen bonds X-H...I (X = B, C) [ru

  2. Forced volume magnetostriction in Mn3.3Sn0.7C compound at room temperature

    International Nuclear Information System (INIS)

    Wen Yongchun; Wang Cong; Sun Ying; Nie Man; Chu Lihua

    2010-01-01

    The negative volume magnetostriction in the external magnetic field for antiperovskite Mn 3.3 Sn 0.7 C compound is discovered. Its magnetic transition temperature from paramagnetism to ferrimagnetism is 348 K. The linear and volume magnetostrictions were investigated by measuring the change in length along the three-dimensional directions of the square samples at room temperature. Volume contraction was observed along all of the three directions throughout the whole magnetization. The value of volume magnetostriction is -44x10 -6 at 1.5 T. The magnetization saturates basically at 1.5 T, however the volume magnetostriction should be higher with further increase in magnetic field.

  3. Scaling of light emission from detonating bare Composition B, 2,4,6-trinitrotoluene [C7H5(NO2)3], and PE4 plastic explosive charges

    CSIR Research Space (South Africa)

    Mostert, FJ

    2011-10-01

    Full Text Available and configuration. In this study, the emission characteristics at wavelengths between 650 and 940 nm were experimentally investigated for cylindrical bare Composition B, 2,4,6-trinitrotoluene [C7H5(NO2)3], and PE4 plastic explosive charges in the mass (M) range of 0...

  4. (S,Z-3-Phenyl-2-[(1,1,1-trichloro-7-methoxy-2,7-dioxohept-3-en-4-ylamino]propanoic acid monohydrate

    Directory of Open Access Journals (Sweden)

    Alex Fabiani Claro Flores

    2014-02-01

    Full Text Available In the title compound, C17H18Cl3NOH2O, intramolecular N—H...O and C—H...Cl hydrogen bonds form S(6 and S(5 ring motifs, respectively. The chiral organic molecule is connected to the solvent water molecule by a short O—H...O hydrogen bond. In the crystal, a weak C—H...Cl interaction connects the organic molecules along [100] while the water molecules act as bridges between the organic molecules in both the [100] and [010] directions, generating layers parallel to the ab plane.

  5. Crystal structure of 2-amino-4-(4-chlorophenyl-1-(4-methylphenyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carbonitrile

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    Shaaban K. Mohamed

    2015-12-01

    Full Text Available In the title compound, C23H20ClN3O, each of the cyclohexene and 1,4-dihydropyridine rings of the 1,4,5,6,7,8-hexahydroquinoline ring system adopts a twisted-boat conformation. The dihedral angle between the two benzene rings is 11.52 (7°. In the crystal, molecules are linked through a pair of amino–nitrile N—H...N hydrogen bonds, forming inversion dimers. These assemble into a three-dimensional network via C—H...O and C—H...π interactions.

  6. Di-n-butyl 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

    2011-09-01

    Full Text Available The complete molecule of the title compound, C31H42N2O6, is generated by crystallographic twofold symmetry, with one C atom lying on the axis. The dihedral angle between the aromatic rings is 57.03 (6°. The central heterocyclic ring adopts a half-chair conformation. The molecular conformation is stabilized by two intramolecular O—H...N hydrogen bonds with the N atoms of the heterocyclic ring as the acceptors. In the crystal, molecules are linked into chains along the c axis by non-classical C—H...O hydrogen bonds.

  7. Sandwich iridium complexes with the monoanionic carborane ligand [9-SMe2-7,8-C2B9H10]-

    International Nuclear Information System (INIS)

    Loginov, D.A.; Vinogradov, M.M.; Perekalin, D.S.; Starikova, Z.A.; Lysenko, K.A.; Petrovskij, P.V.; Kudinov, A.R.

    2006-01-01

    The reaction of the [(η-9-SMe 2 -7,8-C 2 B 9 H 10 )IrBr 2 ] 2 complex with Tl[Tl(η-7,8-C 2 B 9 H 11 )] afforded the iridacarborane compound (η-9-SMe 2 -7,8-C 2 B 9 H 10 )Ir(η-7,8-C 2 B 9 H 11 ). The cationic complex [Cp*Ir(η-9-SMe 2 -7,8-C 2 B 9 H 10 )] + PF 6 - (Cp* is pentamethylcyclopentadienyl) was synthesized by the reaction of [Cp*IrCl 2 ] 2 with Na[9-SMe 2 -7,8-C 2 B 9 H 10 ]. The structures of (η-9-SMe 2 -7,8-C 2 B 9 H 10 )Ir(η-cod) (cod is 1,5-cyclooctadiene) and [Cp*Ir(η-9-SMe 2 -7,8-C 2 B 9 H 10 ]PF 6 were established by X-ray diffraction [ru

  8. (E-N-[2-(9-Fluorenylidene-3a,5,7-trimethyl-3,3a-dihydro-2H-indol-3-ylidene]-2,4,6-trimethylaniline

    Directory of Open Access Journals (Sweden)

    Norihiro Tokitoh

    2008-02-01

    Full Text Available The title compound, C33H30N2, has an E configuration at the imine double bond. The angle between the least-squares planes of the imine C=N—C group and the benzene ring of the 2,4,6-trimethylphenyl substituent is 85.38 (11°. The crystal structure is sustained mainly by intermolecular π–π interactions (3.510 Å between the two fluorene rings and some C—H...π interactions.

  9. Crystal structure of hexaaquanickel(II bis{2-[(5,6-dihydroxy-3-sulfonatoquinolin-1-ium-7-yloxy]acetate} dihydrate

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    Hai Le Thi Hong

    2015-09-01

    Full Text Available The asymmetric unit of the title compound, [Ni(H2O6](C11H8NO8S2·2H2O, features a half-hexaaquanickel(II complex cation with the NiII ion on an inversion center, one deprotonated 5,6-dihydroxy-3-sulfoquinolin-7-yloxyacetic acid (QOH molecule appearing in its zwitterionic form and one lattice water molecule. The sulfonate group is disordered over two positions with occupancy factors of 0.655 (5 and 0.345 (5. The hexaaquanickel(II cation interacts through hydrogen bonding with eight QOH molecules and two water molecules. The six-membered rings of quinoline show π–π stacking [centroid-to-centroid distances of 3.679 (2 Å and 3.714 (2 Å].

  10. {2-[(3,5-Dichloro-2-oxidobenzylideneamino-κ2N,O]-3-methylpentanoato-κO}(N,N′-dimethylformamide-κOcopper(II

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    Xiao Zhen Feng

    2008-05-01

    Full Text Available In the title compound, [Cu(C13H13Cl2NO3(C3H7NO], the CuII atom is coordinated in a slightly distorted square-planar geometry by two O atoms and one N atom from the tridentate chiral ligand 2-[(3,5-dichloro-2-oxidobenzylideneamino]-3-methylpentanoate and by one O atom from dimethylformamide. In the crystal structure, the Cu atom forms contacts with Cl and O atoms of two units (Cu...Cl and Cu...O = 3.401 and 2.947 Å, respectively, thereby forming an approximately octahedral arrangement. A three-dimensional network is constructed through Cl...Cu, O...Cu, Cl...Cl contacts and C—H...O hydrogen bonds.

  11. Syntheses and Thermal Behaviors of Rb(FOX-7H2O and Cs(FOX-7H2O

    International Nuclear Information System (INIS)

    Luo, Jinan; Xu, Kangzhen; Wang, Min; Ren, Xiaolei; Chen, Yongshun; Song, Jirong; Zhao, Fengqi

    2010-01-01

    Two new energetic organic alkali metal salts, 1,1-diamino-2,2-dinitroethylene rubidium salt [Rb(FOX-7H 2 O] and 1,1- diamino-2,2-dinitroethylene cesium salt [Cs(FOX-7H 2 O], were synthesized by reacting of 1,1-diamino-2,2-dinitroethylene (FOX-7) and rubidium chloride or cesium chloride in alkali methanol aqueous solution, respectively. The thermal behaviors of Rb(FOX-7H 2 O and Cs(FOX-7H 2 O were studied with DSC and TG methods. The critical temperatures of thermal explosion of the two compounds are 216.22 and 223.73 .deg. C, respectively. Specific heat capacities of the two compounds were determined with a micro-DSC method, and the molar heat capacities are 217.46 and 199.47 J mol -1 K -1 at 298.15 K, respectively. The adiabatic times-to-explosion were also calculated to be a certain value of 5.81 - 6.36 s for Rb(FOX-7H 2 O, and 9.92 - 10.54 s for Cs(FOX-7H 2 O. After FOX-7 becoming alkali metal salts, thermal decomposition temperatures of the compounds heighten with the rise of element period, but thermal decomposition processes become intense

  12. Crystal structure of (1S,3R,8R,9R-2,2-dichloro-3,7,7-trimethyl-10-methylenetricyclo[6.4.0.01,3]dodecan-9-ol

    Directory of Open Access Journals (Sweden)

    Ahmed Benzalim

    2016-08-01

    Full Text Available The title compound, C16H24Cl2O, was synthesized by treating (1S,3R,8S,9R,10S-2,2-dichloro-3,7,7,10-tetramethyl-9,10-epoxytricyclo[6.4.0.01,3]dodecane with a concentrated solution of hydrobromic acid. It is built up from three fused rings: a cycloheptane ring, a cyclohexyl ring bearing alkene and hydroxy substituents, and a cyclopropane ring bearing two chlorine atoms. The asymmetric unit contains two molecules linked by an O—H...O hydrogen bond. In the crystal, further O—H...O hydrogen bonds build up an R44(8 cyclic tetramer. One of the molecules presents disorder that affects the seven-membered ring. In both molecules, the six-membered rings display a chair conformation, whereas the seven-membered rings display conformations intermediate between boat and twist-boat for the non-disordered molecule and either a chair or boat and twist-boat for the disordered molecule owing to the disorder. The absolute configuration for both molecules is 1S,3R,8R,9R and was deduced from the chemical pathway and further confirmed by the X-ray structural analysis.

  13. Synthesis of new dithiacobaltaborane clusters derived from arachno-6,8-S2B7H9

    International Nuclear Information System (INIS)

    Kang, S.O.; Sneddon, L.G.

    1988-01-01

    A series of air-stable dithiacobaltaborane clusters has been isolated from either the reaction of the arachno-S 2 B 7 H 8 - anion with cobalt chloride and pentamethylcyclopentadienide or the reaction of neutral arachno-6,8-S 2 B 7 H 9 with cobalt atoms and pentamethylcyclopentadiene. Thus, the reaction of arachno-S 2 B 7 H 8 - with CoCl 2 and C 5 (CH 3 ) 5 - in THF gave, as the major products, the triple-decker compound nido-4,6-η-C 5 (CH 3 ) 52 Co 2 -3,5-S 2 B 2 H 2 (I) and the 11-vertex cluster nido-8,10(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (III). Also isolated in smaller amounts were a chloride derivative of I, nido-1-Cl-4,6-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -3,5-S 2 B 2 H (II), two isomers of III, nido-3,10-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (IV) and nido-3,5-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (V), and the eight-boron cluster nido-8-(η-C 5 (CH 3 ) 5 )Co-7,9-S 2 B 8 H 8 (VI). Other trace products of the reaction included the six-boron clusters nido-5,8-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -6,9-S 2 B 6 H 6 (VII) and arachno-7-(η-C 5 (CH 3 ) 5 )Co-6,8-S 2 B 6 H 8 (VIII). Compound III was found to isomerize at 250 degree C to IV, which could then be converted to V at 300 degree C. The reaction of cobalt atoms with arachno-6,8-S 2 B 7 H 9 in the presence of pentamethylcyclopentadiene gave VIII as the major product; however, a number of other clusters including I, V, VI, and [(η-C 5 (CH 3 ) 5 ) 2 Co] + [(SB 10 H 10 ) 2 Co] - were isolated in trace amounts. 16 references, 6 figures, 3 tables

  14. Study of the unimolecular decompositions of the (C3H6)+2 and (c-C3H6)+2 complexes

    International Nuclear Information System (INIS)

    Tzeng, W.; Ono, Y.; Linn, S.H.; Ng, C.Y.

    1985-01-01

    The major product channels identified in the unimolecular decompositions ofC 3 H + 6 xC 3 H 6 and c-C 3 H + 6 xc-C 3 H 6 in the total energy [neutral (C 3 H 6 ) 2 or (c-C 3 H 6 ) 2 heat of formation plus excitation energy] range of approx.230--450 kcal/mol are C 3 H + 7 +C 3 H 5 , C 4 H + 7 +C 2 H 5 , C 4 H + 8 +C 2 H 4 , and C 5 H + 9 +CH 3 . The measured appearance energy for C 4 H + 7 (9.54 +- 0.04 eV) from (C 3 H 6 ) 2 is equal to the thermochemical threshold for the formation of C 4 H + 7 +C 2 H 5 from (C 3 H 6 ) 2 , indicating that the exit potential energy barrier for the ion--molecule reaction C 3 H + 6 +C 3 H 6 →C 4 H + 7 +C 2 H 5 is negligible. There is evidence that the formations of C 4 H + 7 +C 2 H 4 +H from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 also proceed with high probabilities when they are energetically allowed. The variations of the relative abundances for C 4 H + 7 ,C 4 H + 8 , and C 5 H + 9 from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 as a function of ionizing photon energy are in qualitative agreement, suggesting that (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 rearrange to similar C 6 H + 12 isomers prior to fragmentation. The fact that C 6 H + 11 is found to be a primary ion from the unimolecular decomposition of (c-C 3 H 6 ) + 2 but not (C 3 H 6 ) + 2 supports the conclusion that the distribution of C 6 H + 12 collision complexes involved in the C 3 H + 6 +C 3 H 6 reactions is different from that in the cyclopropane ion--molecule reactions

  15. 2′-Methyl-2′-nitro-1′-phenyl-2′,3′,5′,6′,7′,7a'-hexahydrospiro[indoline-3,3′-1′H-pyrrolizin]-2-one

    Directory of Open Access Journals (Sweden)

    Yaghoub Sarrafi

    2008-08-01

    Full Text Available The title compound, C21H21N3O3, was synthesized by a multi-component 1,3-dipolar cycloaddition of azomethine ylide, derived from isatin and proline by a decarboxylative route, and (E-1-phenyl-2-nitropropene. In the molecule, the spiro junction links a planar oxindole ring and a pyrrolidine ring in an envelope conformation. The molecular packing is stabilized by an intermolecular N—H...N interaction of the oxindole and pyrrolizidine rings.

  16. Structural and thermal studies of H2La2/3Ta2O7, a protonated layered perovskite

    International Nuclear Information System (INIS)

    Le Berre, F.; Crosnier-Lopez, M.P.; Fourquet, J.L.

    2006-01-01

    We have synthesised the new protonated layered perovskite H 2 La 2/3 Ta 2 O 7 which is related to the Ruddlesden-Popper family. This compound is obtained by ionic exchange starting from Li 2 La 2/3 Ta 2 O 7 maintained in dilute HNO 3 at 60 deg. C. Thermal X-ray diffraction and DTA/TGA revealed interesting dehydration properties with formation of a layered anhydrous phase leading at higher temperature (1550 deg. C) to La 1/3 TaO 3 . This latter compound exhibits the original lanthanum ordering expected similarly to that of the Li form, while at 900 deg. C a metastable form, presenting a disordered La distribution, is observed

  17. 2,3-Diaminopyridinium 6-carboxypyridine-2-carboxylate

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    Mahsa Foroughian

    2011-12-01

    Full Text Available The asymmetric unit of the title proton-transfer compound, C5H8N3C7H4NO4−, consists of one mono-deprotonated pyridine-2,6-dicarboxylic acid as anion and one protonated 2,3-diaminopyridine as cation. The crystal packing shows extensive O—H...O, N—H...O and N—H...N hydrogen bonds. Thre are also several π–π interactions between the anions and also between the cations [centriod–centroid distances = 3.6634 (7, 3.7269 (7, 3.6705 (7 and 3.4164 (7 Å].

  18. 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.

  19. 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-ylmethyl]-6-hydroxy-1,3-dimethylpyrimidine-2,4(1H,3H-dione

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    Assem Barakat

    2016-09-01

    Full Text Available 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-yl-methyl]-6-hydroxy-1,3-di-methylpyrimidine-2,4(1H,3H-dione 3 was synthesized via a multicomponent reaction. The Aldol–Michael addition reactions of N,N-dimethylbarbituric acid, cyclohexane-1,3-dione, and 3-fluorobenzaldehyde in aqueous solution gave the product in high yield. The molecular structure of the compound was confirmed by spectroscopic methods and X-ray crystallography. The title compound (C19H19FN2O5·H2O crystallizes in the Monoclinic form, P21/c, a = 7.8630 (5 Å, b = 20.0308 (13 Å, c = 11.3987 (8 Å, β = 104.274 (3°, V = 1739.9 (2° Å3, Z = 4, Rint = 0.117, wR(F2 = 0.124, T = 100 K.

  20. 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.

  1. X-ray and NQR studies of bromoindate(III) complexes. [C2H5NH3]4InBr7, [C(NH2)3]3InBr6, and [H3NCH2C(CH3)2CH2NH3]InBr5

    International Nuclear Information System (INIS)

    Iwakiri, Takeharu; Ishihara, Hideta; Terao, Hiromitsu; Lork, Enno; Gesing, Thorsten M.

    2017-01-01

    The crystal structures of [C 2 H 5 NH 3 ] 4 InBr 7 (1), [C(NH 2 ) 3 ] 3 InBr 6 (2), and [H 3 NCH 2 C(CH 3 ) 2 CH 2 NH 3 ]InBr 5 (3) were determined at 100(2) K: monoclinic, P2 1 /n, a=1061.94(3), b=1186.40(4), c=2007.88(7) pm, β= 104.575(1) , Z=4 for 1; monoclinic, C2/c, a=3128.81(12), b=878.42(3), c=2816.50(10) pm, β=92.1320(10) , Z=16 for 2; orthorhombic, P2 1 2 1 2 1 , a=1250.33(5), b=1391.46(6), c=2503.22(9) pm, Z=4 for 3. The structure of 1 contains an isolated octahedral [InBr 6 ] 3- ion and a Br - ion. The structure of 2 contains three different isolated octahedral [InBr 6 ] 3- ions. The structure of 3 has a corner-shared double-octahedral [In 2 Br 11 ] 5- ion and an isolated tetrahedral [InBr 4 ] - ion. The 81 Br nuclear quadrupole resonance (NQR) lines of the terminal Br atoms of the compounds are widely spread in frequency, and some of them show unusual positive temperature dependence. These observations manifest the N-H..Br-In hydrogen bond networks developed between the cations and anions to stabilize the crystal structures. The 81 Br NQR and differential thermal analysis (DTA) measurements have revealed the occurrence of unique phase transitions in 1 and 3. When the bond angles were estimated from the electric field gradient (EFG) directions calculated by the molecular orbital (MO) methods, accurate values were obtained for [InBr 6 ] 3- of 1 and for [In 2 Br 11 ] 5- and [InBr 4 ] - of 3, except for several exceptions in those for the latter two ions. On the other hand, the calculations of 81 Br NQR frequencies have produced up to 1.4 times higher values than the observed ones.

  2. N-[7-Ethoxy-1-(prop-2-en-1-yl-1H-indazol-4-yl]-4-methylbenzenesulfonamide

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    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.

  3. Wet chemical passivation of YBa2Cu3O(7-x)

    Science.gov (United States)

    Vasquez, R. P.; Hunt, B. D.; Foote, M. C.

    1990-01-01

    Wet chemical techniques are described for treatment of YBa2Cu3O(7-x) surfaces, which result in the formation of native compounds known to have little or no reactivity to water. Suitable native compounds include CuI, BaSO4, CuS, Cu2S, YF3, and the oxalates. Formation of surface layers in which these nonreactive native compounds are major constituents is verified with X-ray photoelectron spectroscopy (XPS) measurements on YBa2Cu3O(7-x) films treated with dilute solutions of HI, H2SO4, Na2S, HF, or H2C2O4. No significant changes are observed in the XPS spectra when the sulfide, sulfate, or oxalate films are dipped in water, while the iodide and fluoride films show evidence of reaction with water. X-ray diffraction measurements show that the superconducting phase is absent in the sulfide film, but is unaffected by the oxalate and sulfate treatments.

  4. 2,5-Dimethyl-1-phenylsulfonyl-1H-pyrrole-3,4-dicarbaldehyde

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available In the title compound, C14H13NO4S, the mean planes of the pyrrole and phenyl rings form a dihedral angle of 88.7 (1°. The aldehyde groups are slightly twisted from the pyrrole plane. In the crystal structure, molecules are linked into a three-dimensional framework by C—H...O hydrogen bonds.

  5. Synthesis and structure of a 1,6-hexyldiamine heptaborate, [H3N(CH2)6NH3][B7O10(OH)3

    International Nuclear Information System (INIS)

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

    2007-01-01

    A new 1,6-hexyldiamine heptaborate, [H 3 N(CH 2 ) 6 NH 3 ][B 7 O 10 (OH) 3 ] (1), has been solvothermally synthesized and characterized by single-crystal X-ray diffraction, FTIR, elemental analysis, and thermogravimetric analysis. Compound 1 crystallizes in monoclinic system, space group P2 1 /n with a=8.042(2) A, b=20.004(4) A, c=10.103(2) A, and β=90.42(3) deg. The anionic [B 7 O 10 (OH) 3 ] n 2n- layers are interlinked via hydrogen bonding to form a 3D supramolecular network containing large channels, in which the templated [H 3 N(CH 2 ) 6 NH 3 ] 2+ cations are located. - Graphical abstract: A layered 1,6-hexyldiamine heptaborate, [H 3 N(CH 2 ) 6 NH 3 ][B 7 O 10 (OH) 3 ], was solvothermally synthesized at 150 deg. C. It is a layer borate and crystallized in monoclinic space group P2 1 /n with a=8.042(2) A, b=20.004(4) A, c=10.103(2) A, β=90.42(3) deg

  6. 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.

  7. 1,2,3,3-Tetramethyl-7-nitro-3,4-dihydroisoquinolinium tetrafluoroborate

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    Mouna Bouzid

    2016-04-01

    Full Text Available The title salt, C13H17N2O2+·BF4−, was prepared by the methylation of the imine with Meerwein salt in dichloromethane. The asymmetric unit comprises a 1,3,3-trimethyl-7-nitro-3,4-dihydroisoquinolinium cation and a tetrafluoroborate anion. The coordination around the boron atom in the tetrafluoroborate anion is tetrahedral. The heterocyclic ring adopts a half-chair conformation. The crystal packing is governed by means of C—H...F contacts, which lead to the formation of a three-dimensional network.

  8. Galvanomagnetic properties of atomically disordered compounds YBa2Cu3O7

    International Nuclear Information System (INIS)

    Kar'kin, A.E.; Goshchitskij, B.N.

    2001-01-01

    To clarify the peculiarities of the metal-dielectric transition (MDT) in the HTSC type compounds one investigated into the galvanomagnetic properties of YBa 2 Cu 3 O 7 polycrystalline specimens irradiated by fast neutrons under 80 K temperature with F = 2x10 19 cm -2 fluence and subsequent to their exposure to the isochronal annealings within 150-390 K temperature range. It was determined that temperature dependences of R H Hall coefficient and of MR magnetic resistances of YBa 2 Cu 3 O 7 polycrystalline compounds disordered by fast neutrons retained the anomalous properties peculiar to the HTSC type disordered compounds in spite of the fact that conductivity was not a metallic one. This behavior is explained by the fact that in the disordered compounds there are two co-existing electron phases with conductivity as to the localized and the metallic states. Concentration of metallic phase is lower than threshold of passing, that is why, conductivity of this system is of dielectric type while R H and MR have temperature dependences similar to metallic phase that are renormalized by magnitude [ru

  9. Crystal structure of 3,4a,7,7,10a-pentamethyl-3-vinyldodecahydro-1H-benzo[f]chromen-9-ol isolated from Sideritis perfoliata

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    Ísmail Çelik

    2016-10-01

    Full Text Available The asymmetric unit of the title compound, C20H34O2, contains two crystallographically independent molecules (1 and 2 with similar conformations. In both molecules, the cyclohexane rings adopt a chair conformation, while the oxane rings are also puckered. In the crystal, O—H...O hydrogen bonds connect adjacent molecules, forming C(6 helical chains located around a 21 screw axis and running along the crystallographic a axis. The packing of these chains is governed only by van der Waals interactions. Semi-empirical PM3 quantum chemical calculations are in a satisfactory agreement with the structural results of the X-ray structure analysis. The absolute structure was indeterminate in the present experiment.

  10. 4-(4,4-Difluoro-1,3,5,7-tetramethyl-3a-aza-4a-azonia-4-borata-s-indacen-8-ylbenzonitrile

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    Yuting Chen

    2011-04-01

    Full Text Available The title compound, C20H18BF2N3, contains one C9BN2 (Bodipy framework and one cyanobenzyl group. The Bodipy framework is essentially planar with a maximum deviation of 0.041 (2 Å. The introduction of two methyl groups at positions 1 and 7 of s-indacene in the Bodipy unit results in almost orthogonal configuration between the mean plane of the Bodipy unit and the cyanobenzyl group [dihedral angle = 89.78 (4°].

  11. Investigation into complexing in Re7-H3O+-SO42--H2O system

    International Nuclear Information System (INIS)

    Sinyakova, G.S.

    1979-01-01

    Using the methods of spectrophotometry and conductometry it is shown, that in the ReO 4 - -H 3 O + -SO 4 2- -H 2 O system interaction between rhenium (7) and sulfuric acid takes place in a wide concentration range. In low-acid solutions at pH 2.0-0.9 rhenium(7) complex with proton is formed at the ratio of 1:1 with lgK 1 =3.30+-0.02. In 1-10 mol. sulfuric acid observed is consecutive complexing at the rhenium(7) - sulfuric acid ratio in the complex of 1:1 and 1:2 respectively with lgK 2 =0.93+-0.13 and lgK 3 =0.34+-0.03. At the background of concentrated perchloric acid rhenium (7) and sodium sulfate form two complex compounds at rhenium (7) - sodium sulfate ratio of 1:1 and 1:2 with lgK 1 =1.86+-0.02 and lgK 2 =2.35+-0.03

  12. The orthorhombic fluorite related compounds Ln/sub 3/RuO/sub 7/, Ln=Nd, Sm and Eu

    International Nuclear Information System (INIS)

    Van Berkel, F.P.F.; Ijdo, D.J.W.

    1986-01-01

    Fluorite-related Ru(V) compound with composition Ln/sub 3/RuO/sub 7/ have been found. These compounds with space group Cmcm adopt a superstructure of the cubic fluorite structure with a/sub orth/=2a/sub c/, b/sub orth/=c/sub orth/=a/sub c/√2. These compounds have the same structure as La/sub 3/NbO/sub 7/

  13. 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.

  14. [Pr2(pdc3(Hpdc(H2O4]n·n(H3hp·8n(H2O, a One-Dimensional Coordination Polymer Containing PrO6N3 Tri-Capped Trigonal Prisms and PrO8N Mono-Capped Square Anti-Prisms (H2pdc = Pyridine 2,6-Dicarboxylic Acid, C7H5NO4; 3hp = 3-Hydroxy Pyridine, C5H5NO

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    Shahzad Sharif

    2012-08-01

    Full Text Available The synthesis, structure and some properties of the one-dimensional coordination polymer, [Pr2(pdc3(Hpdc]n·n(H3hp·8n(H2O, (H2pdc = pyridine 2,6-dicarboxylic acid, C7H5NO4; 3hp = 3-hydroxypyridine, C5H5NO are described. One of the Pr3+ ions is coordinated by two O,N,O-tridentate pdc2− ligands and one tridentate Hpdc− anion to generate a fairly regular PrO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The second Pr3+ ion is coordinated by one tridentate pdc2− dianion, four water molecules and two monodentate bridging pdc2− ligands to result in a PrO8N coordination polyhedron that approximates to a mono-capped square-anti-prism. The ligands bridge the metal-atom nodes into a chain, which extends in the [100] direction. The H3hp+ cation and uncoordinated water molecules occupy the inter-chain regions and an N–HLO and numerous O–HLO hydrogen bonds consolidate the structure. The H3hp+ species appears to intercalate between pendant pdc rings to consolidate the polymeric structure. Crystal data: 1 (C33H43N5O29Pr2, Mr = 1255.54, triclinic,  (No. 2, Z = 2, a = 13.2567(1 Å, b = 13.6304(2 Å, c = 13.6409(2 Å, α = 89.695(1°, β = 63.049(1°, γ = 86.105(1°, V = 2191.16(5 Å3, R(F = 0.033, wR(F2 = 0.084.

  15. Ethyl 1-cyclopropyl-6,7-difluoro-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylate

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    De-Cai Wang

    2008-11-01

    Full Text Available In the title compound, C16H15F2NO4, the dihedral angle between the three-membered ring and the quinoline ring system is 64.3 (3°. In the crystal structure, intermolecular C—H...O hydrogen bonds link the molecules, forming a column running along [101].

  16. 7-epi-griffonilide, a new lactone from Bauhinia pentandra: complete {sup 1}H and {sup 13}C chemical shift assignments

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Macia C.S. de; Souza, Luciana G.S.; Ferreira, Daniele A.; Pinto, Francisco C.L.; Santiago, Gilvandete M.P.; Monte, Francisco J.Q.; Lemos, Telma L.G., E-mail: fmonte@dqoi.ufc.br [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil); Oliveira, Debora R. de; Braz-Filho, Raimundo [Universidade Federal Rural do Rio de Janeiro (UFRRJ), Seropedica, RJ (Brazil). Departamento de Quimica

    2017-09-01

    A new lactone, 7-epi-griffonilide (1), and six known compounds, 2, 3a - 3c, 4a and 4b, were isolated from the leaves of Bauhinia pentandra (Fabaceae). The structures elucidation of 1 and 2 were based on detailed 2D NMR techniques and spectral comparison with related compounds, leading to complete assignment of the {sup 1}H and {sup 13}C NMR spectra. (author)

  17. 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.

  18. 4,4′-Dichloro-3,3′,5,5′-tetramethyl-2,2′-[(3aR,7aR/3aS,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diylbis(methylene]diphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2011-08-01

    Full Text Available In the title compound, C25H32Cl2N2O2, there are two intramolecular O—H... N hydrogen-bonding interactions between the hydroxy groups on the aromatic rings and the two N atoms of the heterocyclic group. The cyclohexane ring adopts a chair conformation and the imidazolidine unit to which it is fused has a twisted envelope conformation. The asymmetric unit comprises one half-molecule which is completed by a twofold rotation axis. A C—H...O interaction is observed in the crystal structure.

  19. Crystal structure of 1-methyl-4-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine

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    Mohammed El Fal

    2014-12-01

    Full Text Available In the title compound, C7H8N4S, the non-H atoms of the pyrazolo[3,4-d]pyrimidine ring system and the methylsulfanyl group lie on a crystallographic mirror plane. In the crystal, molecules are linked via a number of π–π interactions [centroid–centroid distances vary from 3.452 (7 to 3.6062 (8 Å], forming a three-dimensional structure.

  20. 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.

  1. Aspartic protease inhibitory and nematocidal activity of phenyl-4-(2-phenylhydrazonohexahydrofuro[3,2-c]pyridazin-7-ol (Percival dianhydroosazone

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    El Sayed H. El Ashry

    2014-04-01

    Full Text Available We synthesized Phenyl-4-(2-phenylhydrazonohexahydrofuro[3,2-c]pyridazin-7-ol (compound 3. The structure compound 3 was elucidated with IR, 1H NMR, 13C NMR and EIMS spectra. Compound 3 showed potent inhibitory activity against aspartic proteases, human cathepsin D and Plasmodium falciparum plasmepsin-II with IC50 = 20 μM. Enzyme-inhibitor complexes were predicted to stabilize by electrostatic and hydrophobic interactions between the side chains of amino acid residues at the active center and compound 3. Moreover, compound 3 displayed good nematocidal activity against all developmental stages of C. elegans.

  2. (6S,7S,8S,8aS-6-Ethyl-7,8-dihydroxy-1,5,6,7,8,8a-hexahydroindolizin-3(2H-one monohydrate

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    Jozefína Žúžiová

    2010-12-01

    Full Text Available The absolute configuration of the title compound, C10H17NO3·H2O, was assigned from the synthesis. In the molecular structure, the central six-membered ring of the indolizine moiety adopts a chair conformation, with two atoms displaced by −0.578 (2 and 0.651 (1 Å from the plane of the other four atoms [maximum deviation 0.019 (2 Å] The conformation of the fused oxopyrrolidine ring is close to that of a flat envelope, with the flap atom displaced by 0.294 (1 Å from the plane through the remaining four atoms. In the crystal, one of the hydroxy groups is hydrogen-bonded to two water molecules, while the other hydroxy group exhibits an intermolecular hydrogen bond to the carbonyl O atom, resulting in a chain parallel to the b axis.

  3. Crystal structure of 2-oxo-2H-chromen-7-yl 4-fluorobenzoate

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    Akoun Abou

    2018-05-01

    Full Text Available In the title compound, C16H9FO4, (I, the benzene ring is oriented at an acute angle of 59.03 (15° relative to the coumarin plane (r.m.s deviation = 0.009 Å. This conformation of (I is stabilized by an intramolecular C—H...O hydrogen bond, which closes a five-membering ring. In the crystal, molecules of (I form infinite zigzag chains along the b-axis direction, linked by C—H...O hydrogen bonds. Furthermore, the crystal structure is supported by π–π stacking interactions between neighbouring pyrone and benzene or coumarin rings [centroid–centroid distances in the range 3.5758 (18–3.6115 (16 Å], as well as C=O...π interactions [O...centroid distances in the range 3.266 (33.567 (3 Å]. The theoretical data for (I obtained from quantum chemical calculations are in good agreement with the observed structure, although the calculated C—O—C—C torsion angle between the coumarin fragment and the benzene ring (73.7° is somewhat larger than the experimental value [63.4 (4°]. Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions.

  4. 2-Methyl-3-(2-methylphenyl-7-nitroquinazolin-4(3H-one

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    Edward R. T. Tiekink

    2012-03-01

    Full Text Available In the title methaqualone analogue, C16H13N3O3, the 2-tolyl group is almost orthogonal [dihedral angle = 85.20 (5°] to the fused ring system (r.m.s. deviation of fitted non-H atoms = 0.029 Å. In the crystal, twofold symmetry generates two-molecule aggregates linked by C—H...O and π–π interactions [ring centroid–centroid distance = 3.4967 (6 Å].

  5. 2-(4-Methoxy-1H-indol-3-ylacetonitrile

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    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. 3-Cyanoanilinium nitrate

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    Bo Wang

    2009-10-01

    Full Text Available In the cation of the title compound, C7H7N2+·NO3−, the nitrile group and the benzene ring are almost coplanar (r.m.s. deviation = 0.006 Å. In the crystal, the ions are connected by bifurcated N—H...(O,O hydrogen bonds, forming a two-dimensional network parallel to (001.

  7. Crystal structure of 1-ethylpyrazolo[3,4-d]pyrimidine-4(5H-thione

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    Mohammed El Fal

    2014-09-01

    Full Text Available In the title compound, C7H8N4S, the methyl C atom is displaced by 1.232 (7 Å from the mean plane of the pyrazolo[3,4-d]pyrimidine ring system (r.m.s. deviation = 0.007 Å. The N—N—C—Cm (m = methyl torsion angle is −60.3 (6°. In the crystal, molecules are linked by N—H...S hydrogen bonds, generating [010] chains, which are reinforced by C—H...N interactions. The chains are cross-linked by weak C—H...S hydrogen bonds, generating (001 sheets.

  8. Systems Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O at 25 deg C. Sistemy Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O pri 25 grad S

    Energy Technology Data Exchange (ETDEWEB)

    Skvortsov, V G; Sadetdinov, Sh V; Akimov, V M; Mitrasov, Yu N; Petrova, O V; Klopov, Yu N [Chuvashskij Gosudarstvennyj Pedagogicheskij Inst., Cheboksary (Russian Federation) Universitet Druzhby Narodov, Moscow (Russian Federation)

    1994-02-01

    Phase equilibriums in the Li[sub 2]B[sub 4]O[sub 7] (Na[sub 2]B[sub 4]O[sub 7], K[sub 2]B[sub 4]O[sub 7])-N[sub 2]H[sub 3]H[sub 4]OH-H[sub 2]O systems were investigated by methods of isothermal solubility, refractometry and PH-metry at 25 deg C for the first time. Lithium and sodium tetraborates was established to form phases of changed composition mM[sub 2]B[sub 4]O[sub 7][center dot]nN[sub 2]H[sub 3]C[sub 2]H[sub 4]OH[center dot]XH[sub 2]O, where M=Li, Na with hydrazine ethanol. K[sub 2]B[sub 4]O[sub 7][center dot]4H[sub 2]O precipitates in solid phase in the case of potassium salt. Formation of isomorphous mixtures was supported by X-ray diffraction and IR spectroscopy methods.

  9. New homo- and heteroleptic derivatives of trivalent ytterbium containing anion-radical 1,4-diazadiene ligands. Synthesis, properties and crystal structure of (C9H7)2Yb[2-MeC6H4NC(Me)C(Me)NC6H4Me-2] and [PhNC(Ph)C(Ph)NPh]3Yb complexes

    International Nuclear Information System (INIS)

    Gudilenkov, I.D.; Fukin, G.K.; Cherkasov, A.V.; Shavyrin, A.S.; Trifonov, A.A.; Larionova, Yu.E.

    2008-01-01

    Reaction of ytterbium bisindenyl complex (C 9 H 7 ) 2 Yb II (THF) 2 (1) with 1,4-diazabutadiene 2-MeC 6 H 4 N=C(Me)-C(Me)=NC 6 H 4 Me-2 ( Me DAD) is accompanied by the oxidation of metal atom until trivalent state and results in the formation of paramagnetic compound of metallocenes type (C 9 H 7 ) 2 Yb III ( Me DAD -. ) (3) containing 1,4-diazabutadiene anion-radical. Structure of complex 3 is ascertained by the X-ray structure analysis. Reactions of bisindenyl (1) and bisfluorenyl (C 13 H 9 ) 2 Yb II (THF) 2 (2) derivatives of bivalent ytterbium with 1,4-diazabutadiene PhN=C(Ph)-C(Ph)=NPh ( Ph DAD) (at 1:2 molar ratio of reagents) proceed with the complete break of Yb-C bonds, oxidation of ytterbium atom until trivalent state, and result in the formation of homoligand complex ( Ph DAD -. ) 3 Yb (6) containing three anion-radical 1,4-diazadiene ligands. Complex 6 was also prepared by the exchange reaction of YbCl 3 with Ph DAD -. K + (1:3) in THF. Complex 6 is characterized by the X-ray structure analysis [ru

  10. Region 7 Title V facilities

    Data.gov (United States)

    U.S. Environmental Protection Agency — This web map shows the Region 7 Title V facilities (Clean Air Act major sources), any Class I areas within 300 km of R7 States, and any Tribal areas within 50 miles...

  11. (2S,7S-10-Ethyl-1,8,10,12-tetraazatetracyclo[8.3.1.18,12.02,7]pentadecan-10-ium iodide

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2012-10-01

    Full Text Available The title chiral quaternary ammonium salt, C13H25N4+·I−, was synthesized through the Menschutkin reaction between the cage aminal (2S,7S-1,8,10,12-tetraazatetracyclo[8.3.1.18,12.02,7]pentadecane and ethyl iodide. The quaternization occurred regioselectively on the nitrogen with major sp3 character. The crystal structure consists of anions and cations separated by normal distances. Ions are not linked through C—H...I hydrogen bonds.

  12. Crystal structure of (1R,3S,8R,11R-11-acetyl-3,7,7-trimethyl-10-oxatricyclo[6.4.0.01,3]dodecan-9-one

    Directory of Open Access Journals (Sweden)

    Abdoullah Bismoussa

    2015-12-01

    Full Text Available The title compound, C16H24O3, is built up from three fused rings, a six-membered, a seven-membered and a three-membered ring. The absolute configuration of the title compound was determined as (1R,3S,8R,11R based on the synthetic pathway. The six-membered ring has an half-chair conformation whereas the seven-membered ring displays a boat conformation. In the cyrstal, C—H...O hydrogen bonds build up a two-dimensional network parallel to (0 0 1. The crystal studied was an inversion twin with a minor twin component of 34%.

  13. Interaction between exo-nido-ruthenacarborane [Cl(Ph3P)2Ru]-5,6,10-(μ-H)3-10-H-7,8-C2B9H8 and bromine

    International Nuclear Information System (INIS)

    Timofeev, S.V.; Lobanova, I.A.; Petrovskij, P.V.; Starikova, Z.A.; Bregadze, V.I.

    2001-01-01

    Interaction between exo-nido-ruthenacarborane [Cl(Ph 3 P) 2 Ru]-5,6,10-(μ-H) 3 -10-H-7,8-C 2 B 9 H 8 with bromine in CH 2 Cl 2 solutions at 0 deg C studied using the methods of elementary analysis, NMR, IR spectroscopy and X-ray diffraction analysis. It was ascertained that the reaction gives rise to bromine atom substitution for chlorine atom in octahedral surrounding of ruthenium atom with formation of complex [Br(Ph 3 P) 2 Ru]-5,6,10-(μ-H) 3 -10-H-7,8-C 2 B 9 H 8 . The complex is crystallized in monoclinic crystal system with the following unit cell parameters a = 12.592 (1), b = 20.687 (2), c = 16.628 (2) A, β = 94.372 (3) deg, sp. gr. P2 1 /n, Z = 4. Coordination octahedron of ruthenium atom is formed by three hydrogen atoms bound with boron atoms in one triangular face of carborane, two phosphorus atoms and one bromine atom [ru

  14. A Green Method for Synthesis of 7H-thiazolo[3,2-b][1,2, 4]-triazin-7-one Derivatives as AChE Inhibitors

    Directory of Open Access Journals (Sweden)

    Liu Sijie

    2015-01-01

    Full Text Available The authors study an efficient and green approach for the synthesis of 7H-thiazolo [3, 2-b][1,2,4]triazin-7-one derivatives as AChE inhibitors. The 7H-thiazolo[3,2-b][1,2,4]triazin-7-ones were designed by molecular docking, and readily prepared via a one-pot reaction in morpholine hydrosulfate ([Hnhm]HSO4 lonic liquid as the catalyst and solvent. The study of AChE inhibitory activity was carried out through using the Ellman colorimetric assay. The 7H-thiazolo[3,2-b][1,2,4]triazin-7-ones had been successfully synthesized by green catalyst. Most of the target compounds exhibited more than 50% inhibition at 10μM.

  15. 4-Phenethylthio-2-phenylpyrazolo[1,5-a][1,3,5]triazin-7(6H-one

    Directory of Open Access Journals (Sweden)

    Sergey A. Smolnikov

    2017-12-01

    Full Text Available Exploring the pharmacologically important pyrazolo[1,5-a][1,3,5]triazin-7(6H-one scaffold for the construction of new bioactive compounds, we developed a synthesis of 4-phenethylthio-2-phenylpyrazolo[1,5-a][1,3,5]triazin-7(6H-one (4 via S-alkylation of 2-phenyl-4-thioxopyrazolo[1,5-a][1,3,5]triazine-7(6H-one (3, prepared by the double ring closure of pyrazole and triazine rings upon the treatment of 1-cyanoacetyl-4-benzoylthiosemicarbazide (2 with alkali. The antiproliferative activity of 4 against human lung cancer (A549 and human breast cancer (MDA-MB231 cell lines was investigated. Compound 4 was found to be more active against lung cancer cells than breast cancer cells.

  16. 4′,5-Dihydroxy-7-methoxyflavanone dihydrate

    Directory of Open Access Journals (Sweden)

    Iván Brito

    2012-01-01

    Full Text Available The title compound, C16H14O5·2H2O [systematic name: 5-hydroxy-2-(4-hydroxyphenyl-7-methoxychroman-4-one dihydrate], is a natural phytoalexin flavone isolated from the native chilean species Heliotropium taltalense and crystallizes with an organic molecule and two water molecules in the asymmetric unit. The 5-hydroxy group forms a strong intramolecular hydrogen bond with the carbonyl group, resulting in a six-membered ring. In the crystal, the components are linked by O—H...O hydrogen bonds, forming a three-dimensional network. The 4-hydroxyphenyl benzene ring is bonded equatorially to the pyrone ring, which adopts a slightly distorted sofa conformation. The title compound is the hydrated form of a previously reported structure [Shoja (1990. Acta Cryst. C46, 1969–1971]. There are only slight variations in the molecular geometry between the two compounds.

  17. N-Cyano-7α-methoxycarbonyl-6,14-endo-ethenotetrahydronorthebaine

    Directory of Open Access Journals (Sweden)

    Mustafa Odabaşoğlu

    2009-09-01

    Full Text Available In the title compound (systematic name: methyl 17-cyano-3,6-dimethoxy-4,5α-epoxy-6,14-endo-ethenomorphinan-7-carboxylate, C23H24N2O5, the dihydrofuran ring adopts a twist conformation, while the piperidine ring is in a chair conformation. The benzene-fused cyclohexene ring adopts an envelope conformation. An intramolecular C—H...O hydrogen bond is observed. Intermolecular C—H...N and C—H...O hydrogen bonds form C(5 chains along the a and b axes, respectively, and together they form a three-dimensional network.

  18. 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

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

    Directory of Open Access Journals (Sweden)

    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. Synthesis and structural characterization of Li{sub 3}K{sub 3}Eu{sub 7}(BO{sub 3}){sub 9}

    Energy Technology Data Exchange (ETDEWEB)

    Braeuchle, Sebastian; Huppertz, Hubert [Innsbruck Univ. (Austria). Inst. fuer Allgemeine, Anorganische und Theoretische Chemie; Seibald, Markus [OSRAM GmbH, Schwabmuenchen (Germany). Corporate Innovation

    2017-07-01

    Li{sub 3}K{sub 3}Eu{sub 7}(BO{sub 3}){sub 9} was prepared by high-temperature solid state synthesis at 900 C in a platinum crucible from lithium carbonate, potassium carbonate, boric acid, and europium(III) oxide. The title compound crystallizes in the orthorhombic space group Pca2{sub 1} (no. 29) (Z = 4). The structure was refined from single-crystal X-ray diffraction data: a = 21.126(2), b = 6.502(2), c = 17.619(2) Aa, V = 2420.1(2) Aa{sup 3}, R1 = 0.0183 and wR2 = 0.0412 for all data. The crystal structure of Li{sub 3}K{sub 3}Eu{sub 7}(BO{sub 3}){sub 9} is isotypic to Li{sub 3}K{sub 3}Y{sub 7}(BO{sub 3}){sub 9} featuring isolated BO{sub 3} units and LiO{sub 6} octahedra forming [Li{sub 3}B{sub 4}O{sub 21}] units in the ac plane, which are linked by additional BO{sub 3} units. The K{sup +} and Eu{sup 3+} cations are arranged in the cavities of the structure.

  1. (7aR-1-[(2R,5S,E-6-Hydroxy-5,6-dimethylhept-3-en-2-yl]-7a-methylhexahydro-1H-inden-4(2H-one

    Directory of Open Access Journals (Sweden)

    Marcos L. Rivadulla

    2013-02-01

    Full Text Available The chiral title compound, C19H32O2, contains a [4.3.0]-bicyclic moiety in which the shared C—C bond presents a trans configuration and a side chain in which the C=C double bond shows an E conformation. The conformations of five- and six-membered rings are envelope (with the bridgehead atom bearing the methyl substituent as the flap and chair, respectively, with a dihedral angle of 4.08 (17° between the idealized planes of the rings. In the crystal, the molecules are self-assembled via classical O—H...O hydrogen bonds, forming chains along [112]; these chains are linked by weak non-classical C—H...O hydrogen bonds, giving a two-dimensional supramolecular structure parallel to (010. The absolute configuration was established according to the configuration of the starting material.

  2. 7-Fluoro-4-oxochromene-3-carbaldehyde

    Directory of Open Access Journals (Sweden)

    Mohammad Asad

    2011-04-01

    Full Text Available In the title compound, C10H5FO3, the chromenone ring is essentially planar, with a maximum deviation of 0.039 (1 Å. The dihedral angle between the fluoro-subsituted benzene ring and the pyran ring is 1.92 (4°. In the crystal, molecules are connected via weak intermolecular C—H...O hydrogen bonds, forming supramolecular ribbons along the b axis. These ribbons are stacked down the a axis.

  3. Synthesis 1-(5-oxohexyl)-3,7-dimethyl-xanthyne labelled with tritium into 8 position from purinic ring

    International Nuclear Information System (INIS)

    Mihaila, V.; Corol, D.

    1999-01-01

    This paper presents the work on synthesis of 1-(5-oxohexyl)-3,7-dimethyl-xanthyne labelled with tritium into 8 position from purinic ring. The obtaining of tritium labelled compound is realized by initial labelling of theobromine with tritium into 8 position and by coupling the purinic derivative to 1-Br-5-hexanone. Theobromine-8- 3 H was obtained by the bromination of theobromine with elementary bromine and after that the bromine was substituted with tritium i.e.: C 7 H 8 O 2 N 4 theobromine Br 2 /(-HBr) C 7 H 7 O 2 N 4 Br (8-Br-theobromine) ( 3 H 2 /cat)/(-KOH) C 7 H 7 3 HO 2 N 4 (theobromine-8- 3 H). Theobromine-8- 3 H was purified by thin layer chromatography with a solvent system i.e. n-BuOH:AcOH:H 2 O (4:1:1, v/v/v) and characterized radiochemically. It was then diluted by unlabelled theobromine to specific activity of 50 mCi/g. After dilution, theobromine-8- 3 H was coupled to 1-Br-5-hexanone i.e.: C 7 H 7 3 HO 2 N 4 (theobromine-8- 3 H) + Br-(CH 2 ) 4 -CO-CH 3 (1-Br-5-hexanone) (NaOH)/(CH 3 OH) C 13 H 17 3 HO 3 N 4 (1-(5-oxohexyl)- 3,7-dimethyl-xanthine-8- 3 H). The raw compound was purified by recrystallization from 2-propanol and it was characterized radiochemically. (authors)

  4. Evaluation of live attenuated H7N3 and H7N7 vaccine viruses for their receptor binding preferences, immunogenicity in ferrets and cross reactivity to the novel H7N9 virus.

    Directory of Open Access Journals (Sweden)

    Qi Xu

    Full Text Available Live attenuated influenza vaccine (LAIV candidates of the H7 subtype, A/Netherlands/219/03 (H7N7, NL03 ca and A/chicken/British Columbia/CN-6/2004 (H7N3, BC04 ca, were evaluated for their receptor binding specificity and immunogenicity in ferrets. The BC04 ca virus exhibited α2,3-SA and α2,6-SA dual receptor binding preference while the NL03 ca virus preferentially bound to α2,3-SA. Substitution of the Q226 and G228 (Q-G by the L226 and S228 (L-S residues in the HA improved binding to α2,6-SA for NL03 ca. The vaccine viruses with L-S retained the attenuation phenotype. NL03 L-S ca replicated more efficiently than the original NL03 ca virus in the upper respiratory tract of ferrets, and induced higher levels of humoral and cellular immune responses. Prior vaccination with seasonal LAIV reduced H7-specific antibody responses, but did not reduce the H7N7 vaccine mediated protection against a heterologous H7N3 BC04 wt virus infection in ferrets. In addition, the H7N3 and H7N7 vaccine immunized ferret sera cross reacted with the newly emerged H7N9 virus. These data, in combination with the safety data from previously conducted Phase 1 studies, suggest that these vaccines may have a role in responding to the threat posed by the H7N9 virus.

  5. New route for the metallation of trihydroheptaphosphine P7H3 with butyllithium

    International Nuclear Information System (INIS)

    Milyukov, V.A.; Kataev, A.V.; Sinyashin, O.G.; Khej-Khokkins, E.

    2006-01-01

    A new route for the metallation of heptaphosphine P 7 H 3 with BuLi, namely, decomposition of the nortricyclane P 7 unit to form dilithium hexadecaphosphide Li 2 P 16 , was found. The composition and structure of the resulting compound were verified by mass spectrometry and 31 P NMR [ru

  6. 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.

  7. 2,6-Diaminopyridinium bis(4-hydroxypyridine-2,6-dicarboxylato-κ3O2,N,O6ferrate(III dihydrate

    Directory of Open Access Journals (Sweden)

    Andya Nemati

    2008-10-01

    Full Text Available The reaction of iron(II sulfate heptahydrate with the proton-transfer compound (pydaH(hypydcH (pyda = pyridine-2,6-diamine; hypydcH2 = 4-hydroxypyridine-2,6-dicarboxylic acid in an aqueous solution led to the formation of the title compound, (C5H8N3[Fe(C7H3NO52]·2H2O. The anion is a six-coordinated complex with a distorted octahedral geometry around the FeIII atom. Extensive intermolecular O—H...O, N—H...O and C—H...O hydrogen bonds, involving the complex anion, (pydaH+ counter-ion and two uncoordinated water molecules, and π–π [centroid-to-centroid distance 3.323 (11 Å] and C—O...π [O–centroid distance 3.150 (15 Å] interactions connect the various components into a supramolecular structure.

  8. 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.

  9. The synthesis of 7-chloro-5-pentadeuteriophenyl-1-methyl-1H-1, 5-benzodiazepine-2,4(3H, 5H)dione ([2H5]clobazam)

    International Nuclear Information System (INIS)

    Borel, A.G.; Abbott, F.S.

    1990-01-01

    Pentadeuteriophenyl clobazam was synthesized in essentially quantitative isotopic purity, and characterized by 1 H-NMR and mass spectroscopy. The title compound was found to be >98% pure by HPLC, and its retention time (t R 6.17 min) was less than that of an authentic clobazam standard (t R 6.32 min). Of the five steps in the synthesis of clobazam, the most susceptible to deuterium exchange was the nucleophilic substitution of 2,4-dichloronitrobenzene by aniline-d 7 to form N-(5-chloro-2-nitrophenyl)penta-deuteriophenylamine. In this step, the isotopic impurity aniline-2,3,4,5-d 5 introduced protons from nitrogen into the ortho and para positions of the deuteriophenyl ring of N-(5-chloro-2-nitrophenyl)pentadeuteriophenylamine. (author)

  10. 4,4′-Dimethoxy-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

    2011-09-01

    Full Text Available The title compound, C23H30N2O4, is a Mannich base useful for studying the effect of an electron-donating phenol substituent on intramolecular hydrogen bonding. In the molecular structure, the cyclohexane ring adopts a chair conformation and the five-membered ring has a twisted envelope conformation. Each methoxy group is oriented in the same plane of the respective aromatic ring, showing torsion angles below 11.8 (3° and bond angles between the methoxy group and the aromatic ring of 116.6 (2 and 116.6 (1°. The structure shows interactions between two the N atoms of the heterocyclic ring and the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. In the crystal, C—H...O interactions are observed. The crystal studied was a racemic mixture of RR and SS enantiomers.

  11. Crystal structure of 5,7,12,14-tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-dione

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    Mohammad Nozari

    2016-12-01

    Full Text Available The lattice of 5,7,12,14-tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-dione, C34H20O2, at 173 K has triclinic (P-1 symmetry and crystallizes with four independent half-molecules in the asymmetric unit. Each molecule is generated from a C17H10O substructure through an inversion center at the centroid of the central quinone ring, generating a wide H-shaped molecule, with a dihedral angle between the mean planes of the terminal benzene rings in each of the two symmetry-related pairs over the four molecules of 68.6 (1 (A, 65.5 (4 (B, 62.3 (9 (C, and 65.8 (8° (D, an average of 65.6 (1°. This compound has applications in gas-separation membranes constructed from polymers of intrinsic microporosity (PIM. The title compound is a product of a double Diels–Alder reaction between anthracene and p-benzoquinone followed by dehydrogenation. It has also been characterized by cyclic voltammetry and rotating disc electrode polarography, FT–IR, high resolution mass spectrometry, elemental analysis, and 1H NMR.

  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. Preparation of (7,8-3H) dopamine

    International Nuclear Information System (INIS)

    Shen Qiyuan; Tang Guozhong; Guo Zili

    1986-01-01

    Dopamine is a neurotransmitter in the central nervous system. (7,8- 3 H) dopamine is an important tracer for the study of physiological functions and metabolic processes. It was prepared by catalytic reduction of 3-hydroxy-4-methoxy-8-nitro-styrene with tritium gas. At the end of reaction, hydrobromic acid was added and heated to remove the methoxyl group. The crude product was purified by paper chromatography. The purity of (7,8- 3 H) dopamine was identified by IR, UV, PC and 3 H-NMR spectra. The radiochemical purity was over 95% and the specific activity was 1.26 x 10 12 Bq/mmol (34 Ci/mmol). The distribution of labelled tritium in molecule was shown as follows: 55.4% at position 7 and 44.6% at position 8

  14. (3-Benzoyl-1,7,7-trimethylbicyclo[2.2.1]heptan-2-olato-κ2O,Obis[2-(2-pyridylphenyl-κ2C1,N]iridium(III

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    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°.

  15. (meso-5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II dibromide dihydrate

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    Yonghong Lu

    2010-10-01

    Full Text Available The asymmetric unit of the title compound, [Ni(C16H32N4]Br2·2H2O, consists of one half [Ni(C16H32N4]2+ cation, one Br− anion and one water molecule of crystallization. The NiII ion lies on an inversion centre in a square-planar environment formed by the four macrocyclic ligand N atoms. In the crystal structure, the cations, anions and water molecules are linked via intermolecular N—H...Br and O—H...Br hydrogen bonds, forming discrete chains with set-graph motif D(2D22(7D21(3D32(8. The water molecules and Br− ions are linked with set-graph motif R42(8.

  16. 2,3-Diamino-pyridinium 6-carb-oxy-pyridine-2-carboxyl-ate.

    Science.gov (United States)

    Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein

    2011-12-01

    The asymmetric unit of the title proton-transfer compound, C(5)H(8)N(3) (+)·C(7)H(4)NO(4) (-), consists of one mono-deprotonated pyridine-2,6-dicarb-oxy-lic acid as anion and one protonated 2,3-diamino-pyridine as cation. The crystal packing shows extensive O-H⋯O, N-H⋯O and N-H⋯N hydrogen bonds. Thre are also several π-π inter-actions between the anions and also between the cations [centriod-centroid distances = 3.6634 (7), 3.7269 (7), 3.6705 (7) and 3.4164 (7) Å].

  17. Crystal structure of [(2R,3R,4S)-3,4-bis(acet-yloxy)-5-iodo-3,4-di-hydro-2H-pyran-2-yl]methyl acetate.

    Science.gov (United States)

    Zukerman-Schpector, Julio; Caracelli, Ignez; Stefani, Hélio A; Shamim, Anwar; Tiekink, Edward R T

    2015-01-01

    In the title compound, C12H15IO7, the 3,4-di-hydro-2H-pyran ring is in a distorted half-boat conformation with the atom bearing the acet-yloxy group adjacent to the C atom bearing the methyl-acetate group lying 0.633 (6) Å above the plane of the remaining ring atoms (r.m.s. deviation = 0.0907 Å). In the crystal, mol-ecules are linked into a supra-molecular chain along the a axis through two C-H⋯O inter-actions to the same acceptor carbonyl O atom; these chains pack with no specific inter-molecular inter-actions between them.

  18. Tris(2,2′-bipyridine-κ2N,N′cobalt(III bis[bis(pyridine-2,6-dicarboxylato-κ3O2,N,O6cobaltate(III] perchlorate dimethylformamide hemisolvate 1.3-hydrate

    Directory of Open Access Journals (Sweden)

    Irina A. Golenya

    2012-10-01

    Full Text Available In the title compound, [Co(C10H8N23][Co(C7H3NO42]2(ClO4·0.5C3H7NO·1.3H2O, the CoIII atom in the complex cation is pseudooctahedrally coordinated by six N atoms of three chelating bipyridine ligands. The CoIII atom in the complex anion is coordinated by two pyridine N atoms and four carboxylate O atoms of two doubly deprotonated pyridine-2,6-dicarboxylate ligands in a distorted octahedral geometry. One dimethylformamide solvent molecule and two water molecules are half-occupied and one water molecule is 0.3-occupied. O—H...O hydrogen bonds link the water molecules, the perchlorate anions and the complex anions. π–π interactions between the pyridine rings of the complex anions are also observed [centroid–centroid distance = 3.804 (3 Å].

  19. Kinetic Investigation of Homogeneous H(2)-D(2) Equilibration Catalyzed by Pt-Au Cluster Compounds. Characterization of the Cluster [(H)Pt(AuPPh(3))(9)](NO(3))(2).

    Science.gov (United States)

    Rubinstein, Leon I.; Pignolet, Louis H.

    1996-11-06

    The new Pt-Au hydrido cluster compound [(H)Pt(AuPPh(3))(9)](NO(3))(2) (3) has been synthesized and characterized by NMR, FABMS, and single-crystal X-ray diffraction [triclinic, P&onemacr;, a = 17.0452(1) Å, b = 17.4045(2) Å, c = 55.2353(1) Å, alpha = 89.891(1) degrees, beta = 85.287(1) degrees, gamma = 75.173(1) degrees, V = 15784.0(2) Å(3), Z = 4 (two molecules in asymmetric unit), residual R = 0.089 for 45 929 observed reflections and 3367 variables, Mo Kalpha radiation]. The Pt(AuP)(9) core geometry is a distorted icosahedron with three vertices vacant. The Pt-Au, Au-Au, and Au-P distances are within the normal ranges observed in other Pt-Au clusters. This cluster is a catalyst for H(2)-D(2) equilibration in homogeneous solution phase and has been used in a general mechanistic study of this reaction catalyzed by Pt-Au clusters. We previously proposed that a key step in the mechanism for catalytic H(2)-D(2) equilibration is the dissociation of a PPh(3) ligand to give a cluster with an open Au site for bonding of H(2) or D(2). This was based on qualitative observations that PPh(3) inhibited the rate of HD production with [Pt(AuPPh(3))(8)](NO(3))(2) (1) as catalyst. In order to test this hypothesis, phosphine inhibition (on the rate of HD production) and phosphine ligand exchange kinetic experiments were carried out with [(H)(PPh(3))Pt(AuPPh(3))(7)](NO(3))(2) (2) and 3. In this paper we show that the rate constant for phosphine dissociation determined from the PPh(3) inhibition rate study of H(2)-D(2) equilibration with cluster 2 is nearly identical to the rate constant for dissociative phosphine ligand exchange. The slower rate for H(2)-D(2) equilibration observed with 3 compared with 2 (5.5 x 10(-3) vs 7.7 x 10(-2) turnover s(-1)) is explained by its smaller rate constant for phosphine dissociation (2.8 x 10(-5) vs 2.9 x 10(-4) s(-1)). The fact that clusters 2 and 3 show similar kinetic behaviors suggests that the PPh(3) dissociation step in the catalytic H(2

  20. Study on the Alkylation Reactions of N(7)-Unsubstituted 1,3-Diazaoxindoles.

    Science.gov (United States)

    Kókai, Eszter; Halász, Judit; Dancsó, András; Nagy, József; Simig, Gyula; Volk, Balázs

    2017-05-19

    The chemistry of the 5,7-dihydro-6 H -pyrrolo[2,3- d ]pyrimidin-6-one (1,3-diazaoxindole) compound family, possessing a drug-like scaffold, is unexplored. In this study, the alkylation reactions of N (7)-unsubstituted 5-isopropyl-1,3-diazaoxindoles bearing various substituents at the C (2) position have been investigated. The starting compounds were synthesized from the C (5)-unsubstituted parent compounds by condensation with acetone and subsequent catalytic reduction of the 5-isopropylidene moiety. Alkylation of the thus obtained 5-isopropyl derivatives with methyl iodide or benzyl bromide in the presence of a large excess of sodium hydroxide led to 5,7-disubstituted derivatives. Use of butyllithium as the base rendered alkylation in the C (5) position possible with reasonable selectivity, without affecting the N (7) atom. During the study on the alkylation reactions, some interesting by-products were also isolated and characterized.

  1. Photoionization of three isomers of the C9H7 radical.

    Science.gov (United States)

    Hemberger, Patrick; Steinbauer, Michael; Schneider, Michael; Fischer, Ingo; Johnson, Melanie; Bodi, Andras; Gerber, Thomas

    2010-04-15

    Three resonance-stabilized radicals, 1-indenyl (Ind), 1-phenylpropargyl (1PPR), and 3-phenylpropargyl (3PPR), all isomers of the composition C(9)H(7), were generated by jet flash pyrolysis. Their photoionization was examined by VUV synchrotron radiation. The mass spectra show a clean and efficient radical generation when the pyrolysis is turned on. To study the photoionization, photoion yield measurements and threshold photoionization spectroscopy techniques were applied. We determined adiabatic ionization energies (IE(ad)) of 7.53 eV for Ind, 7.20 eV for 3PPR, and 7.4 eV for 1PPR. Ab initio calculations show no major change in geometry upon ionization, in agreement with ionization from a nonbonding molecular orbital. The IEs were also computed and are in agreement with the measured ones. The difference in the IE might allow a distinction of the three isomers in flames. In the indenyl spectrum, an excited a(+) (3)B(2) state of the cation was identified at 8.10 eV, which shows a low-energy vibrational progression of 61 meV. Furthermore, we have examined the dissociative photoionization of the precursors. The indenyl precursor, 1-indenyl bromide, undergoes dissociative photoionization to Ind(+). An appearance energy (AE(0K)) of 10.2 eV was obtained from fitting the experimental breakdown diagram. A binding energy of 1.8 eV can thus be determined for the C-Br bond in 1-indenyl bromide. The phenylpropargyl precursors 1PPBr (1-phenylpropargyl bromide/3-phenyl-3-bromopropyne) and 3PPBr (3-phenylpropargyl bromide/1-phenyl-3-bromopropyne) also lose a bromine atom upon dissociative photoionization. Approximate appearance energies of 9.8 eV for 3PPBr and 9.3 eV for 1PPBr have been determined.

  2. Supramolecular architecture of 5-bromo-7-methoxy-1-methyl-1H-benzoimidazole.3H2O: Synthesis, spectroscopic investigations, DFT computation, MD simulations and docking studies

    Science.gov (United States)

    Murthy, P. Krishna; Smitha, M.; Sheena Mary, Y.; Armaković, Stevan; Armaković, Sanja J.; Rao, R. Sreenivasa; Suchetan, P. A.; Giri, L.; Pavithran, Rani; Van Alsenoy, C.

    2017-12-01

    Crystal and molecular structure of newly synthesized compound 5-bromo-7-methoxy-1-methyl-1H-benzoimidazole (BMMBI) has been authenticated by single crystal X-ray diffraction, FT-IR, FT-Raman, 1H NMR, 13C NMR and UV-Visible spectroscopic techniques; compile both experimental and theoretical results which are performed by DFT/B3LYP/6-311++G(d,p) method at ground state in gas phase. Visualize nature and type of intermolecular interactions and crucial role of these interactions in supra-molecular architecture has been investigated by use of a set of graphical tools 3D-Hirshfeld surfaces and 2D-fingerprint plots analysis. The title compound stabilized by strong intermolecular hydrogen bonds N⋯Hsbnd O and O⋯Hsbnd O, which are envisaged by dark red spots on dnorm mapped surfaces and weak Br⋯Br contacts envisaged by red spot on dnorm mapped surface. The detailed fundamental vibrational assignments of wavenumbers were aid by with help of Potential Energy distribution (PED) analysis by using GAR2PED program and shows good agreement with experimental values. Besides frontier orbitals analysis, global reactivity descriptors, natural bond orbitals and Mullikan charges analysis were performed by same basic set at ground state in gas phase. Potential reactive sites of the title compound have been identified by ALIE, Fukui functions and MEP, which are mapped to the electron density surfaces. Stability of BMMBI have been investigated from autoxidation process and pronounced interaction with water (hydrolysis) by using bond dissociation energies (BDE) and radial distribution functions (RDF), respectively after MD simulations. In order to identify molecule's most important reactive spots we have used a combination of DFT calculations and MD simulations. Reactivity study encompassed calculations of a set of quantities such as: HOMO-LUMO gap, MEP and ALIE surfaces, Fukui functions, bond dissociation energies and radial distribution functions. To confirm the potential

  3. Nano crystalline ZnO catalyzed one pot three-component synthesis of 7-alkyl-6H,7H- naphtho[1',2':5,6]pyrano[3,2-c] chromen-6-ones under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    M. J. Piltan

    2016-08-01

    Full Text Available In the present paper, an efficient one-pot synthesis of 7-alkyl-6H,7H-naphtho[1',2':5,6]pyrano[3,2-c]chromen-6-ones is described by three-component reaction of β-naphthol, aromatic aldehydes and 4-hydroxycoumarin using ZnO nanoparticles under solvent-free conditions. The present method provides a novel and efficient procedure for the synthesis of chromene derivatives with some advantageous such as short reaction times, easy workup, high yields, wide range of products, reusability of the catalyst, little catalyst loading and green conditions in the presence of ZnO nanoparticles (7 mol% at 110 ºC.

  4. 3,5-Dimethyl-4-nitroso-1H-pyrazole

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    Inna Safyanova

    2011-09-01

    Full Text Available In the unit cell of the title compound, C5H7N3O, there are two conformers (A and B which differ in the position of the oxime group with respect to the protonated pyrazole nitrogen (trans in the A conformer and cis in the B conformer and in the geometric parameters. The oxime group exists in the nitroso form in both conformers. In the crystal, molecules are linked by intermolecular N—H...O and N—H...N hydrogen bonds into zigzag-like chains along the b axis.

  5. Synthesis and Fungicidal Activities of (Z/E-3,7-Dimethyl-2,6-octadienamide and Its 6,7-Epoxy Analogues

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    Mingyan Yang

    2015-11-01

    Full Text Available In order to find new lead compounds with high fungicidal activity, (Z/E-3,7-dimethyl-2,6-octadienoic acids were synthesized via selective two-step oxidation using the commercially available geraniol/nerol as raw materials. Twenty-eight different (Z/E-3,7-dimethyl-2,6-octadienamide derivatives were prepared by reactions of (Z/E-carboxylic acid with various aromatic and aliphatic amines, followed by oxidation of peroxyacetic acid to afford their 6,7-epoxy analogues. All of the compounds were characterized by HR-ESI-MS and 1H-NMR spectral data. The preliminary bioassays showed that some of these compounds exhibited good fungicidal activities against Rhizoctonia solani (R. solani at a concentration of 50 µg/mL. For example, 5C, 5I and 6b had 94.0%, 93.4% and 91.5% inhibition rates against R. solani, respectively. Compound 5f displayed EC50 values of 4.3 and 9.7 µM against Fusahum graminearum and R. Solani, respectively.

  6. {2-[(4-Nitrobenzylideneamino]-4,5,6,7-tetrahydro-1-benzothiophen-3-yl}(phenylmethanone

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    Manpreet Kaur

    2014-06-01

    Full Text Available In the title compound, C22H18N2O3S, disorder is found in the benzoyl group (A and B, as well as for four C atoms of the cyclohexene ring. Two orientations were modeled in a 0.583 (5:0.417 (5 ratio. The cyclohexene ring is in a distorted chair conformation. The dihedral angles between the mean plane of the thiophene ring and the 4-nitrobenzene and phenyl rings are 30.9 (8 and 64.8 (3 (A and 62.4 (7° (B. The mean planes of the 4-nitrobenzene and the phenyl rings are almost perpendicular to each other, with dihedral angles of 85.4 (1 (A and 83.9 (8° (B. An extensive array of weak C—H...O interactions consolidate molecules into a three-dimensional architecture, forming chains along [001] and [010] and layers parallel to (011.

  7. Proton-transfer compounds of 8-hydroxy-7-iodoquinoline-5-sulfonic acid (ferron) with 4-chloroaniline and 4-bromoaniline.

    Science.gov (United States)

    Smith, Graham; Wermuth, Urs D; Healy, Peter C

    2007-07-01

    The crystal structures of the proton-transfer compounds of ferron (8-hydroxy-7-iodoquinoline-5-sulfonic acid) with 4-chloroaniline and 4-bromoaniline, namely 4-chloroanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)ClN(+) x C(9)H(5)INO(4)S(-) x H(2)O, and 4-bromoanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)BrN(+) x C(9)H(5)INO(4)S(-) x H(2)O, have been determined. The compounds are isomorphous and comprise sheets of hydrogen-bonded cations, anions and water molecules which are extended into a three-dimensional framework structure through centrosymmetric R(2)(2)(10) O-H...N hydrogen-bonded ferron dimer interactions.

  8. Synthesis and reactions of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one

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    NAGWA M.S. EL-DIN HARB

    1999-11-01

    Full Text Available The condensation of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one (3, prepared by the reaction of 6-[5,6,7,8-tetrahydro-2-naphthyl]-4,5-dihydropyridazin-3(2H-one (1 and anisaldehyde, with dimethyl sulphate, formaldehyde and acrylonitrile, and also the formation of the Mannich base, proceeded smoothly at the 2-position to give compounds 4,5,6,7, respectively. 4-p-Methoxybenzyl-3-chloro-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazine (9 was prepared in law yield by the action of phosphorus oxychloride on 3. The reaction of 9 with benzylamine, aniline and piperidine gave 10a,b,c, respectively. 4-p-Methoxybenzyl-6-[5,6,7,8-tetrahydro-2-napthyl]pyridazine-3(2H-thione (12 was prepared either by the action of thiourea on 9, or by the reaction of 3 with phosphorus pentasulphide. The reaction of these thiones with acrylonitrile, morpholine and piperidine to give 13 and 14 a,b, respectively, were also investigated.

  9. Amino Acid Substitutions Improve the Immunogenicity of H7N7HA Protein and Protect Mice against Lethal H7N7 Viral Challenge.

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    Subaschandrabose Rajesh Kumar

    Full Text Available Avian influenza A H7N7/NL/219/03 virus creates a serious pandemic threat to human health because it can transmit directly from domestic poultry to humans and from human to human. Our previous vaccine study reported that mice when immunized intranasally (i.n with live Bac-HA were protected from lethal H7N7/NL/219/03 challenge, whereas incomplete protection was obtained when administered subcutaneously (s.c due to the fact that H7N7 is a poor inducer of neutralizing antibodies. Interestingly, our recent vaccine studies reported that mice when vaccinated subcutaneously with Bac-HA (H7N9 was protected against both H7N9 (A/Sh2/2013 and H7N7 virus challenge. HA1 region of both H7N7 and H7N9 viruses are differ at 15 amino acid positions. Among those, we selected three amino acid positions (T143, T198 and I211 in HA1 region of H7N7. These amino acids are located within or near the receptor binding site. Following the selection, we substituted the amino acid at these three positions with amino acids found on H7N9HA wild-type. In this study, we evaluate the impact of amino acid substitutions in the H7N7 HA-protein on the immunogenicity. We generated six mutant constructs from wild-type influenza H7N7HA cDNA by site directed mutagenesis, and individually expressed mutant HA protein on the surface of baculovirus (Bac-HAm and compared their protective efficacy of the vaccines with Bac-H7N7HA wild-type (Bac-HA by lethal H7N7 viral challenge in a mouse model. We found that mice immunized subcutaneously with Bac-HAm constructs T143A or T198A-I211V or I211V-T143A serum showed significantly higher hemagglutination inhibition and neutralization titer against H7N7 and H7N9 viruses when compared to Bac-HA vaccinated mice groups. We also observed low level of lung viral titer, negligible weight loss and complete protection against lethal H7N7 viral challenge. Our results indicated that amino acid substitution at position 143 or 211 improve immunogenicity of H7N7HA

  10. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

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    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.

  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. 6a-Nitro-6-(2,2,7,7-tetramethyltetrahydro-3aH-bis[1,3]dioxolo[4,5-b:4′,5′-d]pyran-5-yl-6a,6b,7,8,9,11a-hexahydro-6H-spiro[chromeno[3,4-a]pyrrolizine-11,11′-indeno[1,2-b]quinoxaline

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    T. Anuradha

    2014-01-01

    Full Text Available In the title compound, C39H38N4O8, the quinoxaline and indene subunits are essentially planar, with maximum deviations of 0.071 (2 and 0.009 (2 Å, respectively. The indenoquinoxaline system forms a dihedral angle of 72.81 (3° with the chromenopyrrolizine system. The two dioxolane rings, as well as the pyran ring of the chromeno group and the terminal pyrrolizine, each adopt an envelope conformation with O and C as flap atoms. The central pyrrolizine ring adopts a twisted conformation. Intramolecular C—H...O and C—H...N hydrogen bonds occur. The crystal structure exhibits C—H...O hydrogen bonds, and is further stablized by C—H...π interactions, forming a two-dimensional network along the bc plane.

  13. 7α-Methoxycarbonyl-6,7,8,14-tetrahydro-6,14-endo-ethenothebaine

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    Mustafa Odabaşoğlu

    2009-04-01

    Full Text Available In the molecule of the title compound, C23H27NO5, the furan ring adopts an envelope conformation. Intramolecular C—H...O interactions result in the formation of S(5 and S(6 motifs. In the crystal structure, weak intermolecular C—H...O hydrogen bonds link the molecules through C(6 and C(8 chains along the [100] and [010] directions, generating a two-dimensional network.

  14. Synthesis and characterisation of 5-acyl-6,7-dihydrothieno[3,2-c]pyridine inhibitors of Hedgehog acyltransferase

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    Thomas Lanyon-Hogg

    2016-06-01

    Full Text Available In this data article we describe synthetic and characterisation data for four members of the 5-acyl-6,7-dihydrothieno[3,2-c]pyridine (termed “RU-SKI” class of inhibitors of Hedgehog acyltransferase, including associated NMR spectra for final compounds. RU-SKI compounds were selected for synthesis based on their published high potencies against the enzyme target. RU-SKI 41 (9a, RU-SKI 43 (9b, RU-SKI 101 (9c, and RU-SKI 201 (9d were profiled for activity in the related article “Click chemistry armed enzyme linked immunosorbent assay to measure palmitoylation by Hedgehog acyltransferase” (Lanyon-Hogg et al., 2015 [1]. 1H NMR spectral data indicate different amide conformational ratios between the RU-SKI inhibitors, as has been observed in other 5-acyl-6,7-dihydrothieno[3,2-c]pyridines. The synthetic and characterisation data supplied in the current article provide validated access to the class of RU-SKI inhibitors.

  15. (1S,1′S,2′R,4a'S,9a'S,9b'R-1′-Acetyloxy-2,4′-dioxo-2′,4′,4a',7′,8′,9′,9a',9b'-octahydro-1′H,2H-spiro[acenaphthylene-1,5′-pyrano[4,3-a]pyrrolizin]-2′-ylmethyl acetate

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    S. Santhiya

    2013-11-01

    Full Text Available In the title compound C26H25NO7, the mean plane through the lactone-substituted ring of the pyrrolizidine moiety forms dihedral angles of 78.46 (6 and 58.28 (8° with the acenaphthylene moiety and the sugar based-lactone ring, respectively. The sum of the angles at the the N atom of the pyrrolizidine ring (335.0° is in accordance with sp3 hybridization. Some atoms of the acetate group are disordered and were refined using a split model [occupancy ratio 0.673 (10:0.327 (10].

  16. A Theoretical investigation of a potential high energy density compound 3,6,7,8-tetranitro-3,6,7,8-tetraaza-tricyclo[3.1.1.1(2,4]octane

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    Guozheng Zhao

    2013-01-01

    Full Text Available The B3LYP/6-31G (d density functional theory (DFT method was used to study molecular geometry, electronic structure, infrared spectrum (IR and thermodynamic properties. Heat of formation (HOF and calculated density were estimated to evaluate detonation properties using Kamlet-Jacobs equations. Thermal stability of 3,6,7,8-tetranitro-3,6,7,8-tetraaza-tricyclo [3.1.1.1(2,4]octane (TTTO was investigated by calculating bond dissociation energy (BDE at the unrestricted B3LYP/6-31G(d level. Results showed the N-NO2 bond is a trigger bond during the thermolysis initiation process. The crystal structure obtained by molecular mechanics (MM methods belongs to P2(1/C space group, with cell parameters a = 8.239 Å, b = 8.079 Å, c = 16.860 Å, Z = 4 and r = 1.922 g cm-3. Both detonation velocity of 9.79 km s-1 and detonation pressure of 44.22 GPa performed similarly to CL-20. According to the quantitative standards of energetics and stability, TTTO essentially satisfies this requirement as a high energy density compound (HEDC.

  17. 4-(1,3-Diphenyl-4,5-dihydro-1H-pyrazol-5-yl-1,3-diphenyl-1H-pyrazole

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    Hoong-Kun Fun

    2011-11-01

    Full Text Available The title compound, C30H24N4, contains two pyrazole rings and four phenyl rings. The pyrazole rings are essentially planar, with maximum deviations of 0.003 (1 and 0.066 (1 Å and make a dihedral angle of 73.43 (6°. The two pyrazole rings make dihedral angles of 40.08 (6, 9.28 (6, 15.78 (8 and 17.25 (7° with their attached phenyl rings. In the crystal, there are no significant intermolecular hydrogen-bonding interactions. The crystal structure is stabilized by C—H...π interactions.

  18. Crystal structure of 4-(1H-indol-3-yl-2-(4-methoxyphenyl-6-phenylpyridine-3-carbonitrile

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    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".

  19. 7-Chloro-11a-phenyl-2,3,5,10,11,11a-hexahydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11-dione

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    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.

  20. 7,7′,8,8′-Tetramethoxy-4,4′-dimethyl-3,3′-bicoumarin

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    Hoong-Kun Fun

    2009-06-01

    Full Text Available In the crystal structure, the title compound, C24H22O8, lies on a twofold rotation axis and the asymmetric unit comprises one half-molecule. The dihedral angle formed by the coumarin unit with the symmetry-related part is 74.78 (14°. One of the methoxy groups attached to the coumarin unit is considerably twisted, making an angle of 87.17 (17° with respect to the coumarin unit; the other is twisted by 0.66 (19°. No classical hydrogen bonds are found in the sturcture; only a weak C—H...π interaction and short intramolecular O...O contacts [2.683 (2–2.701 (2 Å] are observed.

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

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    Gene-Hsiang Lee

    2006-06-01

    Full Text Available 1-Allyl- (2 and 7-allyl-6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (3 were obtained via the 18-crown-6-ether catalyzed room temperature reactionof 6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (1 with potassiumcarbonate and allyl bromide in dry acetone. The structures of these two derivatives wereverified by 2D-NMR measurements, including gHSQC and gHMBC measurements. Theminor compound 2 may possess aromatic character. A single crystal X-ray diffractionexperiment indicated that the major compound 3 crystallizes from dimethyl sulfoxide in themonoclinic space group P21/n and its molecular structure includes an attached dimethylsulfoxide molecule, resulting in the molecular formula C10H16N6O2S. Molecular structuresof 3 are linked by extensive intermolecular N-H···N hydrogen bonding [graph set C 1 (7]. 1Each molecule is attached to the dimethyl sulfoxide oxygen via N-H···O intermolecularhydrogen bonding. The structure is further stabilized by π-π stacking interactions.

  2. B7-H3 in tumors: friend or foe for tumor immunity?

    Science.gov (United States)

    Li, Gen; Quan, Yanchun; Che, Fengyuan; Wang, Lijuan

    2018-02-01

    B7-H3 is a type I transmembrane co-stimulatory molecule of the B7 family. B7-H3 mRNA is widely distributed in most tissues; however, B7-H3 protein is not constitutively expressed. Few molecules have been shown to mediate the regulation of B7-H3 expression, and their regulatory mechanisms remain unexplored. Recently, TREM-like transcript 2 (TLT-2) has been identified as a potential receptor of B7-H3. However, TLT-2 may not be the only receptor of B7-H3, as B7-H3 has many contradictory roles. As a co-stimulatory molecule, B7-H3 increases the proliferation of both CD4+ and CD8+ T-cells and enhances cytotoxic T-cell activity. However, greatly increased T-cell proliferation and IL-2 levels have been observed in the absence of B7-H3. Thus far, it has been shown that various tumors test positive for B7-H3 expression and that B7-H3 levels correlate with tumor growth, invasion, metastasis, malignant stage, and recurrence rate. Furthermore, transfection of cells with a B7-H3 plasmid and treatment with monoclonal antibodies to block B7-H3 are the main immunotherapeutic strategies for cancer treatment. Several groups have generated anti-B7-H3 antibodies and observed tumor growth suppression in vitro and in vivo. Therefore, it is likely that B7-H3 plays an important role in cancer diagnosis and treatment, aside from its role as a co-stimulatory molecule.

  3. 6-Hydroxy-5-[(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-enyl(4-nitrophenylmethyl]-1,3-dimethylpyrimidine-2,4(1H,3H-dione

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    N. Sureshbabu

    2013-11-01

    Full Text Available In the title compound, C21H23N3O7, the pyrimidinedione ring adopts a screw-boat conformation, whereas the cyclohexenone ring adopts an envelope conformation, with the C atom bearing the methyl groups as the flap atom. The dihedral angle between the mean planes of the pyrimidinedione and cyclohexenone rings is 58.78 (2°. The pyrimidinedione and cyclohexenone rings form dihedral angles of 59.94 (3 and 54.73 (2°, respectively, with the 4-nitrophenyl ring. Relatively strong intramolecular O—H...O hydrogen bonds are observed. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a chain along the c-axis direction.

  4. Solvothermal synthesis, crystal structure, and second-order nonlinear optical properties of a new noncentrosymmetric gallium-organic framework material, [N(C{sub 3}H{sub 7}){sub 4}]{sub 3}Ga{sub 3}[C{sub 6}H{sub 3}(CO{sub 2}){sub 3}]{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Dong Woo; Jo, Vinna [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of); Ok, Kang Min, E-mail: kmok@cau.ac.kr [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of)

    2012-10-15

    A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C{sub 3}H{sub 7}){sub 4}]{sub 3}Ga{sub 3}[C{sub 6}H{sub 3}(CO{sub 2}){sub 3}]{sub 4} (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO{sub 3}){sub 3}{center_dot}xH{sub 2}O, 1,3,5-C{sub 6}H{sub 3}(CO{sub 2}H){sub 3}, N(C{sub 3}H{sub 7}){sub 4}Cl, HNO{sub 3}, and HCON(CH{sub 3}){sub 2} at 180 Degree-Sign C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO{sub 4} tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of {alpha}-SiO{sub 2} and the material is phase-matchable (type-1). - Graphical Abstract: Second-order nonlinear optical measurements on CAUMOF-11 reveal that the material is phase-matchable (type-1) with SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Highlights: Black-Right-Pointing-Pointer A new NCS Ga-organic framework was solvothermally synthesized. Black-Right-Pointing-Pointer CAUMOF-11 exhibits SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Black-Right-Pointing-Pointer Thermal decomposition of CAUMOF-11 crystal maintains the original morphology.

  5. 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.

  6. 3-(4-Fluorophenyl-1-[1′-(4-fluorophenyl-2-oxo-5′,6′,7′,7a′-tetrahydro-1H-indole-3(2H-spiro-3′(2′H-1H′-pyrrolizin-2′-yl]prop-2-en-1-one

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    S. Sriman Narayanan

    2008-09-01

    Full Text Available In the title compound, C29H24F2N2O2, one of the pyrrolidine rings of the pyrrolizine system is disordered over two sites, with occupancy factors 0.734:0.266 (12. Both components of the disordered pyrrolidine ring adopt envelope conformations, whereas the other pyrrolidine ring adopts a twist conformation. The molecules are linked into centrosymmetric dimers by N—H...O hydrogen bonds and the dimers are connected via C—H...π interactions. The crystal structure is also stabilized by intermolecular C—H...F hydrogen bonds.

  7. Targeting B7x and B7-H3 as New Immunotherapies for Prostate Cancer

    Science.gov (United States)

    2017-11-01

    prostate   cancer  and  other   cancers .   15. SUBJECT TERMS B7x, B7-H3, HHLA2, TMIGD2, Receptors , Immune Checkpoint, Prostate Cancer , Monoclonal...H3,  HHLA2,  TMIGD2,   Receptors ,  Immune  Checkpoint,   Prostate   Cancer ,   Monoclonal  Antibodies,  Crystal  Structure,  Immunotherapy,  T  Cells... prostate   cancer  immunotherapy.       Unlike  B7x  and  B7H3  whose   receptors  have  not  been  found  yet,  we  have   quickly  discovered  two

  8. 3′,6′-Bis(ethylamino-2′,7′-dimethyl-2-{2-(E-[(thiophen-2-ylmethylideneamino]ethyl}spiro[isoindoline-1,9′-xanthen]-3-one methanol monosolvate

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    Rui Guo

    2012-05-01

    Full Text Available The title compound, C33H34N4O2S·CH3OH, was prepared as a spirolactam ring formation of rhodamine 6 G dye for comparison with a ring-opened form. The xanthene and spirolactam rings are approximately planar [r.m.s. deviations from planarity = 0.122 (3 and 0.072 (6 Å, respectively]. The dihedral angles formed by the spirolactam and thiophene rings with the xanthene ring system are 89.7 (6 and 86.5 (2°, respectively. The crystal structure features N—H...O and C—H...O hydrogen bonds.

  9. Synthesis, Characterization and Biological Studies of New Phenyltin(IV) Dithiocarbamate Compounds

    International Nuclear Information System (INIS)

    Amirah Faizah Abdul Muthalib; Ibrahim Baba; Nazlina Ibrahim

    2015-01-01

    Nine chlorophenyl tin(IV) dithiocarbamate compounds of general formula PhSnCl[S 2 CNR ' R '' ] 2 (R ' = CH 3 , C 2 H 5 , C 7 H 7 and R ' = C 2 H 5 , C 6 H 11 , iC 3 H 7 , C 7 H 7 ) were prepared in one pot reaction of various secondary amine, carbon disulphide and phenyltin(1V) trichloride with the ratio of 2:2:1. These compounds have been characterized by elemental analysis, infrared spectroscopy, ultraviolet spectroscopy, 1 H, 13 C NMR spectroscopy as well as single crystal X-ray crystallography. Data from X-ray crystallography showed that (C 6 H 5 )SnCl[S 2 CN(C 2 H 5 )(iC 3 H 7 )] 2 is six coordinated bonded with two chelating dithiocarbamate ligands in bidentate fashion, methyl-C and chloride atom thus form a distorted octahedral geometry. Five selected compounds, (C 6 H 5 )SnCl[S 2 CN(CH 3 )(C 2 H 5 )] 2 , (C 6 H 5 )SnCl[S 2 CN(CH 3 )(C 6 H 11 )] 2 , (C 6 H 5 )SnCl[S 2 CN(C 2 H 5 )(iC 3 H 7 )] 2 , (C 6 H 5 )SnCl[S 2 CN(C 7 H 7 )(iC 3 H 7 )] 2 and (C 6 H 5 )SnCl[S 2 CN(C 7 H 7 ) 2 ] 2 were screened for anticancer activity against Chang liver cells. These compounds were demonstrated no cytotoxic effect for all concentrations under the condition of the study with no IC 50 value. The minimum inhibitory concentration (MIC) and maximum bactericidal concentration (MBC) determinations for these five compounds used Escherichia coli and Pseudomonas aeruginosa as Gram negative bacteria together with Staphylococcus aureus and Staphylococcus epidermis as Gram positive bacteria. Compound (C 6 H 5 )SnCl[S 2 CN(CH 3 )(C 2 H 5 )] 2 was the most active compared to the other compounds by having the lowest MIC values of 1.25 mg/ mL and MBC value of 5.0 mg/ mL against E. Coli and S. Aureus bacteria. Compounds (C 6 H 5 )SnCl[S 2 CN(C 7 H 7 )(iC 3 H 7 )] 2 and (C 6 H 5 )SnCl[S 2 CN(C 7 H 7 ) 2 ] 2 that having a benzyl group showed their MIC and MBC values slightly higher compared to the other compounds againts certain bacteria indicating their low

  10. The 3H(α,γ)7Li reaction below Ec.m. = 1 MeV

    International Nuclear Information System (INIS)

    Brune, C.R.; Kavanagh, R.W.; Rolfs, C.

    1993-01-01

    The 3 H(α,γ) reaction, and its mirror 3 He(α,γ) are responsible for 7 Li production in the big bang. It has been demonstrated that the uncertainty in the 3 H(α,γ) reaction rate significantly affects the calculated amount of 7 Li, which is important for comparison to the observed 7 Li abundance and constraining the baryon density allowed by the standard big-bang model. Using specially prepared thin Ti- 3 H targets and an 85% high-purity germanium detector, the authors have measured the γ rays produced by the 3 H(α,γ) reaction for 50 c.m. 7 Li bound states, and angular distributions of the capture γ rays. The results are compared to previous experiments and nuclear model calculations

  11. The synthesis of 7-chloro-5-pentadeuteriophenyl-1-methyl-1H-1, 5-benzodiazepine-2,4(3H, 5H)dione (( sup 2 H sub 5 )clobazam)

    Energy Technology Data Exchange (ETDEWEB)

    Borel, A.G.; Abbott, F.S. (British Columbia Univ., Vancouver, BC (Canada). Dept. of Pharmaceutical Sciences)

    1990-07-01

    Pentadeuteriophenyl clobazam was synthesized in essentially quantitative isotopic purity, and characterized by {sup 1}H-NMR and mass spectroscopy. The title compound was found to be >98% pure by HPLC, and its retention time (t{sub R} 6.17 min) was less than that of an authentic clobazam standard (t{sub R} 6.32 min). Of the five steps in the synthesis of clobazam, the most susceptible to deuterium exchange was the nucleophilic substitution of 2,4-dichloronitrobenzene by aniline-d{sub 7} to form N-(5-chloro-2-nitrophenyl)penta-deuteriophenylamine. In this step, the isotopic impurity aniline-2,3,4,5-d{sub 5} introduced protons from nitrogen into the ortho and para positions of the deuteriophenyl ring of N-(5-chloro-2-nitrophenyl)pentadeuteriophenylamine. (author).

  12. Experimental and computational thermochemistry of 6,7-dihydro-4(5H)-benzofuranone

    International Nuclear Information System (INIS)

    Sousa, Clara C.S.; Morais, Victor M.F.; Matos, M. Agostinha R.

    2013-01-01

    Highlights: ► Standard molar enthalpy of formation of 6,7-dihydro-4(5H)-benzofuranone was obtain. ► Computational estimative of the standard molar enthalpy of formation. ► Computational and experimental values agree. ► Estimates of the standard molar enthalpy of formation of the isomers were obtain. - Abstract: The standard (p = 0.1 MPa) molar enthalpy of formation of 6,7-dihydro-4(5H)-benzofuranone was measured, at T = 298.15 K, by static bomb calorimetry and the standard molar enthalpy of vaporization, at T = 298.15 K, was obtained using Calvet microcalorimetry. These values were combined together to derive the standard molar enthalpy of formation of the title compound in gaseous phase, at T = 298.15 K, −(226.0 ± 2.8) kJ · mol −1 . Additionally, density functional theoretical calculations using the B3LYP hybrid exchange-correlation energy functional with extended basis sets and also other higher-level ab initio quantum calculations have been performed.

  13. [KDy(Hptc3(H3ptc]n·2n(Hbipy·5n(H2O, a Layered Coordination Polymer Containing DyO6N3 Tri-Capped Trigonal Prisms (H3ptc = Pyridine 2,4,6-Tricarboxylic Acid, C8H5NO6; Bipy = 2,2'-Bipyridine, C10H8N2

    Directory of Open Access Journals (Sweden)

    Shoaib Anwar

    2012-08-01

    Full Text Available The synthesis, structure and properties of the bimetallic layered coordination polymer, [KDy(C8H3NO63(C8H5NO6]n·2n(C10H9N2·5n(H2O = [KDy(Hptc3(H3ptc]n·2n(Hbipy·5n(H2O, are described. The Dy3+ ion is coordinated by three O,N,O-tridentate doubly-deprotonated pyridine tri-carboxylate (Hptc ligands to generate a fairly regular DyO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The potassium ion is coordinated by an O,N,O-tridentate H3ptc molecule as well as monodentate and bidentate Hptc ligands to result in an irregular KNO9 coordination geometry. The ligands bridge the metal-atom nodes into a bimetallic, layered, coordination polymer, which extends as corrugated layers in the (010 plane, with the mono-protonated bipyridine cations and water molecules occupying the inter-layer regions: Unlike related structures, there are no dysprosium–water bonds. Many O–HLO and N–HLO hydrogen bonds consolidate the structure. Characterization and bioactivity data are described. Crystal data: C52H42DyKN8O29, Mr = 1444.54, triclinic,  (No. 2, Z = 2, a = 9.188(2 Å, b = 15.7332(17 Å, c = 19.1664(19 Å, α = 92.797(6°, β = 92.319(7°, γ = 91.273(9°, V = 2764.3(7 Å3, R(F = 0.029, wR(F2 = 0.084.

  14. 6β-Acetoxy-1α,7β,11β,15β-tetrahydroxy-7α,20-epoxy-ent-kaur-16-ene

    Directory of Open Access Journals (Sweden)

    Fu-Lin Yan

    2010-02-01

    Full Text Available The title compound, C22H32O7, a natural ent-kaurane diterpenoid also referred to as Maoyecrystal F, was obtained from the medicinal plant Isodon nervosa. There are four rings with the expected cis and trans junctions. Cyclohexane ring A adopts a chair conformation, rings B and C adopt boat conformations, while the five-membered ring has an envelope conformation. The molecules stack along the a axis in the crystal and are linked together by intermolecular O—H...O hydrogen bonds.

  15. 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.

  16. 2-(7-Methoxy-1-naphthylacetonitrile

    Directory of Open Access Journals (Sweden)

    Wen-bin Wei

    2010-07-01

    Full Text Available The molecule of the title compound, C13H11NO, is almost planar (r.m.s. deviation = 0.013 Å, apart from the cyanide group, for which the C and N atoms deviate from the mean plane of the other atoms by 0.341 (3 and 0.571 (4 Å, respectively. In the crystal, weak aromatic π–π stacking [centroid–centroid distance = 3.758 (3 Å] may help to stabilize the structure.

  17. Crystal structure of ethyl (4R-2-amino-7-hydroxy-4-phenyl-4H-chromene-3-carboxylate

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    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.

  18. 5-(4-Methylphenylsulfonyl-1,3-dithiolo[4,5-c]pyrrole-2-thione

    Directory of Open Access Journals (Sweden)

    Ning-Juan Zheng

    2012-04-01

    Full Text Available The asymmetric unit of the title compound, C12H9NO2S4, contains one half-molecule with the N, two S amd four C atoms lying on a mirror plane. The molecule exhibits a V-shaped conformation, with a dihedral angle of 87.00 (7° between the benzene and dithiolopyrrole rings. The methyl group was treated as rotationally disordered between two orientations in a 1:1 ratio. In the crystal, weak C—H...O hydrogen bonds link the molecules into chains in [010].

  19. Radiosynthesis and in vitro validation of 3H-NS14492 as a novel high affinity alpha7 nicotinic receptor radioligand

    DEFF Research Database (Denmark)

    Magnussen, Janus H.; Ettrup, Anders; Donat, Cornelius K.

    2015-01-01

    The neuronal alpha 7 nicotinic acetylcholine receptor is a homo-pentameric ligand-gated ion channel that is a promising drug target for cognitive deficits in Alzheimer's disease and schizophrenia. We have previously described 11C-NS14492 as a suitable agonist radioligand for in vivo positron...... emission tomography (PET) occupancy studies of the alpha 7 nicotinic receptor in the pig brain. In order to investigate the utility of the same compound for in vitro studies, 3H-NS14492 was synthesized and its binding properties were characterized using in vitro autoradiography and homogenate binding...... assays in pig frontal cortex. 3H-NS14492 showed specific binding to alpha 7 nicotinic receptors in autoradiography, revealing a dissociation constant (Kd) of 2.1 ± 0.7 nM and a maximum number of binding sites (Bmax) of 15.7±2.0 fmol/mg tissue equivalent. Binding distribution was similar...

  20. 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.

  1. Crystal structure of 4′-allyl-4,5,6,7,2′,7′-hexachlorofluorescein allyl ester unknown solvate

    Directory of Open Access Journals (Sweden)

    Lili Wang

    2018-01-01

    Full Text Available In the title compound, 4′-allyl-4,5,6,7,2′,7′-hexachlorofluorescein allyl ester {systematic name: prop-2-en-1-yl 2,3,4,5-tetrachloro-6-[2,7-dichloro-6-hydroxy-3-oxo-4-(prop-2-en-1-yl-3H-xanthen-9-yl]benzoate}, C26H14Cl6O5, accompanied by unknown solvate molecules, the dihedral angle between the xanthene ring system (r.m.s. deviation = 0.046 Å and the pentasubstituted benzene ring is 71.67 (9°. Both allyl groups are disordered over two sets of sites in statistical ratios. The scattering contributions of the disordered solvent molecules (both Ph2O and CHCl3, as identified by NMR were removed with the PLATON SQUEEZE algorithm [Spek (2015. Acta Cryst. C71, 9–18]. In the crystal, tetrameric supramolecular aggregates linked by O—H...O hydrogen bonds occur; these further interact with neighboring aggregates through C—Cl...π interactions arising from the benzene rings, forming infinite two-dimensional sheets. Each C6Cl4 ring shifts in the direction perpendicular to the two-dimensional sheet, exhibiting a helical chain in which every C6Cl4 ring is utilized as both a donor and an acceptor of Cl...π contacts. Thus, these two-dimensional sheets pack in a helical fashion, constructing a three-dimensional network.

  2. 2,3-Diamino­pyridinium 6-carb­oxy­pyridine-2-carboxyl­ate

    Science.gov (United States)

    Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein

    2011-01-01

    The asymmetric unit of the title proton-transfer compound, C5H8N3C7H4NO4 −, consists of one mono-deprotonated pyridine-2,6-dicarb­oxy­lic acid as anion and one protonated 2,3-diamino­pyridine as cation. The crystal packing shows extensive O—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds. Thre are also several π–π inter­actions between the anions and also between the cations [centriod–centroid distances = 3.6634 (7), 3.7269 (7), 3.6705 (7) and 3.4164 (7) Å]. PMID:22199823

  3. New kaempferol 3,7-diglycosides from Asplenium ruta-muraria and Asplenium altajense.

    Science.gov (United States)

    Iwashina, Tsukasa; Kitajima, Junichi; Mizuno, Takayuki; Smirnov, Sergey V; Damdinsuren, Oyunchimeg; Kondo, Katsuhiko

    2015-03-01

    A flavonoid was isolated from the fronds of Asplenium ruta-muraria and A. altajense (Aspleniaceae) collected in the Altai Mountains and adjacent area. The compound was identified as kaempferol 3-O-β-[(6'''-E-caffeoylglucopyranosyl)-(1-->3)-glucopyranoside]-7-O-β-glucopyranoside (1) by UV, 1H and 13C NMR spectroscopy, LC-MS, and acid and alkaline hydrolyses. Another flavonoid (2) was isolated from A. altajense, as a minor compound, together with 1 and identified as deacylated compound 1, i.e. kaempferol 3-O-laminaribioside-7-O-glucoside. They were found in nature for the first time.

  4. Genotoxicity evaluation of two kinds of smoke-water and 3,7-dimethyl-2H-furo[2,3-c]pyran-2-one

    Czech Academy of Sciences Publication Activity Database

    Trinh, C.; Gevaert, L.; Kohout, Ladislav; van Staden, J.; Verschaeve, L.

    2010-01-01

    Roč. 30, č. 6 (2010), s. 596-602 ISSN 0260-437X Institutional research plan: CEZ:AV0Z40550506 Keywords : butenolide * smoke -water * 3,7-dimethyl-2H-furo[2,3-c]pyran-2-one * assay * seed germination Subject RIV: CC - Organic Chemistry Impact factor: 2.322, year: 2010

  5. 1,8-Dihydroxy-2,4,5,7-tetranitro-9,10-anthraquinone

    Directory of Open Access Journals (Sweden)

    Mahsa Armaghan

    2010-05-01

    Full Text Available The ring system in the title compound, C14H4N4O12, is essentially planar (r.m.s. deviation of the carbon atoms = 0.085 Å; the two hydroxy groups form intramolecular hydrogen bonds to the same carbonyl O atom. The nitro groups are twisted with respect to the mean plane of the ring system by 74.3 (1 (1-nitro, 42.3 (3 (3-nitro, 45.7 (3 (6-nitro and 66.9 (1° (8-nitro.

  6. Expressions of B7-H4 and B7-H3 Proteins and Effect of Sorafenib on ...

    African Journals Online (AJOL)

    21. Pardoll DM. The blockage of immune checkpoints in cancer immunotherapy. Nat Rev Cancer 2012; 12(4):. 252-264. 22. Wang L, Liu LH, Shan BE. B7-H3: a promising target for tumor immunotherapy. Immunol J 2012; 28(8): 726-729. 23. Liu CZ, Yang KG, Cheng SS. B7-H4: a new negative regulator of T cell immunity.

  7. Crystal structure of (Z-ethyl 3-[2-(5-methyl-7-nitro-1H-indole-2-carbonylhydrazinylidene]butanoate

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    Amal Errossafi

    2015-09-01

    Full Text Available The reaction of 5-methyl-7-nitro-1H-indole-2-carbohydrazide with ethyl acetoacetate yielded the title molecule, C16H18N4O5, in which the indole ring is almost planar, with the greatest deviation from the mean plane being 0.006 (2 Å. The nine atoms of the indole ring are almost perpendicular to the mean plane through the ethyl acetate group, as indicated by the dihedral angle of 87.02 (4° between them. In the crystal, centrosymmetric supramolecular dimers are formed via N—H...O hydrogen bonds and eight-membered amide {...HNCO}2 synthons. These are consolidated into a three-dimensional architecture by C—H...O contacts, and by π–π interactions between six-membered rings [inter-centroid distance = 3.499 (2 Å].

  8. 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

  9. ANTIMICROBIAL ACTIVITY OF [1,2,4]TRIAZOLO[4,3-а]PYRAZIN-8(7H-ONE DERIVATIVES

    Directory of Open Access Journals (Sweden)

    Kulikovska K. Yu.

    2014-12-01

    Full Text Available Today the problem of microbial resistance to antibacterial agents becomes the global one. Antimicrobial drugs that are in the pharmaceutical market do not satisfy the needs of modern treatment regimens, particularly Hospitalacquired infections. Therefore, the search for new and effective means of this pharmacological group is an important task of medical chemistry. From the literature it is known that derivatives of [1,2,4]triazolo[4,3-a]pyrazine show a wide range of biological actions, including antimicrobial and fungicidal. This makes it relevant microbiological study of primary derivatives of [1,2,4]triazolo[4,3-a]pyrazine for identifying promising compounds of the series and then study it in biological experiment.Using the PASS C&T (Prediction Activity Spectra for Substances: Complex & Training program and based on published data, we have generated virtual library of derivatives of [1,2,4]triazolo[4,3-a]pyrazine. As a result, we have received 35 new synthetic compounds of 7 series that were not previously described in the literature. Materials and methods The research of antimicrobial and fungicidal activity of the synthesized compounds was carried out in the laboratory of antimicrobial agents GA "Mechnikov Institute of microbiology and immunology" under the leadership of PhD, senior scientist V.V.Kazmirchuka. The activity of the synthesized compounds were studied by conventional method of the two-fold serial dilutions in liquid and solid nutrient medium. For primary screening we have used a set of clinical and reference strains of microorganism: Escherichia coli ATCC 25922 (F-50, Staphylococcus aureus ATCC 25923 (F-49, Bacillus anthracoides ATCC 1312, Pseudomonas aeruginosa ATCC 27853, Candida albicans ATCC 885-653. As the reference preparations were chosen Palin - modern antimicrobial agent of class of fluoroquinolones, Nevigramon - nalidixic acid derivative and Fluconazole -38 Annals of Mechnikov Institute, N 4, 2014 www

  10. Hydrothermal synthesis and crystal structure of the Ni2(C4H4N2)(V4O12)(H2O)2 and Ni3(C4H4N2)3(V8O23) inorganic-organic hybrid compounds. Thermal, spectroscopic and magnetic studies of the hydrated phase

    International Nuclear Information System (INIS)

    Larrea, Edurne S.; Mesa, Jose L.; Pizarro, Jose L.; Arriortua, Maria I.; Rojo, Teofilo

    2007-01-01

    Ni 2 (C 4 H 4 N 2 )(V 4 O 12 )(H 2 O) 2 , 1, and Ni 3 (C 4 H 4 N 2 ) 3 (V 8 O 23 ), 2, have been synthesized using mild hydrothermal conditions at 170 deg. C under autogenous pressure. Both phases crystallize in the P-1 triclinic space group, with the unit-cell parameters, a=7.437(7), b=7.571(3), c=7.564(4) A, α=65.64(4), β=76.09(4), γ=86.25(3) o for 1 and a=8.566(2), b=9.117(2), c=12.619(3) A, α=71.05(2), β=83.48(4), γ=61.32(3) o for 2, being Z=2 for both compounds. The crystal structure of the three-dimensional 1 is constructed from layers linked between them through the pyrazine molecules. The sheets are formed by edge-shared [Ni 2 O 6 (H 2 O) 2 N 2 ] nickel(II) dimers octahedra and rings composed by four [V 4 O 12 ] vanadium(V) tetrahedra linked through vertices. The crystal structure of 2 is formed from vertex shared [VO 4 ] tetrahedra that give rise to twelve member rings. [NiO 4 (C 4 H 4 N 2 ) 2 ] ∞ chains, resulting from [NiO 4 N 2 ] octahedra and pyrazine molecules, give rise to a 3D skeleton when connecting to [VO 4 ] tetrahedra. Diffuse reflectance measurements of 1 indicate a slightly distorted octahedral geometry with values of Dq=880, B=980 and C=2700 cm -1 . Magnetic measurements of 1, carried out in the 5.0-300 K range, indicate the existence of antiferromagnetic couplings with a Neel temperature near to 38 K. - Graphical abstract: Crystal structure of a sheet of Ni 2 (C 4 H 4 N 2 )(V 4 O 12 )(H 2 O) 2

  11. Butane-1,4-diammonium bis(pyridine-2,6-dicarboxylato-κ3O2,N,O6cadmate(II dihydrate

    Directory of Open Access Journals (Sweden)

    Najmeh Firoozi

    2008-10-01

    Full Text Available In the title compound, (C4H14N2[Cd(C7H3NO42]·2H2O, the CdII ion is coordinated by four O atoms [Cd—O = 2.2399 (17–2.2493 (17 Å] and two N atoms [Cd—N = 2.3113 (15 and 2.3917 (15 Å] from two tridentate pyridine-2,6-dicarboxylato ligands in a distorted octahedral geometry. The uncoordinated water molecules are involved in O—H...O and N—H...O hydrogen bonds, which contribute to the formation of a three-dimensional supramolecular structure, along with π–π stacking interactions [centroid–centroid distances of 3.5313 (13 and 3.6028 (11 Å between the pyridine rings of neighbouring dianions].

  12. 1-[2-Oxo-1′-phenyl-2′,3′,5′,6′,7′,7a'-hexahydroindoline-3-spiro-3′-1′H-pyrrolizin-2′-yl]-3-phenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    S. Sriman Narayanan

    2008-09-01

    Full Text Available In the title compound, C29H26N2O2, one of the pyrrolidine rings in the pyrrolizine system is disordered, with site occupancies of ca 0.55 and 0.45. Both components of the disordered pyrrolidine ring adopt envelope conformations, whereas the other pyrrolidine ring adopts a twist conformation. The molecules are linked into centrosymmetric dimers by N—H...O hydrogen bonds and the dimers are connected via C—H...π interactions.

  13. Preparation of YBa2Cu3O7-δ powders by the thermal decomposition of a heteronuclear complex, CuY1/3Ba2/3(dhbaen)(NO3)1/3(H2O)3

    International Nuclear Information System (INIS)

    Hasegawa, E.; Aono, H.; Sadaoka, Y.; Traversa, E.

    1999-01-01

    YBa 2 Cu 3 O 7-δ powders were prepared by the thermal decomposition of a heteronuclear complex, CuY 1/3 Ba 2/3 (dhbaen)(NO 3 ) 1/3 (H 2 O) 3 . The products of the complex thermal decomposition were analyzed by TG-DTA, XRD, SEM-Auger and XPS. The decomposition of the CuY 1/3 Ba 2/3 -complex was obtained at about 500 C and the product was a mixture of oxides and carbonates. The formation of YBa 2 Cu 3 O 7-δ proceeded at 800 C, with a gradual decomposition of the carbonates. A homogeneous distribution of each element, Y, Ba, and Cu, was observed for the decomposed CuY 1/3 Ba 2/3 -complex by SEM-Auger analysis. The binding energy values of Ba3d 5/2 and O1s photolines from Ba and O in the superconductive lattice did not shift during the sputtering period. Furthermore, the formation of Ba rich regions on the surface was depressed by using the complex as a starting material for homogeneous 123-oxide, YBa 2 Cu 3 O 7-δ . (orig.)

  14. Second order magnetic phase transition and scaling analysis in iron doped manganite La0.7Ca0.3Mn1−xFexO3 compounds

    International Nuclear Information System (INIS)

    Ginting, Dianta; Nanto, Dwi; Denny, Yus Rama; Tarigan, Kontan; Hadi, Syamsul; Ihsan, Mohammad; Rhyee, Jong-Soo

    2015-01-01

    We investigated magnetic properties of La 0.7 Ca 0.3 Mn 1−x Fe x O 3 (x=0.09 and 0.11) compounds in terms of isothermal magnetization analysis and scaling behavior with various critical exponents. From the Landau theory of magnetic phase transition, we found that the paramagnetic to ferromagnetic phase transition in La 0.7 Ca 0.3 Mn 1−x Fe x O 3 (x=0.09 and 0.11) compounds is the type of second order magnetic transition (SOMT), which contrary to the first order magnetic transition (FOMT) for low Fe-doped compounds (x<0.09) in previous reports. When we investigate the critical behavior of the compounds near T=T c by the modified Arrott plot, Kouvel–Fisher plots, and critical isothermal analysis, the estimated critical exponents β, γ, and δ are in between the theoretically predicted values for three-dimensional Heisenberg and mean-field interaction models. It is noteworthy that the scaling relations are obeyed in terms of renormalization magnetization m=ε −β M(H,ε) and renormalized field h=|ε| β+γ H. Temperature-dependent effective exponents β eff and γ eff correspond to the ones of disordered ferromagnets. It is shown that the magnetic state of the compounds is not fully described by the conventional localized-spin interaction model because the ferromagnetic interaction has itinerant character by increasing Fe-doping concentration. - Highlights: • The ferromagnetic phase transition is of second order in La 0.7 Ca 0.3 Mn 1−x Fe x O 3 . • The critical exponents are in between the 3D Heisenberg and mean-field models. • The ferromagnetic interaction becomes more itinerant by Fe-doping

  15. Crystal structure of (1S,3R,8R,9R,10S-2,4,6-tris(2,2-dichloro-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodec-9-ylcyclotriboroxane

    Directory of Open Access Journals (Sweden)

    Ahmed Benharref

    2015-08-01

    Full Text Available The title compound, C48H75B3Cl6O3, was synthesized in two steps from β-himachalene (3,5,5,9-tetramethyl-2,4a,5,6,7,8-hexahydro-1H-benzocycloheptene, which was isolated from the essential oil of the Atlas cedar (Cedrus Atlantica. The molecule consists of an almost planar cyclotriboroxane ring [maximum deviation = 0.036 (2 Å] linked to three identical fused ring systems with different conformations. Each of the three attached ring systems is built up from a seven-membered ring to which a six- and a three-membered ring are fused. The three six-membered rings have a twist-boat conformation, whereas the seven-membered rings display boat, chair and twist-boat conformations. The dihedral angles between the central boroxane ring and the mean planes of the attached six-membered rings are 63.67 (18, 54.89 (2 and 56.57 (19°. The crystal packing is governed only by van der Waals interactions.

  16. C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings prepared from TiC_0_._7N_0_._3 powder using ball milling followed by oxidation

    International Nuclear Information System (INIS)

    Hao, Liang; Wang, Zhenwei; Zheng, Yaoqing; Li, Qianqian; Guan, Sujun; Zhao, Qian; Cheng, Lijun; Lu, Yun; Liu, Jizi

    2017-01-01

    Highlights: • TiO_2/TiC_0_._7N_0_._3 coatings were prepared by ball milling followed by oxidation. • In situ co-doping of C and N with simultaneous TiO_2 formation was observed. • Improved photocatalytic activity under UV/visible light was noticed. • Synergism in co-doping and heterojunction formation promoted carrier separation. - Abstract: Ball milling followed by heat oxidation was used to prepared C, N co-doped TiO_2 coatings on the surfaces of Al_2O_3 balls from TiC_0_._7N_0_._3 powder. The as-prepared coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible spectrophotometer (UV–vis). The results show that continuous TiC_0_._7N_0_._3 coatings were formed after ball milling. C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings were prepared after the direct oxidization of TiC_0_._7N_0_._3 coatings in the atmosphere. However, TiO_2 was hardly formed in the surface layer of TiC_0_._7N_0_._3 coatings within a depth less than 10 nm during the heat oxidation of TiC_0_._7N_0_._3 coatings in carbon powder. Meanwhile, the photocatalytic activity evaluation of these coatings was conducted under the irradiation of UV and visible light. All the coatings showed photocatalytic activity in the degradation of MB no matter under the irradiation of UV or visible light. The C, N co-doped TiO_2/TiC_0_._7N_0_._3 composite coatings showed the most excellent performance. The enhancement under visible light irradiation should attribute to the co-doping of carbon and nitrogen, which enhances the absorption of visible light. The improvement of photocatalytic activity under UV irradiation should attribute to the synergistic effect of C, N co-doping, the formation of rutile-anatase mixed phases and the TiO_2/TiC_0_._7N_0_._3 composite microstructure.

  17. 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.

  18. 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

    Directory of Open Access Journals (Sweden)

    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.

  19. No-carrier-added (NCA) synthesis of 6-[18F]fluoro-L-DOPA using 3,5,6,7,8,8a-hexahydro-7,7,8a-trimethyl-[6S-(6α, 8α, 8αβ)]-6,8-methano-2H-1,4-benzoxazin-2-one

    International Nuclear Information System (INIS)

    Horti, A.; Yale Univ., West Haven, CT; Redmond, D.E. Jr.; Soufer, R.

    1995-01-01

    3,5,6,7,8,8a-Hexahydro-7,7,8a-trimethyl-[6S-(6α,8α , 8αβ)]-6,8-methano-2H-1,4-benzoxazino-2-one (2) was investigated as chiral auxiliary for asymmetric NCA nucleophilic synthesis of 6-[ 18 F]Fluoro-L-DOPA. Direct condensation of 3,4-dimethoxy-2-[ 18 F]fluorobenzaldehyde (1a) or 6-[ 18 F]fluoro-piperonal (1b) in the presence of NaH with 2 gave the corresponding [ 18 F]-3-[(2-fluorophenyl)methylene]-3,5,6,7,8,8a-hexahydro-7,7,8 a-trimethyl-[6S-(3Z,3α,6α,8α,8αβ)]-6, 8-methano-2H-1,4-benzoxazin-2-one derivative 3a or 3b as a single stereoisomer. L-Selectride promoted hydrogenation of the olefinic double bond of these derivatives, in presence of tertbutyl alcohol, afforded the corresponding [ 18 F]-3-[(2-fluorophenyl) methyl]-3,5,6,7,8,8a-hexahydro-7,7,8a-trimethyl-[3S-(3α, 6α, 8α8αβ)]-6,8-methano-2H-1,4-benzoxazin-2-one derivatives (4a,b) without affecting the orientation of diasterofacial discrimination. Deprotection of the derivatives 4a,b yielded 6-[ 18 F]fluoro-L-DOPA (e.e. >90%, 3% radiochemical yield (EOB), total synthesis time 125 min, specific activity >2000 mCi/μmol). Direct deprotection/reduction of the compounds 3a,b provides the enantiomeric mixture of 6-[ 18 F]fluoro-D,L-DOPA (10-12% radiochemical yield) and, after chiral separation, 6-[ 18 F]fluoro-L-DOPA (e.e. 98%, 4-5% radiochemical yield). (author)

  20. Synthesis of (19E)-3 beta,7 alpha-dihydroxy-17-oxoandrost-5-en-19-al 19-(O-carboxymethyl)oxime, a new hapten for 7 alpha-hydroxydehydroepiandrosterone (3 beta,7 alpha-dihydroxyandrost-5-en-17-one).

    Science.gov (United States)

    Pouzar, V; Slavíková, T; Cerńy, I

    1998-09-01

    The title compound was prepared in 11 steps from 17,17-ethylenedioxy-19-hydroxyandrost-5-en-3 beta-yl acetate. After tert-butyldimethylsilyl protection of the 19-hydroxyl group, a 7-oxo group was introduced by oxidation with 3,5-dimethylpyrazole-chromium trioxide complex, and then selectively reduced with L-Selectride to give a 7 alpha-hydroxy derivative. This partially protected triol was acetylated and desilylated to 3,7-diacetate. Subsequent oxidation with pyridine-chromium trioxide complex gave 19-aldehyde, which was transformed into the corresponding protected 19-(O-carboxymethyl)oxime. Successive ketal cleavage, deacetylation, and methyl ester splitting gave the final (19E)-3 beta,7 alpha-dihydroxy-17-oxoandrost-5-en-19-al 19-(O-carboxymethyl)oxime, designed as a hapten for 7 alpha-hydroxydehydroepiandrosterone immunoassays.

  1. Synthesis and the crystal and molecular structures of 4-(piperidyl-1)-2-phenylpyrido[2,3-a]anthraquinone-7,12 Mono- and dibromohydrates (HL)Br . 3H2O and (H2L)Br2 . 3H2O

    International Nuclear Information System (INIS)

    Kovalchukova, O. V.; Stash, A. I.; Belsky, V. K.; Strashnova, S. B.; Zaitsev, B. E.; Ryabov, M. A.

    2009-01-01

    4-(Piperidyl-1)-2-phenylpyrido[2,3-a]anthraquinone-7,12 monobromohydrate (HL)Br . 3H 2 O (I) and 4-(piperidyl-1)-2-phenylpyrido[2,3-a]anthraquinone-7,12 dibromohydrate (H 2 L)Br 2 . 3H 2 O (II) are isolated in the crystalline state. The crystal structures of compounds I and II are determined using X-ray diffraction. It is established that the protonation of 4-(piperidyl-1)-2-phenylpyrido[2,3-a]anthraquinone-7,12 proceeds primarily through the pyridine atom at pH 2-3. The attachment of the second proton occurs through the piperidine nitrogen atom at pH ∼ 1.

  2. 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 Csp3H...Cl hydrogen bonds, H...S contacts and π–π stacking interactions between phenothiazine units.

  3. Actoprotective properties of 7'-((3-thio-4-methyl-4H-1,2,4-triazole-5-ylmethyltheophylline derivatives

    Directory of Open Access Journals (Sweden)

    A. S. Gotsulya

    2016-06-01

    Full Text Available The aim of this work was the study of actoprotective activity of compounds, which combine sintons of 1,2,4-triazole-3-thiol and theophylline. Materials and methods. The first time synthesized 7'-((3-thio-4-phenyl-4H-1,2,4-triazole-5-ylmethyltheophylline derivatives have been used for the research. The systemic toxicity and the acute toxicity of the studied compounds have been performed by the rapid method of Prozorovskiy to determine the optimal conditions for dispensing substances. Experiments have been conducted on a group of white nonlinear rats, 159–221 g weight. During the study of actoprotective activity the method of forced immersion in water with a load of 10% by weight of the rats has been used. The substances were administered at a dose 1/10 of LD50, and the reference drug «Riboxin» at a dose of 100 mg/kg. The swim time was recorded in seconds. The control group of animals was used for comparison; these animals received saline solution intraperitoneally 20 minutes before immersion. The obtained results were statistically processed using the standard software package of Microsoft Office 2007 and «STATISTICA@ for Windows 6.0». Results. According to the results of conducted researches it has been established that the most active compound among the studied was 7'-((5-(2-hydroxyethylthio-4-phenyl-4H-1,2,4-triazole-3-ylmethyltheophylline, which increased the duration of swimming by 14.31% comparing to control group, whereas the reference drug increased it by 20.57%. It has been established that 2-((5-((theophylline-7'-ylmethyl-4-phenyl-4H-1,2,4-triazol-3-ylthio-N'-(3,4-difluorobenzylideneacetohydrazide also increases the duration of swimming. Conclusion. The study of actoprotective activity of 13 first time synthesized compounds has been conducted. 7'-((5-(2-Hydroxyethylthio-4-phenyl-4H-1,2,4-triazole-3-ylmethyltheophylline has been detected as the most active compound among the studied ones.

  4. Kaempferol 3,7,4'-glycosides from the flowers of Clematis cultivars.

    Science.gov (United States)

    Sakaguchi, Keisuke; Kitajima, Junichi; Iwashina, Tsukasa

    2013-08-01

    A new kaempferol glycoside, kaempferol 3-O-alpha-rhamnopyranosyl-(1 --> 6)-beta-glucopyranoside-7,4'-di-O-beta-glucopyranoside (1) was isolated from the flowers of Clematis cultivars "Jackmanii Superba" and "Fujimusume", together with the known compound kaempferol 3,7,4'-tri-O-beta-glucopyranoside (2). The chemical structures of the isolated kaemferol glycosides were established by UV, 1H and 13C NMR spectroscopy, LC-MS, and characterization of acid hydrolysates.

  5. 2,3-Diamino?pyridinium 6-carb?oxy?pyridine-2-carboxyl?ate

    OpenAIRE

    Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein

    2011-01-01

    The asymmetric unit of the title proton-transfer compound, C5H8N3C7H4NO4−, consists of one mono-deprotonated pyridine-2,6-dicarboxylic acid as anion and one protonated 2,3-diaminopyridine as cation. The crystal packing shows extensive O—H...O, N—H...O and N—H...N hydrogen bonds. Thre are also several π–π interactions between the anions and also between the cations [centriod–centroid distances = 3.6634&...

  6. Expression of immunosuppresive B7-H3 ligand by hormone-treated prostate cancer tumors and metastases.

    Science.gov (United States)

    Chavin, Grant; Sheinin, Yuri; Crispen, Paul L; Boorjian, Stephen A; Roth, Timothy J; Rangel, Laureano; Blute, Michael L; Sebo, Thomas J; Tindall, Don J; Kwon, Eugene D; Karnes, R Jeffrey

    2009-03-15

    Prostate cancer cells uniformly express the immune cell inhibitory B7-H3 ligand. Enhanced B7-H3 expression correlates with increased disease progression and cancer-specific death after radical prostatectomy (RP). To further assess whether B7-H3 expression is hormone regulated and persists as a viable target during (or after) androgen-ablative therapy, we examined B7-H3 ligand expression within primary and metastatic cancer lesions in response to neoadjuvant hormone therapy (NHT) or palliative hormone deprivation. Tumor B7-H3 in RP specimens from men treated with >/=3 months of NHT was compared with B7-H3 in tumors from matched patients who received no therapy before RP. Hormone-treated and untreated metastatic lesions involving bone were also compared for levels of B7-H3 expression. Of 165 consecutive RP specimens in each cohort studied, sufficient tissues were available for 148 patients (89.7%) treated with NHT versus 127 patients (77.0%) treated with surgery alone. B7-H3 was expressed in 142 (95.9%) tumors from NHT patients compared with 122 (96.0%) tumors from patients treated with surgery alone (P = 0.91). B7-H3 expression intensity in RP specimens was not affected by NHT (P = 0.12). Bone metastases from 11 (32.4%) untreated and 23 (67.6%) androgen-ablated patients revealed that B7-H3 expression increased in response to hormone therapy (P = 0.04) relative to untreated lesions. Taken together, B7-H3 expression seems to remain stable (or may even increase) in response to hormone therapy. As such, B7-H3 may represent an attractive target to improve treatment of men with high-risk hormone-treated or refractory prostate cancer.

  7. (Diethyl ether{1-[2-(1-methyl-1H-imidazol-2-yl-κN3-1,1-diphenylethyl]-(1,2,3,3a,7a-η-indenyl}lithium(I

    Directory of Open Access Journals (Sweden)

    Maxim V. Borzov

    2009-05-01

    Full Text Available In the title compound, [Li(C27H23N2(C4H10O], the Li atom possesses a nearly planar trigonal coordination environment (assuming the cyclopentadienyl ring of the indenyl group occupies one coordination place. The diethyl ether ligand adopts a nearly planar W-type conformation.

  8. New alkali metal diphosphates how materials to preserve the security of the environment: CsNaCu(P2O7), Rb2Cu(P2O7) and CsNaCo(P2O7) synthesis and crystal structure determination

    Science.gov (United States)

    Chernyatieva, Anastasiya; Filatova, Alyona; Spiridonova, Dariya; Krivovichev, Sergey

    2013-04-01

    In this work we describe preliminary results of the synthesis and of a crystal-chemical study of synthetic phosphates with transition metals. Due to the increasing requirements for environmental safety specialists from various industries, we are searching for sustainable forms of immobilization of hazardous waste during storage. We are also developing a component-based waste for new materials. In our continued exploratory synthesis of compounds containing transition-metals, we were able to produce the new diphosphate phases CsNaCu(P2O7), Rb2Cu(P2O7) and CsNaCo(P2O7). A crystal chemical study has allowed us to identify new phosphates. Crystals of CsNaCu(P2O7) (Phase 1) is orthorhombic, crystallizes in space group Pmn21, with a = 5.147(8), b = 15.126(2), c = 9.717(2) Å, V = 756.20 Å3, R1 = 0.066 and Rb2Cu(P2O7) (Phase 2) is orthorhombic as well, crystallizes in space group Pmcn, with a = 5.183(8), b = 10.096(1), c = 15.146(3) Å, V = 793.55 Å3, R1 = 0.063, they have been obtained by high-temperature reaction of RbNO3, CsNO3, Cu(NO3)2, NaOH and (NH4)4P2O7. Synthetic crystals of the phosphate of copper and rubidium were studied in detail by us on the structures of Rb2Cu(P2O7) and Rb2Cu3(P2O7)2 - new alkali metal copper diphosphates (CHERNYATIEVA et al., 2008). Here we report the synthesis, the structure and the properties of the title compounds and we compare these phases with the previously discovered K2CuP2O7 (ELMAADI et al., 1995) and CsNaMnP2O7 (HUANG et al., 1998). These structures crystallize in other space groups, although their structures are also based on 2-D layers, formed by P2O7 groups combined with polyhedra of the transition metals (CHERNYATIEVA et al., 2012). A crystal chemical study has allowed us to identify even new diphosphates CsNaCu(P2O7) (Phase 3). Crystals of CsNaCoP2O7 is monoclinic, space group P 21/n, with a = 7,424(2), b = 7,648(1), c = 12,931(3)Å, β = 90,71(2)° , V = 734.2(3) Å3 and R1 = 0.060. The structure is based framework of Co

  9. 2-Phenyl-7-(4-pyridylmethylamino-1,2,4-triazolo[1,5-a][1,3,5]triazin-5(4H-oneFused heterocyclic systems with s-triazine ring. Part 17. For part 16, see Dolzhenko et al. (2011.

    Directory of Open Access Journals (Sweden)

    Lip Lin Koh

    2011-01-01

    Full Text Available In the title compound, C16H13N7O, the 1,2,4-triazolo[1,5-a][1,3,5]triazine heterocyclic system is essentially planar (r.m.s. deviation = 0.0375 Å. The attached benzene ring lies almost in the mean plane of 1,2,4-triazolo[1,5-a][1,3,5]triazine [dihedral angle = 1.36 (23°], while the pyridine ring is turned out of this plane by the aminomethyl bridge [dihedral angle = 69.22 (9°]. The amino group H atom is involved in intramolecular hydrogen bonding with a triazole N atom. In the crystal, molecules are connected via C(=ONH...N hydrogen bonds into C(11 chains parallel to [100]. The amino group H atom acts as a hydrogen-bond donor, forming an NH...O=C hydrogen bond with the carbonyl O atom, which links the molecules into C(6 chains running along [011] and [01overline{1}].

  10. Novel series of potent, nonsteroidal, selective androgen receptor modulators based on 7H-[1,4]oxazino[3,2-g]quinolin-7-ones.

    Science.gov (United States)

    Higuchi, Robert I; Arienti, Kristen L; López, Francisco J; Mani, Neelakhanda S; Mais, Dale E; Caferro, Thomas R; Long, Yun Oliver; Jones, Todd K; Edwards, James P; Zhi, Lin; Schrader, William T; Negro-Vilar, Andrés; Marschke, Keith B

    2007-05-17

    Recent interest in orally available androgens has fueled the search for new androgens for use in hormone replacement therapy and as anabolic agents. In pursuit of this, we have discovered a series of novel androgen receptor modulators derived from 7H-[1,4]oxazino[3,2-g]quinolin-7-ones. These compounds were synthesized and evaluated in competitive binding assays and an androgen receptor transcriptional activation assay. A number of compounds from the series demonstrated single-digit nanomolar agonist activity in vitro. In addition, lead compound (R)-16e was orally active in established rodent models that measure androgenic and anabolic properties of these agents. In this assay, (R)-16e demonstrated full efficacy in muscle and only partially stimulated the prostate at 100 mg/kg. These data suggest that these compounds may be utilized as selective androgen receptor modulators or SARMs. This series represents a novel class of compounds for use in androgen replacement therapy.

  11. Yb5Ni4Sn10 and Yb7Ni4Sn13: New polar intermetallics with 3D framework structures

    International Nuclear Information System (INIS)

    Lei Xiaowu; Sun Zhongming; Li Longhua; Zhong Guohua; Hu Chunli; Mao Jianggao

    2010-01-01

    The title compounds have been obtained by solid state reactions of the corresponding pure elements at high temperature, and structurally characterized by single-crystal X-ray diffraction studies. Yb 5 Ni 4 Sn 10 adopts the Sc 5 Co 4 Si 10 structure type and crystallizes in the tetragonal space group P4/mbm (No. 127) with cell parameters of a=13.785(4) A, c=4.492 (2) A, V=853.7(5) A 3 , and Z=2. Yb 7 Ni 4 Sn 13 is isostructural with Yb 7 Co 4 InGe 12 and crystallizes in the tetragonal space group P4/m (No. 83) with cell parameters of a=11.1429(6) A, c=4.5318(4) A, V=562.69(7) A 3 , and Z=1. Both structures feature three-dimensional (3D) frameworks based on three different types of one-dimensional (1D) channels, which are occupied by the Yb atoms. Electronic structure calculations based on density functional theory (DFT) indicate that both compounds are metallic. These results are in agreement with those from temperature-dependent resistivity and magnetic susceptibility measurements. - Graphical abstract: Two new ytterbium nickel stannides, namely, Yb 5 Ni 4 Sn 10 and Yb 7 Ni 4 Sn 13 , have been synthesized and structurally characterized by single-crystal X-ray diffraction studies. Both their structures feature three-dimensional (3D) frameworks based on three different types of one-dimensional (1D) channels, which are situated by all the Yb atoms. Electronic structure calculations based on density functional theory (DFT) indicate that both compounds are metallic, which are in accordance with the results from temperature-dependent resistivity and magnetic susceptibility measurements.

  12. 4-(2,4-Dichlorophenyl-2-(1H-indol-3-yl-6-methoxypyridine-3,5-dicarbonitrile

    Directory of Open Access Journals (Sweden)

    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.

  13. 3-Aminobenzoic acid–4,4′-bipyridine (2/3

    Directory of Open Access Journals (Sweden)

    Pornsuda Lhengwan

    2012-08-01

    Full Text Available The asymmetric unit of the title compound, 3C10H8N2·2C7H7NO2, consists of three molecules of 4,4′-bipyridine (bpy and two molecules of 3-aminobenzoic acid (bza. Two molecules of bza and two molecules of bpy are connected via O—H...N, N—H...N and N—H...O hydrogen bonds, forming forming infinite double-stranded zigzag chains along the c axis. The third molecule of bpy is linked to the chain by weak C—H...O interactions. Adjacent chains are linked via π–π interactions [centroid–centroid distances = 3.759 (33.928 (3 Å] involving the pyridine rings of bpy molecules, resulting in a sheet-like structure parallel to (100. These sheets are stacked via C—H...π interactions, resulting finally in the formation of a three-dimensional supramolecular structure.

  14. Synthesis of the water soluble ligands dmPTA and dmoPTA and the complex [RuClCp(HdmoPTA)(PPh(3))](OSO(2)CF(3)) (dmPTA = N,N'-Dimethyl-1,3,5-triaza-7-phosphaadamantane, dmoPTA = 3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane, HdmoPTA = 3,7-H-3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane).

    Science.gov (United States)

    Mena-Cruz, Adrian; Lorenzo-Luis, Pablo; Romerosa, Antonio; Saoud, Mustapha; Serrano-Ruiz, Manuel

    2007-07-23

    The new water-soluble ligand dmPTA(OSO(2)CF(3))(2) (1) (dmPTA = N,N'-dimethyl-1,3,5-triaza-7-phosphaadamantane) has been synthesized by reaction of PTA with MeOSO(2)CF(3) in acetone (PTA = 1,3,5-triaza-7-phosphatricycle[3.3.1.1(3,7)]decane). The reaction of 1 with KOH gave rise to the new water-soluble ligand dmoPTA (3) (dmoPTA = 3,7-dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane) by elimination of the -CH(2)- group located between both NCH(3) units. Compound dmPTA(BF(4))(2) (2) and complex [RuClCp(HdmoPTA)(PPh(3))](OSO(2)CF(3)) (4) have also been synthesized, while compounds HdmoPTA(BF(4)) (3a) and [RuClCp(dmPTA)(PPh(3))](OSO(2)CF(3)) (5) were characterized but not isolated. The new ligands and the complex have been fully characterized by NMR, IR, elemental analysis, and X-ray crystal structure determination (ligand 1 and complex 4). The synthetic processes for 3 and 4 were studied.

  15. (E)-Methyl 3-(3,4-dimeth­oxy­phen­yl)-2-[(1,3-dioxoisoindolin-2-yl)meth­yl]acrylate

    OpenAIRE

    Kannan, D.; Bakthadoss, M.; Lakshmanan, D.; Murugavel, S.

    2012-01-01

    In the title compound, C21H19NO6, the isoindole ring system is essentially planar [maximum deviation = 0.019 (2) Å for the N atom] and is oriented at a dihedral angle of 51.3 (1)° with respect to the benzene ring. The two methoxy groups are almost coplanar with the attached benzene ring [C—O—C—C = 3.7 (4) and 4.3 (4)°]. The molecular conformation is stabilized by an intramolecular C&...

  16. 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.

  17. Crystal structure of 4-(4b,8a-dihydro-9H-pyrido[3,4-b]indol-1-yl-7-methyl-2H-chromen-2-one

    Directory of Open Access Journals (Sweden)

    S. Samundeeswari

    2017-01-01

    Full Text Available The title compound, C21H14N2O2, was prepared by Pictet–Spengler cyclization of tryptamine and 4-formyl coumarin. In the molecule, the dihedral angle between the mean planes of the coumarin and β-carboline ring systems is 63.8 (2°. In the crystal, molecules are linked via N—H...N hydrogen bonds, forming chains along the b-axis direction. Within the chains, there are a number of offset π–π interactions present [shortest intercentroid distance = 3.457 (2 Å].

  18. The Phenolic Compound from Kalanchoe blossfeldiana (Crassulaceae Leaf and Its Antiplasmodial Activity against Plasmodium falciparum 3D7

    Directory of Open Access Journals (Sweden)

    Yenny Febriani Yun

    2016-08-01

    Full Text Available Various species of Kalanchoe plants have been widely used as raw materials in traditional medicines. This study was the continuation of the researches on secondary metabolites from Indonesia Kalanchoe plants, focused on Kalanchoe blossfeldiana. Fresh K. blossfeldiana leaf was extracted with methanol at room temperature to obtain the concentrated extract. The concentrated methanol extract was dissolved in water and then partitioned successively with n-hexane and ethyl acetate. The methanol, n-hexane, ethyl acetate extracts were tested using antiplasmodial assay against Plasmodium falciparum 3D7. The IC50 of methanol, n-hexane, and ethyl acetate extract were 13.002; 2.807, and 11 nM, respectively. Ethyl acetate extract was separated by the combination of chromatography on silica and ODS. This process produced the yellow solid. The chemical structure of the compound was determined based on UV, IR, MS, 1H-NMR, and 13C-NMR analyses and the comparison of data obtained from the literature and identified as phenolic compound, namely 3,3',4',5,7-pentahydroxyflavone or quercetin (1, and displayed antiplasmodial activity with IC50 3.97x10-2 nM.

  19. Synthesized of 2,7 dihydroxyxanthone from xanthone and antimalarial activities

    Science.gov (United States)

    Amanatie; Jumina; Mustofa; Hanafi

    2018-03-01

    The purpose of the research is to synthesize 2,7-di-hydroxyxanthone compounds from xanthone and to evaluate antiplasmodial against activities. The synthesize of 2,7-di-hydroxyxanthone compounds worked with chromatogramphy methods including Thin Layer Chromatography (TLC), Vacuum Liquid Chromatography (VLC). A compound structures were determined based on the spectroscopic evidences including, Infrared (IR), one dimension (1-D) and two dimension (2-D) Nuclear Magnetic Resonance (NMR) spectra and comparison the spectroscopy data with related data from references. The biological properties of compounds are evaluated towards antiplasmodial against activity. The result of the product was obtained as white solid in 63.49% yield. The IR spectrum showed the absorption at 3433 cm-1 Which was reinforced with a sharp attack at 1087cm-1 indicating the stretching of OH, while the stretching of aromatic C=C appeared at 1620 cm-1. The 1H-NMR (500MHz, and DMSO –d6) spectrum showed that the aryl protons appeared in the region of δ12.98 ppm. In this region, there were 2 singlet at δH 12.98 ppm (1H, 2-OH) and (1H,7-OH) and shows the presence of two OH groups. Based on spectroscopy analyses, it could be started that the reaction of 2.7 di-aminoxanthone with NaNO2/HCl and H3PO4 produced 2.7-di-hydroxyxanthone. In vitro antiplasmodial assay of the product synthesized 2,7 di-hydroxyxanthones against. Falciparum strain of 3D7 showed that the IC50 values of 2,7-di-hydroxy xanthone, were 0.31 μg/mL, respectively.

  20. No-carrier-added (NCA) synthesis of 6-[{sup 18}F]fluoro-L-DOPA using 3,5,6,7,8,8a-hexahydro-7,7,8a-trimethyl-[6S-(6{alpha}, 8{alpha}, 8{alpha}{beta})]-6,8-methano-2H-1,4-benzoxazin-2-one

    Energy Technology Data Exchange (ETDEWEB)

    Horti, A. [Yale Univ., New Haven, CT (United States). School of Medicine]|[Yale Univ., West Haven, CT (United States). PET Center; Redmond, D.E. Jr. [Yale Univ., New Haven, CT (United States). School of Medicine; Soufer, R. [Yale Univ., West Haven, CT (United States). PET Center

    1995-12-31

    3,5,6,7,8,8a-Hexahydro-7,7,8a-trimethyl-[6S-(6{alpha},8{alpha} , 8{alpha}{beta})]-6,8-methano-2H-1,4-benzoxazino-2-one (2) was investigated as chiral auxiliary for asymmetric NCA nucleophilic synthesis of 6-[{sup 18}F]Fluoro-L-DOPA. Direct condensation of 3,4-dimethoxy-2-[{sup 18}F]fluorobenzaldehyde (1a) or 6-[{sup 18}F]fluoro-piperonal (1b) in the presence of NaH with 2 gave the corresponding [{sup 18}F]-3-[(2-fluorophenyl)methylene]-3,5,6,7,8,8a-hexahydro-7,7,8 a-trimethyl-[6S-(3Z,3{alpha},6{alpha},8{alpha},8{alpha}{beta})]-6, 8-methano-2H-1,4-benzoxazin-2-one derivative 3a or 3b as a single stereoisomer. L-Selectride promoted hydrogenation of the olefinic double bond of these derivatives, in presence of tertbutyl alcohol, afforded the corresponding [{sup 18}F]-3-[(2-fluorophenyl) methyl]-3,5,6,7,8,8a-hexahydro-7,7,8a-trimethyl-[3S-(3{alpha}, 6{alpha}, 8{alpha}8{alpha}{beta})]-6,8-methano-2H-1,4-benzoxazin-2-one derivatives (4a,b) without affecting the orientation of diasterofacial discrimination. Deprotection of the derivatives 4a,b yielded 6-[{sup 18}F]fluoro-L-DOPA (e.e. >90%, 3% radiochemical yield (EOB), total synthesis time 125 min, specific activity >2000 mCi/{mu}mol). Direct deprotection/reduction of the compounds 3a,b provides the enantiomeric mixture of 6-[{sup 18}F]fluoro-D,L-DOPA (10-12% radiochemical yield) and, after chiral separation, 6-[{sup 18}F]fluoro-L-DOPA (e.e. 98%, 4-5% radiochemical yield). (author).

  1. Synthesis of Novel Heterocyclic Compounds Incorporate 4,5,6,7-Tetrahydrobenzo[b]thiophene Together with Their Cytotoxic Evaluations.

    Science.gov (United States)

    Abdallah, Amira Elsayed Mahmoud; Mohareb, Rafat Milad; Khalil, Eid Metwally; Elshamy, Menna Alla Mohamed Abd Elaleem

    2017-01-01

    The 2-amino-3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophene was the key starting compound used to synthesize new thiazole, pyrimidine, pyran, pyridine and thiazine derivatives. The cytotoxicity of the synthesized compounds was studied towards the three cancer cell lines namely MCF-7 (breast adenocarcinoma), NCI-H460 (non-small cell lung cancer) and SF-268 (central nervous system (CNS) cancer) in addition to the normal cell line (WI-38) using doxorubicin as the reference drug. The study showed that compounds 5, 9a, 15b, 17c, 18 and 21b were the most potent compounds.

  2. 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.

  3. Structuring effects of [Ln6O(OH)8(NO3)6(H2O)12]2+ entities

    International Nuclear Information System (INIS)

    Guillou, O.; Daiguebonne, C.; Calvez, G.; Le Dret, F.; Car, P.-E.

    2008-01-01

    In order to obtain highly porous lanthanide-based coordination polymers we are currently investigating reactions between [Ln 6 O(OH) 8 (NO 3 ) 6 (H 2 O) 12 ] 2+ di-cationic hexanuclear entities and sodium salts of benzene-poly-carboxylic acids. Two new coordination polymers obtained during this study are reported here. In both cases, the hexanuclear entity has been destroyed during the reaction. However the resulting compounds are original thanks to a structuring effect of the poly-metallic complex. The first compound of chemical formula [Y 2 (C 8 H 4 O 4 ) 3 (DMF)(H 2 O)],2DMF crystallizes in the monoclinic system, space group P121/n (n o 14) with a = 16.0975(3) A, b = 14.4605(3) A, c = 17.7197(4) A, β = 92.8504(9) o and Z = 4. The second compound of chemical formula Y 2 (NO 3 ) 2 (C 10 H 2 O 8 )(DMF) 4 crystallizes in the triclinic system, space group P-1 (n o 2) with a = 7.5312(3) A, b = 9.0288(3) A, c = 13.1144(6) A, α = 92.6008(14) o , β = 94.9180(14) o , γ = 112.1824(16) o and Z = 2. Both crystal structures are 2D. Both crystal structures are described and the original structural features are highlighted and related to a potential structuring effect of the hexanuclear precursor

  4. (1R,3S,8R-3,7,7,10-Tetramethyltricyclo[6.4.0.01,3]dodec-9-en-11-one

    Directory of Open Access Journals (Sweden)

    Abdoullah Bimoussa

    2014-01-01

    Full Text Available The absolute configuration of the title compound, C16H24O, has been deduced from the chemical pathway. The six-membered ring has a roughly half-chair conformation with the quaternary C atom as the flap. The seven-membered ring displays a chair conformation. In the crystal, there is a weak C—H...O hydrogen bond between the methylene group of the cyclopropane ring and the carbonyl group of a screw-axis-related molecule, which builds up a zigzag-like chain along the b-axis direction.

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

    Directory of Open Access Journals (Sweden)

    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.

  6. 10-{4-[(2-Hydroxybenzylideneamino]phenyl}-5,5-difluoro-1,3,7,9-tetramethyl-5H-dipyrrolo[1,2-c:2′,1′-f][1,3,2]diazaborinin-4-ium-5-uide

    Directory of Open Access Journals (Sweden)

    Zhensheng Li

    2013-07-01

    Full Text Available The title compound, C26H24BF2N3O, comprises a boron–dipyrromethene (BODIPY framework and a phenolic Schiff base substituent group. The BODIPY unit is close to planar [maximum deviation from the least-squares plane = 0.040 (3 Å], and forms a dihedral angle of 80.38 (13° with the meso-substituent phenyl ring and an angle of 56.57 (13° with the phenolic ring in the extended substituent chain. An intramolecular O—H...N hydrogen bond is formed between the phenolic hydroxyl group and the Schiff base N-atom. The crystal studied was a non-merohedral twin with a BASF factor of 0.447 (3 for the two components.

  7. Heterocycles [h]-Fused Onto 4-Oxoquinoline-3-Carboxylic Acid, Part VIII [1]. Convenient Synthesis and Antimicrobial Properties of Substituted Hexahydro[1,4]diazepino[2,3-h]quinoline-9-carboxylic acid and Its Tetrahydroquino[7,8-b]benzodiazepine Analog

    Directory of Open Access Journals (Sweden)

    Yusuf M. Al-Hiari

    2008-11-01

    Full Text Available [1,4]Diazepino[2,3-h]quinolone carboxylic acid 3 and its benzo-homolog tetrahydroquino[7,8-b]benzodiazepine-3-carboxylic acid 5 were prepared via PPAcatalyzed thermal lactamization of the respective 8-amino-7-substituted-1,4-dihydroquinoline-3-carboxylic acid derivatives 8, 10. The latter compounds were obtained by reduction of their 8-nitro-7-substituted-1,4-dihydroquinoline-3-carboxylic acid precursors 7, 9 which, in turn, were prepared by reaction of 7-chloro-1-cyclopropyl-6-fluoro-8-nitro-1,4-dihydroquinoline-3-carboxylic acid (6 with each of β-alanine and anthranilic acid. All intermediates and target compounds were characterized using elemental analysis, NMR, IR and MS spectral data. The prepared targets and the intermediates have shown interesting antibacterial activity mainly against Gram positive strains. In particular, compound 8 showed good activity against S. aureus (MIC = 0.39 μg/mL and B. subtilis (MIC = 0.78 μg/mL. Compounds 5a and 9 have also displayed good antifungal activity against C. albicans (MIC = 1.56 μg/mL and 0.78 μg/mL, respectively. None of the compounds tested showed any anticancer activity against solid breast cancer cell line MCF-7 cells or a human breast adenocarcinoma cell line.

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

    Directory of Open Access Journals (Sweden)

    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.

  9. Supra-molecular hydrogen-bonding patterns in the N(9)-H protonated and N(7)-H tautomeric form of an N(6) -benzoyl-adenine salt: N (6)-benzoyl-adeninium nitrate.

    Science.gov (United States)

    Karthikeyan, Ammasai; Jeeva Jasmine, Nithianantham; Thomas Muthiah, Packianathan; Perdih, Franc

    2016-02-01

    In the title molecular salt, C12H10N5O(+)·NO3 (-), the adenine unit has an N (9)-protonated N(7)-H tautomeric form with non-protonated N(1) and N(3) atoms. The dihedral angle between the adenine ring system and the phenyl ring is 51.10 (10)°. The typical intra-molecular N(7)-H⋯O hydrogen bond with an S(7) graph-set motif is also present. The benzoyl-adeninium cations also form base pairs through N-H⋯O and C-H⋯N hydrogen bonds involving the Watson-Crick face of the adenine ring and the C and O atoms of the benzoyl ring of an adjacent cation, forming a supra-molecular ribbon with R 2 (2)(9) rings. Benzoyl-adeninum cations are also bridged by one of the oxygen atoms of the nitrate anion, which acts as a double acceptor, forming a pair of N-H⋯O hydrogen bonds to generate a second ribbon motif. These ribbons together with π-π stacking inter-actions between the phenyl ring and the five- and six-membered adenine rings of adjacent mol-ecules generate a three-dimensional supra-molecular architecture.

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

    Directory of Open Access Journals (Sweden)

    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.

  11. X-ray and NQR studies of bromoindate(III) complexes. [C{sub 2}H{sub 5}NH{sub 3}]{sub 4}InBr{sub 7}, [C(NH{sub 2}){sub 3}]{sub 3}InBr{sub 6}, and [H{sub 3}NCH{sub 2}C(CH{sub 3}){sub 2}CH{sub 2}NH{sub 3}]InBr{sub 5}

    Energy Technology Data Exchange (ETDEWEB)

    Iwakiri, Takeharu; Ishihara, Hideta [Saga Univ. (Japan). Faculty of Culture and Education; Terao, Hiromitsu [Tokushima Univ. (Japan). Faculty of Integrated Arts and Sciences; Lork, Enno; Gesing, Thorsten M. [Bremen Univ. (Germany). Inst. of Inorganic Chemistry and Crystallography

    2017-03-01

    The crystal structures of [C{sub 2}H{sub 5}NH{sub 3}]{sub 4}InBr{sub 7}(1), [C(NH{sub 2}){sub 3}]{sub 3}InBr{sub 6}(2), and [H{sub 3}NCH{sub 2}C(CH{sub 3}){sub 2}CH{sub 2}NH{sub 3}]InBr{sub 5}(3) were determined at 100(2) K: monoclinic, P2{sub 1}/n, a=1061.94(3), b=1186.40(4), c=2007.88(7) pm, β= 104.575(1) , Z=4 for 1; monoclinic, C2/c, a=3128.81(12), b=878.42(3), c=2816.50(10) pm, β=92.1320(10) , Z=16 for 2; orthorhombic, P2{sub 1}2{sub 1}2{sub 1}, a=1250.33(5), b=1391.46(6), c=2503.22(9) pm, Z=4 for 3. The structure of 1 contains an isolated octahedral [InBr{sub 6}]{sup 3-} ion and a Br{sup -} ion. The structure of 2 contains three different isolated octahedral [InBr{sub 6}]{sup 3-} ions. The structure of 3 has a corner-shared double-octahedral [In{sub 2}Br{sub 11}]{sup 5-} ion and an isolated tetrahedral [InBr{sub 4}]{sup -} ion. The {sup 81}Br nuclear quadrupole resonance (NQR) lines of the terminal Br atoms of the compounds are widely spread in frequency, and some of them show unusual positive temperature dependence. These observations manifest the N-H..Br-In hydrogen bond networks developed between the cations and anions to stabilize the crystal structures. The {sup 81}Br NQR and differential thermal analysis (DTA) measurements have revealed the occurrence of unique phase transitions in 1 and 3. When the bond angles were estimated from the electric field gradient (EFG) directions calculated by the molecular orbital (MO) methods, accurate values were obtained for [InBr{sub 6}]{sup 3-} of 1 and for [In{sub 2}Br{sub 11}]{sup 5-} and [InBr{sub 4}]{sup -} of 3, except for several exceptions in those for the latter two ions. On the other hand, the calculations of {sup 81}Br NQR frequencies have produced up to 1.4 times higher values than the observed ones.

  12. 1-[(6-Chloro-3-pyridylmethyl]-N-(4-ethoxyphenyl-3-phenyl-1H-pyrazole-5-carboxamide

    Directory of Open Access Journals (Sweden)

    Zheng Tang

    2009-04-01

    Full Text Available In the title compound, C24H21ClN4O2, the pyrazole ring makes dihedral angles of 7.70 (11, 89.17 (11 and 40.68 (11° with the phenyl, pyridine and ethoxyphenyl rings, respectively. There are some intramolecular C—H...O and C—H...π bonds giving rigidity to the molecule, while weak intermolecular N—H...N and C—H...π hydrogen bonds link the molecules into a two-dimensional structure.

  13. Theoretical study on the mechanism of the reaction of FOX-7 with OH and NO2 radicals: bimolecular reactions with low barrier during the decomposition of FOX-7

    Science.gov (United States)

    Zhang, Ji-Dong; Zhang, Li-Li

    2017-12-01

    The decomposition of 1,1-diamino-2,2-dinitroethene (FOX-7) attracts great interests, while the studies on bimolecular reactions during the decomposition of FOX-7 are scarce. This study for the first time investigated the bimolecular reactions of OH and NO2 radicals, which are pyrolysis products of ammonium perchlorate (an efficient oxidant usually used in solid propellant), with FOX-7 by computational chemistry methods. The molecular geometries and energies were calculated using the (U)B3LYP/6-31++G(d,p) method. The rate constants of the reactions were calculated by canonical variational transition state theory. We found three mechanisms (H-abstraction, OH addition to C and N atom) for the reaction of OH + FOX-7 and two mechanisms (O abstraction and H abstraction) for the reaction of NO2 + FOX-7. OH radical can abstract H atom or add to C atom of FOX-7 with barriers near to zero, which means OH radical can effectively degrade FOX-7. The O abstraction channel of the reaction of NO2 + FOX-7 results in the formation of NO3 radical, which has never been detected experimentally during the decomposition of FOX-7.

  14. 6-Methoxy-1-(4-methoxyphenyl-1,2,3,4-tetrahydro-9H-β-carbolin-2-ium acetate

    Directory of Open Access Journals (Sweden)

    Mohd Mustaqim Rosli

    2012-05-01

    Full Text Available In the title compound, C19H21N2O2+·C2H3O2−, the 1H-indole ring system is essentially planar [maximum deviation = 0.0257 (14 Å] and forms a dihedral angle of 87.92 (7 Å with the benzene ring attached to the tetrahydropyridinium fragment. The tetrahydropyridinium ring adopts a half-chair conformation. In the crystal, cations and anions are linked by interionic N—H...O, C—H...O and C—H...N hydrogen bonds into chains along the a axis.

  15. Synthesis and investigation of the physicochemical properties of 2-(5-((theophylline-7'-ylmethyl-4-phenyl-4H-1,2,4-triazole-3-ylthio-acetic acid salts

    Directory of Open Access Journals (Sweden)

    A. S. Gotsulya

    2014-02-01

    spectrometer “Mercury 400” (solvent - DMSO-d6 or DMSO-d6 + CCl4, the internal standard - tetramethylsilane. Chromatography-mass spectral researches were performed on the instrument Agilent 1100 Series LC/MSD System, method of ionization - chemical ionization at the atmospheric pressure (APCI. Propyl ester of the theophylline-7-acetic acid. To the 0,055 mol of sodium hydrogencarbonate in 150 ml of DMF adds 0,05 mole of the theophylline and heated with stirring 5 - 10 minutes. To the reaction compound adds 0,055 mole of the monochloracetate acid propyl ester and boil with constant stirring 5 - 6 hours. After cooling to the reaction mixture with stirring, adds an equal volume of water. The precipitate dissolves, then falles again. Ester precipitate is filtered, washed with water, then with a small amount of methanol and dried. White crystalline solid, insoluble in water, soluble in organic solvents (alcohols, dioxane, DMF, DMSO. For the analysis is purified from 1-propanol. Yield 82%. Hydrazide of the theophylline -7-acetic acid. To the heated 0,03 mole solution of the propyl ester theophylline -7- acetic acid in 200 ml of ethanol adds 0.3 mole of hydrazine hydrate. Reactionary compound leave at room temperature for 12 hours. Hydrazide precipitate is filtered, washed with water, acetone and dried. Output 79%. White, amorphous substance, insoluble in water, acetone, soluble in alcohols, dioxane, soluble in DMF, DMSO. Crystallized from a mixture DMF-water (1:1. Tm. = 210-211 ºC. 2-(2-(theophylline-7'-ylacetyl-N-phenylhydrazinecarbothioamide. 0,05 mol of phenylisothiocyanate, 130 ml of dioxane and 90 ml of water heated up to boiling for 1 hour, cooled, add 100 ml of water, the precipitate is filtered, washed with water, 2-propanol and crystallized from a mixture water- dioxane, dimethylformamide. Output - 71 %. Tm . = 262-265 ºC. 7-((5-mercapto-4-phenyl-4H-1,2,4-triazoles-3-ylmethyltheophylline. 0,01 mol of compound 2 -(2-(theophyllineacetyl-N-phenylhydrazyncarbothio-amide, 0

  16. Synthesis and characterization of a Ruddlesden-Popper compound: Sr3FeMoO7

    International Nuclear Information System (INIS)

    Li Zhaofei; Li Guobao; Sun Junliang; You Liping; Loong, Chun-K.; Wang Yingxia; Liao Fuhui; Lin Jianhua

    2005-01-01

    A powder sample of Sr 3 FeMoO 7 was synthesized by solid-state reaction in reduced atmosphere (5% H 2 /Ar). At room temperature, Sr 3 FeMoO 7 crystallizes in a typical Ruddlesden-Popper (n=2) structure in the space group I4/mmm, a=3.9309(2)A and c=20.435(2)A. The structure refinement indicates that the Fe and Mo ions are randomly distributed in a single B-site with small fraction of B-site and oxygen vacancies. At low temperature, long-range magnetic interaction was observed. The antiferromagnetic magnetic interaction can be described with a large unit cell, a m =b m =2a n and c m =c n , in the magnetic space group An'

  17. 2,2′-[(3aRS,7aRS-Perhydrobenzimidazole-1,3-diylbis(methylene]diphenol

    Directory of Open Access Journals (Sweden)

    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.

  18. Crystal structure, thermochromic and magnetic properties of organic-inorganic hybrid compound: (C7H7N2S)2CuCl4

    Science.gov (United States)

    Vishwakarma, Ashok K.; Kumari, Reema; Ghalsasi, Prasanna S.; Arulsamy, Navamoney

    2017-08-01

    The synthesis, thermal analysis, crystal structure and magnetic properties of (2-aminobenzothiazolium)2CuCl4, organic-inorganic hybrid compound, have been described. The compound crystallizes in the monoclinic space group P21/c with two formula units in a unit cell of dimensions a = 6.9522(4) Å, b = 9.6979(4) Å, c = 13.9633(6) Å, β = 97.849(3)° and volume 930.83(8) Å3 at 150(2) K. The structure consists of isolated nearly square planer [CuC14]2- units, with somewhat longer than normal Cusbnd Cl bond lengths [Cusbnd Cl (average) = 2.2711 Å]. The magnetic measurements of (2-aminobenzothiazolium)2CuCl4 using SQUID magnetometer show paramagnetic nature of the compound. Thermal measurements (TG-DTA and DSC) on this compound showed reversible phase transition at 83 °C. This transition is accompanied by the reversible change in colour of the prismatic crystal from green to dark brown, thermochromic behaviour. Temperature dependent EPR measurements on powdered sample ascertain change in coordination sphere around Cu(II) with shift in g|| = 2.150 and g⊥ = 2.071 at room temperature, typical of square planar, to g|| = 2.201 and g⊥ = 2.182 at 170 °C, typical of distorted tetrahedral geometry.

  19. (Dimethylformamide-κO(2-hydroxybenzoato-κ2O1,O1′[tris(1-methyl-1H-benzimidazol-2-ylmethyl-κN3amine-κN]manganese(II perchlorate dimethylformamide monosolvate

    Directory of Open Access Journals (Sweden)

    Baoliang Qi

    2010-10-01

    Full Text Available In the title complex, [Mn(C7H5O3(C27H27N7(C3H7NO]ClO4·C3H7NO, the MnII ion is coordinated in a slightly distorted monocapped trigonal-prismatic geometry. The tris(1-methyl-1H-benzimidazol-2-ylmethylamine (Mentb ligand coordinates in a tetradentate mode and the coordination is completed by a bis-chelating salicylate ligand and a dimethylformamide ligand. The hydroxy group and the ortho H atoms of the salicylate ligand were refined as disordered over two sites with occupancies of 0.581 (8 and 0.419 (8. Both disorder components of the hydroxy group form intramolecular O—H...O hydrogen bonds.

  20. (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.

  1. 2-Isopropyl-4,7-dimethyl-1-nitronaphthalene

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    Ahmed Benharref

    2017-04-01

    Full Text Available All the non-H atoms of the title compound, C15H17NO2, except the CH3 groups of the isopropyl unit and the O atoms of the nitro group, lie on a crystallographic mirror plane. The dihedral angle between the naphthalene plane and the nitro group is constrained to be 90° by symmetry. In the crystal, molecules are linked by π–π interactions [centroid–centroid separation = 3.6591 (4 Å] and stacked along the b-axis direction.

  2. Tris(2,2′-bipyridine-κ2 N,N′)cobalt(III) bis­[bis­(pyridine-2,6-dicarboxyl­ato-κ3 O 2,N,O 6)cobaltate(III)] perchlorate dimethyl­formamide hemisolvate 1.3-hydrate

    Science.gov (United States)

    Golenya, Irina A.; Boyko, Alexander N.; Kotova, Natalia V.; Haukka, Matti; Iskenderov, Turganbay S.

    2012-01-01

    In the title compound, [Co(C10H8N2)3][Co(C7H3NO4)2]2(ClO4)·0.5C3H7NO·1.3H2O, the CoIII atom in the complex cation is pseudoocta­hedrally coordinated by six N atoms of three chelating bipyridine ligands. The CoIII atom in the complex anion is coordinated by two pyridine N atoms and four carboxyl­ate O atoms of two doubly deprotonated pyridine-2,6-dicarboxyl­ate ligands in a distorted octa­hedral geometry. One dimethyl­formamide solvent mol­ecule and two water mol­ecules are half-occupied and one water mol­ecule is 0.3-occupied. O—H⋯O hydrogen bonds link the water mol­ecules, the perchlorate anions and the complex anions. π–π inter­actions between the pyridine rings of the complex anions are also observed [centroid–centroid distance = 3.804 (3) Å]. PMID:23125573

  3. (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.

  4. Model calculations on LIS. II1. 2-, 3- and 7-substituted indanones

    International Nuclear Information System (INIS)

    Hofer, O.

    1979-01-01

    The space close to the coordination site of 1-indanone is modified systematically by placing alkyl groups of different bulkiness on C-2, C-3 and C-7, resp. The 1 H-LIS for the compounds are interpreted using the one site and two site model for carbonyl. Precautionary measures are discussed for both models to give reliable results in the calculation. (author)

  5. Investigation into complexing in Re/sup 7/-H/sub 3/O/sup +/-SO/sub 4//sup 2 -/-H/sub 2/O system

    Energy Technology Data Exchange (ETDEWEB)

    Sinyakova, G S [AN Latvijskoj SSR, Riga. Inst. Neorganicheskoj Khimii

    1979-10-01

    Using the methods of spectrophotometry and conductometry it is shown, that in the ReO/sub 4//sup -/-H/sub 3/O/sup +/-SO/sub 4//sup 2 -/-H/sub 2/O system interaction between rhenium (7) and sulfuric acid takes place in a wide concentration range. In low-acid solutions at pH 2.0-0.9 rhenium(7) complex with proton is formed at the ratio of 1:1 with lgK/sub 1/=3.30+-0.02. In 1-10 mol. sulfuric acid observed is consecutive complexing at the rhenium(7) - sulfuric acid ratio in the complex of 1:1 and 1:2 respectively with lgK/sub 2/=0.93+-0.13 and lgK/sub 3/=0.34+-0.03. At the background of concentrated perchloric acid rhenium (7) and sodium sulfate form two complex compounds at rhenium (7) - sodium sulfate ratio of 1:1 and 1:2 with lgK/sub 1/=1.86+-0.02 and lgK/sub 2/=2.35+-0.03.

  6. Long Carbon Chains in the Warm Carbon-chain-chemistry Source L1527: First Detection of C7H in Molecular Clouds

    Science.gov (United States)

    Araki, Mitsunori; Takano, Shuro; Sakai, Nami; Yamamoto, Satoshi; Oyama, Takahiro; Kuze, Nobuhiko; Tsukiyama, Koichi

    2017-09-01

    Long carbon-chain molecules were searched for toward the low-mass star-forming region L1527, which is a prototypical source of warm carbon-chain chemistry (WCCC), using the 100 m Green Bank Telescope. Long carbon-chain molecules, C7H (2Π1/2), C6H (2Π3/2 and 2Π1/2), CH3C4H, and C6H2 (cumulene carbene, CCCCCCH2), and cyclic species of C3H and C3H2O were detected. In particular, C7H was detected for the first time in molecular clouds. The column density of C7H is determined to be 6 × 1010 cm-2. The column densities of the carbon-chain molecules including CH3C4H and C6H in L1527 relative to those in the starless dark cloud Taurus Molecular Cloud-1 Cyanopolyyne Peak (TMC-1 CP) tend to be systematically lower for long carbon-chain lengths. However, the column densities of C7H and C6H2 do not follow this trend and are found to be relatively abundant in L1527. This result implies that these long carbon-chain molecules are remnants of the cold starless phase. The results—that both the remnants and WCCC products are observed toward L1527—are consistent with the suggestion that the protostar can also be born in the parent core at a relatively early stage in the chemical evolution.

  7. 7 CFR 761.3 - Civil rights.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 7 2010-01-01 2010-01-01 false Civil rights. 761.3 Section 761.3 Agriculture... SPECIAL PROGRAMS GENERAL PROGRAM ADMINISTRATION General Provisions § 761.3 Civil rights. Part 15d of this title contains applicable regulations pertaining to civil rights and filing of discrimination complaints...

  8. Divergent H7 immunogens offer protection from H7N9 virus challenge.

    Science.gov (United States)

    Krammer, Florian; Albrecht, Randy A; Tan, Gene S; Margine, Irina; Hai, Rong; Schmolke, Mirco; Runstadler, Jonathan; Andrews, Sarah F; Wilson, Patrick C; Cox, Rebecca J; Treanor, John J; García-Sastre, Adolfo; Palese, Peter

    2014-04-01

    infections during the summer months of 2013, an increased number of cases has already been reported for the 2013-2014 winter season. The high case fatality rate, the ability to bind to receptors in the human upper respiratory tract in combination with several family clusters, and the emergence of neuraminidase inhibitor-resistant variants that show no loss of pathogenicity and the ability to transmit in animal models have raised concerns about a potential pandemic and have spurred efforts to produce vaccine candidates. Here we show that antigen preparations from divergent H7 strains are able to induce protective immunity against H7N9 infection.

  9. 3,5-Dimethyl-4-nitroso-1H-pyrazole

    Science.gov (United States)

    Safyanova, Inna; Dudarenko, Nikolay M.; Pavlenko, Vadim A.; Iskenderov, Turganbay S.; Haukka, Matti

    2011-01-01

    In the unit cell of the title compound, C5H7N3O, there are two conformers (A and B) which differ in the position of the oxime group with respect to the protonated pyrazole nitro­gen (trans in the A conformer and cis in the B conformer) and in the geometric parameters. The oxime group exists in the nitroso form in both conformers. In the crystal, mol­ecules are linked by inter­molecular N—H⋯O and N—H⋯N hydrogen bonds into zigzag-like chains along the b axis. PMID:22059058

  10. (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.

  11. 5α,6α-Epoxy-7-norcholestan-3β-yl acetate

    Directory of Open Access Journals (Sweden)

    L. C. R. Andrade

    2012-01-01

    Full Text Available The title cholestan, C28H46O3, was prepared by epoxidation of 7-norcholest-5-en-3β-yl acetate and crystallized by slow evaporation from an ethanolic solution. All rings are trans fused. The 3β-acetate and the 17β-cholestane side chain are in equatorial positions. The molecule is highly twisted due to its B-nor characteristic. A quantum chemical ab-initio Roothaan Hartree–Fock calculation of the equilibrium geometry of the isolated molecule gives values for bond lengths and valency angles in close agreement with the experimental ones.

  12. SYNTHESIS, CHARACTERIZATION AND ANTIOXIDANT ACTIVITY OF 7-HYDROXY-3',4'-DIMETHOXYFLAVONE

    Directory of Open Access Journals (Sweden)

    Elfi Susanti VH

    2012-03-01

    Full Text Available Synthesis of flavones and their derivatives has attracted considerable attention due to their significant pharmaceutical effects. 7-hydroxy-3',4'-dimethoxyflavone has been synthesized and its antioxidant activity has been investigated. Flavone was synthesized by oxidative cyclization of chalcone. 2',4'-dihydroxy-3,4-dimethoxychalcone was prepared by Claisen-Schmidt condensation of 2,4-dihydroxyacetophenones with 3,4-dimethoxybenzaldehydes in the presence of aqueous solution of sodium hydroxide and ethanol at room temperature. Oxidative cyclization of 2',4'-dihydroxy-3,4-dimethoxychalcone was done by using I2 catalyst in DMSO to form 7-hydroxy-3',4'-dimethoxyflavone. The synthesized compounds were characterized by means of their UV-Vis, IR, 1H-NMR and 13C-NMR spectral data. The compound was tested for their antioxidant activities by DPPH method.

  13. Astrophysical 3He(α ,γ )7Be and 3H(α ,γ )7Li direct capture reactions in a potential-model approach

    Science.gov (United States)

    Tursunov, E. M.; Turakulov, S. A.; Kadyrov, A. S.

    2018-03-01

    The astrophysical 3He(α ,γ )7Be and 3H(α ,γ )7Li direct capture processes are studied in the framework of the two-body model with potentials of a simple Gaussian form, which describe correctly the phase shifts in the s , p , d , and f waves, as well as the binding energy and the asymptotic normalization constant of the ground p3 /2 and the first excited p1 /2 bound states. It is shown that the E 1 transition from the initial s wave to the final p waves is strongly dominant in both capture reactions. On this basis the s -wave potential parameters are adjusted to reproduce the new data of the LUNA Collaboration around 100 keV and the newest data at the Gamov peak estimated with the help of the observed neutrino fluxes from the sun, S34(23-5+6keV ) =0.548 ±0.054 keV b for the astrophysical S factor of the capture process 3He(α ,γ )7Be . The resulting model describes well the astrophysical S factor in the low-energy big-bang nucleosynthesis region of 180-400 keV; however, it has a tendency to underestimate the data above 0.5 MeV. The energy dependence of the S factor is mostly consistent with the data and the results of the no-core shell model with continuum, but substantially different from the fermionic molecular dynamics model predictions. Two-body potentials, adjusted for the properties of the 7Be nucleus, 3He+α elastic scattering data, and the astrophysical S factor of the 3He(α ,γ )7Be direct capture reaction, are able to reproduce the properties of the 7Li nucleus, the binding energies of the ground 3 /2- and first excited 1 /2- states, and phase shifts of the 3H+α elastic scattering in partial waves. Most importantly, these potential models can successfully describe both absolute value and energy dependence of the existing experimental data for the mirror astrophysical 3H(α ,γ )7Li capture reaction without any additional adjustment of the parameters.

  14. 3-(1H-Indol-3-yl-2-(2-nitrobenzenesulfonamidopropanoic acid including an unknown solvate

    Directory of Open Access Journals (Sweden)

    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.

  15. 2,3-Diphenylmaleimide 1-methylpyrrolidin-2-one monosolvate

    Directory of Open Access Journals (Sweden)

    Evgeny Bulatov

    2014-03-01

    Full Text Available In the title compound, C16H11NOC5H9NO, the dihedral angles between the maleimide and phenyl rings are 34.7 (2 and 64.8 (2°. In the crystal, the 2,3-diphenylmaleimide and 1-methylpyrrolidin-2-one molecules form centrosymmetrical dimers via pairs of strong N—H...O hydrogen bonds and π–π stacking interactions between the two neighboring maleimide rings [centroid–centroid distance = 3.495 (2 Å]. The dimers are further linked by weak C—H...O and C—H...π hydrogen bonds into a three-dimensional framework.

  16. 4-Chloroselanyl-3,5-diethyl-1H-pyrazol-2-ium chloride

    Directory of Open Access Journals (Sweden)

    Maksym Seredyuk

    2011-11-01

    Full Text Available In the cation of the title compound, C7H12ClN2Se+·Cl−, the ethylene groups and the Se–Cl fragment adopt a cis configuration with a C—Se—Cl angle of 96.09 (6°. In the crystal, intermolecular N—H...Cl hydrogen bonds link two cations and two chlorine anions into centrosymmetric clusters. π–π interactions between the pyrazole rings [centroid–centroid distance of 3.530 (2 Å] link these clusters into columns along [001] with short intermolecular Se...Cl− contacts of 2.995 (1 Å.

  17. 4-Methyl-2-oxo-2H-chromen-7-yl 4-methoxybenzenesulfonate

    Directory of Open Access Journals (Sweden)

    Suman Sinha

    2011-12-01

    Full Text Available In the title compound, C17H14O6S, the 2H-chromene ring is essentially planar, with a maximum deviation of 0.016 (1 Å. The dihedral angle between the 2H-chromene and the benzene rings is 54.61 (5°. The C atom of the methoxy group is close to coplanar with its attached ring [deviation = 0.082 (2 Å]. In the crystal, molecules are connected via C—H...O hydrogen bonds, forming sheets lying parallel to the bc plane. Weak C—H...π interactions are also observed.

  18. 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.

  19. 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.

  20. Semiconducting perovskites (2-XC6H4C2H4NH3)2SnI4 (X = F, Cl, Br): steric interaction between the organic and inorganic layers.

    Science.gov (United States)

    Xu, Zhengtao; Mitzi, David B; Dimitrakopoulos, Christos D; Maxcy, Karen R

    2003-03-24

    Two new semiconducting hybrid perovskites based on 2-substituted phenethylammonium cations, (2-XC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) (X = Br, Cl), are characterized and compared with the previously reported X = F compound, with a focus on the steric interaction between the organic and inorganic components. The crystal structure of (2-ClC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) is solved in a disordered subcell [C2/m, a = 33.781(7) A, b = 6.178(1) A, c = 6.190(1) A, beta = 90.42(3)(o), and Z = 2]. The structure is similar to the known (2-FC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) structure with regard to both the conformation of the organic cations and the bonding features of the inorganic sheet. The (2-BrC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) system adopts a fully ordered monoclinic cell [P2(1)/c, a = 18.540(2) A, b = 8.3443(7) A, c = 8.7795(7) A, beta = 93.039(1)(o), and Z = 2]. The organic cation adopts the anti conformation, instead of the gauche conformation observed in the X = F and Cl compounds, apparently because of the need to accommodate the additional volume of the bromo group. The steric effect of the bromo group also impacts the perovskite sheet, causing notable distortions, such as a compressed Sn-I-Sn bond angle (148.7(o), as compared with the average values of 153.3 and 154.8(o) for the fluoro and chloro compounds, respectively). The optical absorption features a substantial blue shift (lowest exciton peak: 557 nm, 2.23 eV) relative to the spectra of the fluoro and chloro compounds (588 and 586 nm, respectively). Also presented are transport properties for thin-film field-effect transistors (TFTs) based on spin-coated films of the two hybrid semiconductors.

  1. Metabolism of 7-14C-2,3,5 triodobenzoic acid (TIBA) in soybeans plant (Glycine max)

    International Nuclear Information System (INIS)

    Sant'Anna, R.; Ohlrogge, A.J.; Christian, J.E.

    1975-01-01

    A metabolic study was done in mature seeds of field grown soybeans sprayed with 7- 14 C-2,3,5 triiodobenzoic acid (TIBA) at the onset of flowering. Seed extraction with 95% alcohol yielded only 65% of the total radioactivity present. No further studies were performed on the ethanol insoluble fraction. Upon acid base purification of the 14 C seed extracts, the ether phase (pH 9,0) contained about 70% of the activity suggesting the existence of a low polarity compound(s). Acid hydrolysis of the alcoholic extracts increased the radioactivity in the ether soluble fraction, while the basic treatment decreased it about the same level as for free TIBA. The latter behaviour seemed to indicate hydrolysis of a conjugation product(s). Alumina column chromatography was unsuccessful for separating the oil-activity combination; however, three radioactive peaks were obtained. The first two peaks degrated to form the last one, which coincided with the TIBA peak. When the alcoholic extracts were run in a Sephadex LH-20 column, oils, proteins and pigments separated from the radioactivity. Two main peaks appeared for the 14 C seeds extracts. Peak I was essentially unaltered when it was co-cromatographed with the standard 14 C-TIBA, peak II was indistinguishable from the TIBA peak. Although the work did not reach the final stage of caracterization, postulation was made for a conjugate nature of the ester type for peak I and the correspondence of peak II with free TIBA or TIBA in mixture with related compounds, such as 2,5 DIBA and 3,5 DIBA, products of its deiodination [pt

  2. N-(4-Chloro-1,3-benzothiazol-2-yl-2-(3-methylphenylacetamide monohydrate

    Directory of Open Access Journals (Sweden)

    H. S. Yathirajan

    2011-10-01

    Full Text Available In the title compound, C16H13ClN2OS·H2O, the dihedral angle between the mean planes of the benzothiazole ring system and the methylphenyl ring is 79.3 (6°. The crystal packing features intermolecular O—H...N, O—H...O and N—H...O hydrogen bonds involving the water molecule and weak C—H...O, C—H...Cg and π–π stacking interactions [centroid–centroid distances = 3.8743 (7, 3.7229 (7 and 3.7076 (8 Å].

  3. Effects of pH upon the environmental fate of [14C]fenitrothion in an aquatic microcosm

    International Nuclear Information System (INIS)

    Fisher, S.W.

    1985-01-01

    The environmental fate of [ 14 C]fenitrothion was evaluated in aquatic microcosms held at pH 8.3 or 6.7. No general effect attributable to pH was observed; however, several significant interactions were identified. Of these, the findings that statistically higher amounts of radioactivity were present in water held at pH 6.7 and that significantly less metabolism of the parent compound occurred in the organisms at pH 8.3 were preeminent. These differences seen in metabolism and environmental fate between pH values are relatively minor and do not compromise the safety of the compound

  4. Construction of three metal-organic frameworks based on multifunctional T-shaped tripodal ligands, H3PyImDC

    KAUST Repository

    Jing, Xuemin

    2010-08-04

    Three novel metal-organic frameworks (MOFs), |(C3H 7NO)2(H2O)|[Zn3(C10H 5N3O4)3(C3H 7NO)2] (1), |(H2O)5(H 3O)(NO3)|[Nd2(C10H5N 3O4)3(H2O)4] (2), and |(H2O)2|[Nd3(C10H5N 3O4)3(C10H4N 3O4)] (3), based on the T-shaped tripodal ligands 2-(pyridine-4-yl)-1H-4,5-imidazoledicarboxylic acid and 2-(pyridine-3-yl)-1H-4, 5-imidazoledicarboxylic acid (H3PyImDC), have been constructed under solvo-/hydrothermal conditions. The diverse coordination modes of H 3PyImDC ligands have afforded the assembly of three novel compounds. In compound 1, two oxygen atoms and three nitrogen atoms of the H 3PyImDC ligand, a T-shaped linker, coordinate to two zinc centers to form a novel bbm net with two distinct channels along the [100] and [001] directions. In compound 2, H3PyImDC ligands coordinate to neodymium centers to form a ladder-like chain which then interacts with a water molecules chain via hydrogen-bondings to construct a 3D supermolecular structure. In compound 3, H3PyImDC ligands, a T-shaped linker, coordinate to neodymium centers to form a (3,6)-connected net with an ant topology. In compounds 1-3, the two H3PyImDC ligands exhibit different coordination modes with zinc and neodymium centers, which afforded the expected structural diversity. Additionally, all three compounds exhibit strong fluorescence emissions in the solid state at room temperature. © 2010 American Chemical Society.

  5. (Benzyl isocyanide-κC1chlorido(2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl-κ2C1,Npalladium(II

    Directory of Open Access Journals (Sweden)

    Ana C. Mafud

    2013-01-01

    Full Text Available In the title compound, [Pd(C11H13ClNCl(C8H7N], which crystallized in the chiral space group P212121, the PdII atom is coordinated by two C atoms, a Csp2 atom of the 2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl ligand and a Csp atom from the benzyl isocyanide ligand, as well as an N atom of the ligand and a Cl atom, in a square-planar geometry. In the complex, there is a short C—H...Cl hydrogen bond and a C—H...π interaction. In the crystal, molecules are linked via C—H...Cl hydrogen bonds, forming chains along the a-axis direction.

  6. Solid-State Synthesis and Structure of the Enigmatic Ammonium Octaborate: (NH4)2[B7O9(OH)5]·3/4B(OH)3·5/4H2O.

    Science.gov (United States)

    Neiner, Doinita; Sevryugina, Yulia V; Schubert, David M

    2016-09-06

    The compound known since the 19th century as ammonium octaborate was structurally characterized revealing the ammonium salt of the ribbon isomer of the heptaborate anion, [B7O9(OH)5](2-), with boric acid and water molecules. Of composition (NH4)2B7.75O12.63·4.88H2O, it approximates the classical ammonium octaborate composition (NH4)2B8O13·6H2O and has the structural formula {(NH4)2[B7O9(OH)5]}4·3B(OH)3·5H2O. It spontaneously forms at room temperature in solid-state mixtures of ammonium tetraborate and ammonium pentaborate. It crystallizes in the monoclinic space group P21/c with a = 11.4137(2) Å, b = 11.8877(2) Å, c = 23.4459(3) Å, β = 90.092(1)°, V = 3181.19(8) Å(3), and Z = 2 and contains well-ordered ammonium cations and [B7O9(OH)5](2-) anions and disordered B(OH)3 and H2O molecules linked by extensive H bonding. Expeditious solid-state formation of the heptaborate anion under ambient conditions has important implications for development of practical syntheses of industrially useful borates.

  7. Bis(4-cyanophenolato[hydrotris(3,5-dimethylpyrazolylborato]nitrosylmolybdenum(II–4-hydroxybenzonitrile–dichloromethane (1/1/1

    Directory of Open Access Journals (Sweden)

    Jon A. McCleverty

    2010-12-01

    Full Text Available In the title compound, [Mo(C15H22BN6(C7H4NO2(NO]·C7H5NO·CH2Cl2, the central MoII atom adopts a distorted cis-MoO2N4 octahedral geometry with the hydrotris(3,5-dimethylpyrazolylborate anion attached to the metal in an N,N′,N′′-tridentate tripodal coordination mode. Two O-bonded 4-cyanophenolate anions and a nitrosyl cation complete the coodination of the MoII atom. Two intramolecular C—H...O and one C—H...N hydrogen bonds help to establish the configuration of the complex molecule. The crystal structure is stabilized by intermolecular C—H...N and C—H...O hydrogen bonds.

  8. C-terminal region of MAP7 domain containing protein 3 (MAP7D3 promotes microtubule polymerization by binding at the C-terminal tail of tubulin.

    Directory of Open Access Journals (Sweden)

    Saroj Yadav

    Full Text Available MAP7 domain containing protein 3 (MAP7D3, a newly identified microtubule associated protein, has been shown to promote microtubule assembly and stability. Its microtubule binding region has been reported to consist of two coiled coil motifs located at the N-terminus. It possesses a MAP7 domain near the C-terminus and belongs to the microtubule associated protein 7 (MAP7 family. The MAP7 domain of MAP7 protein has been shown to bind to kinesin-1; however, the role of MAP7 domain in MAP7D3 remains unknown. Based on the bioinformatics analysis of MAP7D3, we hypothesized that the MAP7 domain of MAP7D3 may have microtubule binding activity. Indeed, we found that MAP7 domain of MAP7D3 bound to microtubules as well as enhanced the assembly of microtubules in vitro. Interestingly, a longer fragment MDCT that contained the MAP7 domain (MD with the C-terminal tail (CT of the protein promoted microtubule polymerization to a greater extent than MD and CT individually. MDCT stabilized microtubules against dilution induced disassembly. MDCT bound to reconstituted microtubules with an apparent dissociation constant of 3.0 ± 0.5 µM. An immunostaining experiment showed that MDCT localized along the length of the preassembled microtubules. Competition experiments with tau indicated that MDCT shares its binding site on microtubules with tau. Further, we present evidence indicating that MDCT binds to the C-terminal tail of tubulin. In addition, MDCT could bind to tubulin in HeLa cell extract. Here, we report a microtubule binding region in the C-terminal region of MAP7D3 that may have a role in regulating microtubule assembly dynamics.

  9. Inorganic-organic hybrid structure: Synthesis, structure and magnetic properties of a cobalt phosphite-oxalate, [C4N2H12][Co4(HPO3)2(C2O4)3

    International Nuclear Information System (INIS)

    Mandal, Sukhendu; Natarajan, Srinivasan

    2005-01-01

    A hydrothermal reaction of a mixture of cobalt (II) oxalate, phosphorous acid, piperazine and water at 150 o C for 96h followed by heating at 180 o C for 24h gave rise to a new inorganic-organic hybrid solid, [C 4 N 2 H 12 ][Co 4 (HPO 3 ) 2 (C 2 O 4 ) 3 ], I. The structure consists of edge-shared CoO 6 octahedra forming a [Co 2 O 10 ] dimers that are connected by HPO 3 and C 2 O 4 units forming a three-dimensional structure with one-dimensional channels. The amine molecules are positioned within these channels. The oxalate units have a dual role of connecting within the plane of the layer as well as out of the plane. Magnetic susceptibility measurement shows the compound orders antiferromagnetically at low temperature (T N =22K). Crystal data: I, monoclinic, space group=P2 1 /c (No. 14). a=7.614(15), b=7.514(14), c=17.750(3)A, β=97.351(3) o , V=1007.30(3)A 3 , Z=2, ρ calc =2.466g/cm 3 , μ (MoKα) =3.496mm -1 , R 1 =0.0310 and wR 2 =0.0807 data [I>2σ(I)

  10. Protective Effects of Moringa oleifera on HBV Genotypes C and H Transiently Transfected Huh7 Cells

    Science.gov (United States)

    Feustel, Sina; Ayón-Pérez, Fabiola; Sandoval-Rodriguez, Ana; Rodríguez-Echevarría, Roberto; Contreras-Salinas, Homero

    2017-01-01

    Chronic hepatitis B infection treatment implicates a long-lasting treatment. M. oleifera extracts contain compounds with antiviral, antioxidant, and antifibrotic properties. In this study, the effect of M. oleifera was evaluated in Huh7 cells expressing either HBV genotypes C or H for the antiviral, antifibrotic, anti-inflammatory, and antioxidative responses. Huh7 cells were treated with an aqueous extract of M. oleifera (leaves) at doses of 0, 30, 45, or 60 μg/mL. The replicative virus and TGF-β1, CTGF, CAT, IFN-β1, and pgRNA expressions were measured by real time. HBsAg and IL-6 titers were determined by ELISA. CTGF, TGF-β1, IFN-β1, and pgRNA expressions decreased with M. oleifera treatment irrespective of the HBV genotype. HBsAg secretion in the supernatant of transfected Huh7 cells with both HBV genotypes was decreased regardless of the dose of M. oleifera. Similar effect was observed in proinflammatory cytokine IL-6, which had a tendency to decrease at 24 hours of treatment. Transfection with both HBV genotypes strongly decreased CAT expression, which is retrieved with M. oleifera treatment. M. oleifera treatment reduced fibrosis markers, IL-6, and HBsAg secretion in HBV genotypes C and H. However, at the level of replication, only HBV-DNA genotype C was slightly reduced with this treatment. PMID:29214184

  11. 4,10-Diallyloxy-1,2,3,6b,7,8,9,12b-octahydroperylene

    Directory of Open Access Journals (Sweden)

    Terrill D. Smith

    2010-01-01

    Full Text Available In the title compound, C26H28O2, the central atoms are coplanar, with the –CH2—CH2– links of the cyclohexene groups lying to either side of the plane and with the diallyloxy residues twisted out of this plane [C—C—O—C torsion angles = 16.6 (3 and −13.9 (3°]. In the crystal structure, molecules are connected into chains propagating in [100] via C—H...π interactions.

  12. Static susceptibility and heat capacity studies on V{sub 3}O{sub 7}.H{sub 2}O{sub 7} nanobelts

    Energy Technology Data Exchange (ETDEWEB)

    Hellmann, I., E-mail: i.hellmann@ifw-dresden.d [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung (IFW) Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Zakharova, G.S.; Volkov, V.L. [Institute of Solid State Chemistry, Ural Division, Russian Academy of Sciences, Pervomaiskaya ul. 91, Yekaterinburg 620219 (Russian Federation); Taeschner, C.; Leonhardt, A.; Buechner, B.; Klingeler, R. [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung (IFW) Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany)

    2010-04-15

    V{sub 3}O{sub 7}.H{sub 2}O nanobelts were prepared by a hydrothermal method at 190 deg. C using V{sub 2}O{sub 5}.nH{sub 2}O gel and H{sub 2}C{sub 2}O{sub 4}.2H{sub 2}O as starting agents. The obtained nanobelts have diameters ranging from 40 to 70 nm with lengths up to several micrometers. Measurements of the static magnetic susceptibility and the specific heat show a discontinuous phase transition at around T=145 K, which separates two regions of paramagnetic behavior.

  13. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  15. N,N-Dimethyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine monohydrate

    Directory of Open Access Journals (Sweden)

    Mohamed El Hafi

    2018-02-01

    Full Text Available The asymmetric unit of the title compound, C7H9N5·H2O, consists of two formula units differing slightly in the orientation of the dimethylamino groups. In the crystal, a combination of O—H...N and N—H...O hydrogen bonds involving the water molecules of crystallization, as well as slipped π-stacking interactions between pyrazolopyrimidine units form layers parallel to the bc plane.

  16. Poly[μ2-aqua-aqua-μ5-naphthalene-2,7-disulfonato-strontium

    Directory of Open Access Journals (Sweden)

    Shan Gao

    2011-12-01

    Full Text Available In the crystal structure of the polymeric title compound, [Sr(C10H6O6S2(H2O2]n, the naphthalene-2,7-disulfonate dianion uses one –SO3 unit to bind to two SrII cations and the other –SO3 unit to bind to three SrII cations; of the two coordinated water molecules, one is monodentate to one SrII cation, whereas the other bridges two SrII cations. The μ5-bridging mode of the dianon and the μ2-bridging mode of the water molecule generate a polymeric three-dimensional network which is consolidated by O—H...O hydrogen bonds. The SrII cation exists in an undefined eight-coordinate environment.

  17. 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.

  18. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  20. Investigation of the magnetic structure of KFeCl3, KFeBr3, Rb2MnCl4, and Rb3Mn2Cl7 compounds with magnetic correlations in one and two dimensions

    International Nuclear Information System (INIS)

    Gurewitz, E.

    1976-12-01

    The crystallographic structure of KFeCl 3 and KFeBr 3 consists of (FeCl) - octahedra packed in isolated zigzagging chains. These compounds order antiferromagnetically at Tsub(N) approximately 16 deg K and Tsub(N) approximately 9.5 deg K, respectively. Below Tsub(N) the Fe 2+ magnetic moments within a chain are ferromagnetically coupled, parallel to the chain axis, while the chains are coupled antiferromagnetically. In the temperatures Tsub(N) 3 has magnetic correlations within the chains only, whereas the correlations between the chains are negligible. Moessbauer effect measurements at these temperatures show a distinct hyperfine magnetic splitting, characteristic of relaxation phenomena. Cs 2 MnCl 4 , Rb 2 MnCl 4 and Rb 3 Mn 2 Cl 7 belong to the Asub(n+1)Bsub(n)Xsub(3n+1) family of compounds, with the Dsub(4h)sup(17) space group. These compounds order antiferromagnetically at Tsub(N) approximately 55 deg K for Cs 2 MnCl 4 and Rb 2 MnCl 4 , and Tsub(N) approximately 64.5 deg K for Rb 3 Mn 2 Cl 7 . Below Tsub(N) each Mn 2+ moment is along the c-axis and is coupled antiferromagnetically to the moments of its nearest neighbours (nn). These compounds behave like a two-dimensional antiferromagnet at T >= Tsub(N). Neutron scans of the reciprocal space exhibit rods of reflections along c vectorsup(*). The negligible interactions between next nn sets of MnCl 2 layers, a distance c vector apart, yield both in Rb 2 MnCl 4 and in Rb 3 Mn 2 Cl 7 , two distinctive magnetic structures (polytypes) below Tsub(N). (author)

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

    Directory of Open Access Journals (Sweden)

    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.

  2. A live attenuated cold-adapted influenza A H7N3 virus vaccine provides protection against homologous and heterologous H7 viruses in mice and ferrets

    International Nuclear Information System (INIS)

    Joseph, Tomy; McAuliffe, Josephine; Lu, Bin; Vogel, Leatrice; Swayne, David; Jin, Hong; Kemble, George; Subbarao, Kanta

    2008-01-01

    The appearance of human infections caused by avian influenza A H7 subtype viruses underscores their pandemic potential and the need to develop vaccines to protect humans from viruses of this subtype. A live attenuated H7N3 virus vaccine was generated by reverse genetics using the HA and NA genes of a low pathogenicity A/chicken/BC/CN-6/04 (H7N3) virus and the six internal protein genes of the cold-adapted A/Ann Arbor/6/60 ca (H2N2) virus. The reassortant H7N3 BC 04 ca vaccine virus was temperature sensitive and showed attenuation in mice and ferrets. Intranasal immunization with one dose of the vaccine protected mice and ferrets when challenged with homologous and heterologous H7 viruses. The reassortant H7N3 BC 04 ca vaccine virus showed comparable levels of attenuation, immunogenicity and efficacy in mice and ferret models. The safety, immunogenicity, and efficacy of this vaccine in mice and ferrets support the evaluation of this vaccine in clinical trials

  3. The oxonitridoborate Eu{sub 5}(BO{sub 2.51(7)}N{sub 0.49(7)}){sub 4} and the mixed-valent borates Sr{sub 3}Ln{sub 2}(BO{sub 3}){sub 4} (Ln = Ho, Er)

    Energy Technology Data Exchange (ETDEWEB)

    Hoeppe, Henning A.; Kazmierczak, Karolina; Grumbt, Christine; Schindler, Lisa [Institut fuer Physik, Universitaet Augsburg (Germany); Schellenberg, Inga; Poettgen, Rainer [Westfaelische Wilhelms-Universitaet Muenster, Institut fuer Anorganische und Analytische Chemie (Germany)

    2013-11-04

    The crystal structures of the mixed borates Sr{sub 3}Er{sub 2}(BO{sub 3}){sub 4} [Pnma, no. 62, Z = 4, a = 738.08(2), b = 1588.94(4), c = 867.81(2) pm, 683 reflections, 70 parameters, R1 = 0.037, wR2 = 0.077] and Sr{sub 3}Ho{sub 2}(BO{sub 3}){sub 4} [Pnma, no. 62, Z = 4, a = 738.45(7), b = 1591.55(12), c = 871.03(9) pm, 691 reflections, 59 parameters, R1 = 0.069, wR2 = 0.098] and europium oxonitridoborate Eu{sub 5}(BO{sub 2.51(7)}N{sub 0.49(7)}){sub 4} [Pnma, no. 62, Z = 12, a = 2232.2(5), b = 1603.1(3), c = 879.59(18) pm, 2880 reflections, 313 parameters, R1 = 0.027, wR2 = 0.059] were solved from single-crystal X-ray diffraction data. Eu{sub 5}(BO{sub 2.51(7)}N{sub 0.49(7)}){sub 4} adopts a threefold superstructure of the structure of Sr{sub 3}Ln{sub 2}(BO{sub 3}){sub 4} (Ln = Ho, Er). In both structure types, the different cations are situated on common sites with a pronounced preferential occupation but no complete ordering. These conclusions are based on the crystal structure refinement, {sup 151}Eu Moessbauer spectroscopy and MAPLE (Madelung part of lattice energy) calculations. The proposed Eu{sub 5}(BO{sub 3}){sub 4} contains nitrogen and has a formula Eu{sub 5}(BO{sub 2.51(7)}N{sub 0.49(7)}){sub 4} as confirmed by {sup 151}Eu Moessbauer spectroscopy. The optical reflectance spectrum of Eu{sub 5}(BO{sub 2.51(7)}N{sub 0.49(7)}){sub 4} is in accordance with the yellow colour of the compound. (Copyright copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. About the reactions sup 3 H(alpha,gamma) sup 7 Li and sup 3 He(alpha,gamma) sup 7 Be

    CERN Document Server

    Loeffler, W

    1993-01-01

    In this article the current experimental and theoretical status of the radiative alpha capture reactions sup 3 H(alpha,gamma) sup 7 Li and sup 3 He(alpha,gamma) sup 7 Be and their relations to primordial nucleosynthesis and the solar neutrino problem are reviewed. (author)

  5. Propane-1,3-diammonium bis[aquachlorido(4-hydroxypyridine-2,6-dicarboxylato-κ3O2,N,O6mercurate(II] tetrahydrate

    Directory of Open Access Journals (Sweden)

    Hossein Aghabozorg

    2008-08-01

    Full Text Available The reaction of mercury(II chloride dihydrate, propane-1,3-diamine and 4-hydroxypyridine-2,6-dicarboxylic acid in a 1:1:1 molar ratio in aqueous solution, resulted in the formation of the title compound, (C3H12N2[Hg(C7H3NO5Cl(H2O]2·4H2O or (pnH2[Hg(hypydcCl(H2O]2·4H2O (where pn is propane-1,3-diamine and hypydcH2 is 4-hydroxypyridine-2,6-dicarboxylic acid. The metal atom is coordinated by one chloride group, one water molecule cis to the chloride ligand and one (hypydc2− ligand. The coordinated water molecule is almost perpendicular to the plane of the aromatic ring of (hypydc2−. The geometry of the resulting HgClNO3 coordination can be described as distorted square-pyramidal. This structure also contains propane-1,3-diammonium (site symmetry 2 as a counter-ion and four uncoordinated water molecules. There is a wide range of non-covalent interactions consisting of hydrogen bonding [of the types O—H...O, N—H...O and C—H...O, with D...A ranging from 2.548 (5 to 3.393 (6 Å] and ion pairing.

  6. Targeting B7x and B7 H3 as New Immunotherapies for Prostate Cancer

    Science.gov (United States)

    2015-09-01

    well of 2% BSA/TBS for 1 h at 37 °C. Sera from unimmunized or immunized mice were serially diluted into 96 well plates in triplicate, and incubated...then added to each well, and the plates were incubated 1 h at 25 °C before absorbance at 405 nmwasmeasured in an ELISA reader. Serial dilutions and...CD4 helper T cells over CD8 killer T was significantly higher in older p27T187A/T187Amice compared with olderWTmice (Fig. 7B). This finding suggests

  7. Cross-reactivity between avian influenza A (H7N9) virus and divergent H7 subtypic- and heterosubtypic influenza A viruses.

    Science.gov (United States)

    Guo, Li; Wang, Dayan; Zhou, Hongli; Wu, Chao; Gao, Xin; Xiao, Yan; Ren, Lili; Paranhos-Baccalà, Gláucia; Shu, Yuelong; Jin, Qi; Wang, Jianwei

    2016-02-24

    The number of human avian H7N9 influenza infections has been increasing in China. Understanding their antigenic and serologic relationships is crucial for developing diagnostic tools and vaccines. Here, we evaluated the cross-reactivities and neutralizing activities among H7 subtype influenza viruses and between H7N9 and heterosubtype influenza A viruses. We found strong cross-reactivities between H7N9 and divergent H7 subtypic viruses, including H7N2, H7N3, and H7N7. Antisera against H7N2, H7N3, and H7N7 could also effectively neutralize two distinct H7N9 strains. Two-way cross-reactivities exist within group 2, including H3 and H4, whereas one-way cross-reactivities were found across other groups, including H1, H10, H9, and H13. Our data indicate that the hemaglutinins from divergent H7 subtypes may facilitate the development of vaccines for distinct H7N9 infections. Moreover, serologic diagnoses for H7N9 infections need to consider possible interference from the cross-reactivity of H7N9 with other subtype influenza viruses.

  8. 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

  9. Crystal structure of poly[N,N-diethyl-2-hydroxyethan-1-aminium [μ3-cyanido-κ3C:C:N-di-μ-cyanido-κ4C:N-dicuprate(I

    Directory of Open Access Journals (Sweden)

    Peter W. R. Corfield

    2016-07-01

    Full Text Available In the title compound, {(C6H16NO[Cu2(CN3]}n, the cyanide groups link the CuI atoms into an open three-dimensional anionic network, with the molecular formula Cu2(CN3−. One CuI atom is tetrahedrally bound to four CN groups, and the other CuI atom is bonded to three CN groups in an approximate trigonal-planar coordination. The tetrahedrally coordinated CuI atoms are linked into centrosymmetric dimers by the C atoms of two end-on bridging CN groups which bring the CuI atoms into close contact at 2.5171 (7 Å. Two of the cyanide groups bonded to the CuI atoms with trigonal-planar surrounding link the dimeric units into columns along the a axis, and the third links the columns together to form the network. The N,N-diethylethanolamine molecules used in the synthesis have become protonated at the N atoms and are situated in cavities in the network, providing charge neutrality, with no covalent interactions between the cations and the anionic network.

  10. Molecular structure and vibrational spectrum of the complex [ErL(H2O)(NO3)3] (L 1,4,10,13-tetraoxi-7,16-diaza(diphenylphosphinylmethyl) cyclooctadecane

    International Nuclear Information System (INIS)

    Minacheva, L.Kh.; Ivanova, I.S.; Kireeva, I.K.; Sakharova, V.G.; Tsivadze, A.Yu.; Sergienko, V.S.; Baulin, V.E.

    2000-01-01

    Synthesis of podandocoronand on the basis of diazo-18-crown-6 (DA18K6) 1,4,10,13-tetraoxi-7,16-diazo (diphenylphosphynylmethyl)cyclooctadecane (L) and erbium nitrate complex with L of the [ErL(H 2 O)(NO 3 ) 3 ] (I) composition is described. The IR-spectra of the free ligand L and complex I are studied and interpreted.The crystals are monoclinic: a = 10.432(2), b = 19.909(4), c = 21.361(4), β = 100.39(3) Deg, V = 4364(2) A 3 , sp. gr. P2 1 /n, Z = 4, ρ = 1.617 g/cm 3 . The structure I is formed of discrete molecular complexes. The Er atom coordination number is equal to 9. Three nitrate groups are bidentate-cyclic coordinated; two of them are in trans-position to each other; the H 2 O molecule is trans-position to the third NO 3 -group. The ligand L is coordinated by metal through two oxygen phosphoryl atoms. Thus, the Er atom coordination polyhedron may be described as octahedron, if each NO 3 -group occupies one coordination position. The Er-O(L) and Er-O(NO 3 ) overage distances are equal to 2.25 and 2.43 A correspondingly. Er-O(H 2 O) - 2.29 A. The H 2 O coordinated molecule forms intermolecular hydrogen atom and two oxygen atoms of the DA18K6 macrocycle [ru

  11. 1-{(Z-[2-Methoxy-5-(trifluoromethylanilino]methylidene}naphthalen-2(1H-one

    Directory of Open Access Journals (Sweden)

    Hakan Kargılı

    2013-02-01

    Full Text Available The title compound, C19H14F3NO2, crystallizes in the keto–amine tautomeric form, with a strong intramolecular N—H...O hydrogen bond. The molecule is almost planar; the dihedral angle between the naphthalene ring system and the benzene ring is 4.60 (7°. In the crystal, molecules are linked into chains along the c axis by C—H...O hydrogen bonds. The F atoms of the trifluoromethyl group are disordered over two positions with refined site occupancies of 0.668 (9 and 0.332 (9.

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

    Directory of Open Access Journals (Sweden)

    Cevher Gündoğdu

    2011-06-01

    Full Text Available In the title compound, C15H15NO3, the carbazole skeleton includes 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 0.89 (4°. The cyclohexenone ring has an envelope conformation. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into a three dimensional network. A weak C—H...π interaction is also observed.

  13. (E-3-Methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone

    Directory of Open Access Journals (Sweden)

    Yordanka Ivanova

    2016-09-01

    Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone, was synthesized by both an acid- and base-catalyzed aldol condensation of 3-methyl-6-acetyl-2(3H-benzothiazolone and 3,4,5-trimethoxyacetophenone. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

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

    Directory of Open Access Journals (Sweden)

    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].

  15. Preparation of Sm3H7 nanoparticles and their application in ammonia synthesis

    International Nuclear Information System (INIS)

    Liu Tong; Zhang Yaohua; Li Xingguo

    2006-01-01

    Sm 3 H 7 nanoparticles have been successfully produced by hydrogen plasma-metal reaction (HPMR) method, and then used to synthesize ammonia at 298 K and 1 atm. The morphologies of the Sm 3 H 7 nanoparticles before and after reaction were investigated by transmission electron microscopy, and the crystal structures at different steps by X-ray diffraction. Nessler's test was adopted to detect ammonia. It was found that the passivated Sm 3 H 7 nanoparticles possess polyhedron shape and smooth surface, with the average size of about 50 nm and the specific surface area 11.2 m 2 g -1 . It was proposed that Sm 3 H 7 nanoparticles react with oxygen and nitrogen to form ammonia, but ammonia production is not observable in the case of coarse particles. After ammonia synthesis, the morphology of Sm 3 H 7 nanoparticles changes into spongy surface and the mean particle size and specific surface area increase to 100 nm and 28.6 m 2 g -1 , respectively, due to the release of hydrogen. The hydrogen conversion percentage from samarium hydride is estimated to be 1.5%. Without O 2 , Sm 3 H 7 nanoparticles cannot react with N 2 or N 2 + H 2 at 298 K and 1 atm

  16. A novel layered bimetallic phosphite intercalating with organic amines: Synthesis and characterization of Co(H2O)4Zn4(HPO3)6.C2N2H1

    International Nuclear Information System (INIS)

    Lin Zhien; Fan Wei; Gao Feifei; Chino, Naotaka; Yokoi, Toshiyuki; Okubo, Tatsuya

    2006-01-01

    A new layered cobalt-zinc phosphite, Co(H 2 O) 4 Zn 4 (HPO 3 ) 6 .C 2 N 2 H 1 has been synthesized in the presence of ethylenediamine as the structure-directing agent. The compound crystallizes in the monoclinic system, space group Cc (No. 9), a=18.2090(8), b=9.9264(7), c=15.4080(7) A, β=114.098(4) o , V=2542.3(2) A 3 , Z=4, R=0.0323, wR=0.0846. The structure consists of ZnO 4 tetrahedra, CoO 6 octahedra and HPO 3 pseudopyramids through their vertices forming bimetallic phosphite layers parallel to the ab plane. Organic cations, which reside between the inorganic layers, are mobile and can be exchanged by NH 4 + cations without the collapse of the framework

  17. 3-Nitrobenzanthrone and 3-aminobenzanthrone induce DNA damage and cell signalling in Hepa1c1c7 cells.

    Science.gov (United States)

    Landvik, N E; Arlt, V M; Nagy, E; Solhaug, A; Tekpli, X; Schmeiser, H H; Refsnes, M; Phillips, D H; Lagadic-Gossmann, D; Holme, J A

    2010-02-03

    3-Nitrobenzanthrone (3-NBA) is a mutagenic and carcinogenic environmental pollutant found in diesel exhaust and urban air pollution. In the present work we have characterised the effects of 3-NBA and its metabolite 3-aminobenzanthrone (3-ABA) on cell death and cytokine release in mouse hepatoma Hepa1c1c7 cells. These effects were related to induced DNA damage and changes in cell signalling pathways. 3-NBA resulted in cell death and caused most DNA damage as judged by the amount of DNA adducts ((32)P-postlabelling assay), single strand (ss)DNA breaks and oxidative DNA lesions (comet assay) detected. An increased phosphorylation of H2AX, chk1, chk2 and partly ATM was observed using flow cytometry and/or Western blotting. Both compounds increased phosphorylation of p53 and MAPKs (ERK, p38 and JNK). However, only 3-NBA caused an accumulation of p53 in the nucleus and a translocation of Bax to the mitochondria. The p53 inhibitor pifithrin-alpha inhibited 3-NBA-induced apoptosis, indicating that cell death was a result of the triggering of DNA signalling pathways. The highest phosphorylation of Akt and degradation of IkappaB-alpha (suggesting activation of NF-kappaB) were also seen after treatment with 3-NBA. In contrast 3-ABA increased IL-6 release, but caused little or no toxicity. Cytokine release was inhibited by PD98059 and curcumin, suggesting that ERK and NF-kappaB play a role in this process. In conclusion, 3-NBA seems to have a higher potency to induce DNA damage compatible with its cytotoxic effects, while 3-ABA seems to have a greater effect on the immune system. Copyright 2009 Elsevier B.V. All rights reserved.

  18. 3-Nitrobenzanthrone and 3-aminobenzanthrone induce DNA damage and cell signalling in Hepa1c1c7 cells

    Energy Technology Data Exchange (ETDEWEB)

    Landvik, N.E. [Division of Environmental Medicine, Norwegian Institute of Public Health, P.O. Box 404 Torshov N-4303 Oslo (Norway); Arlt, V.M.; Nagy, E. [Section of Molecular Carcinogenesis, Institute of Cancer Research, Brookes Lawley Building, Sutton, Surrey SM2 5NG (United Kingdom); Solhaug, A. [Section for Toxicology, Department of Feed and Food Safety, National Veterinary Institute Pb 750 Sentrum, N-0106 Oslo (Norway); Tekpli, X. [EA SeRAIC, Equipe labellisee Ligue contre le Cancer, IFR 140, Universite de Rennes 1, Rennes (France); Schmeiser, H.H. [Research Group Genetic Alteration in Carcinogenesis, German Cancer Research Center, Im Neuenheimer Feld 280, 69120 Heidelberg (Germany); Refsnes, M. [Division of Environmental Medicine, Norwegian Institute of Public Health, P.O. Box 404 Torshov N-4303 Oslo (Norway); Phillips, D.H. [Section of Molecular Carcinogenesis, Institute of Cancer Research, Brookes Lawley Building, Sutton, Surrey SM2 5NG (United Kingdom); Lagadic-Gossmann, D. [EA SeRAIC, Equipe labellisee Ligue contre le Cancer, IFR 140, Universite de Rennes 1, Rennes (France); Holme, J.A., E-mail: jorn.holme@fhi.no [Division of Environmental Medicine, Norwegian Institute of Public Health, P.O. Box 404 Torshov N-4303 Oslo (Norway)

    2010-02-03

    3-Nitrobenzanthrone (3-NBA) is a mutagenic and carcinogenic environmental pollutant found in diesel exhaust and urban air pollution. In the present work we have characterised the effects of 3-NBA and its metabolite 3-aminobenzanthrone (3-ABA) on cell death and cytokine release in mouse hepatoma Hepa1c1c7 cells. These effects were related to induced DNA damage and changes in cell signalling pathways. 3-NBA resulted in cell death and caused most DNA damage as judged by the amount of DNA adducts ({sup 32}P-postlabelling assay), single strand (ss)DNA breaks and oxidative DNA lesions (comet assay) detected. An increased phosphorylation of H2AX, chk1, chk2 and partly ATM was observed using flow cytometry and/or Western blotting. Both compounds increased phosphorylation of p53 and MAPKs (ERK, p38 and JNK). However, only 3-NBA caused an accumulation of p53 in the nucleus and a translocation of Bax to the mitochondria. The p53 inhibitor pifithrin-alpha inhibited 3-NBA-induced apoptosis, indicating that cell death was a result of the triggering of DNA signalling pathways. The highest phosphorylation of Akt and degradation of I{kappa}B-{alpha} (suggesting activation of NF-{kappa}B) were also seen after treatment with 3-NBA. In contrast 3-ABA increased IL-6 release, but caused little or no toxicity. Cytokine release was inhibited by PD98059 and curcumin, suggesting that ERK and NF-{kappa}B play a role in this process. In conclusion, 3-NBA seems to have a higher potency to induce DNA damage compatible with its cytotoxic effects, while 3-ABA seems to have a greater effect on the immune system.

  19. 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.

  20. Skeleton polyhedral rearrangements of 8-alkyl-7,9-dicarba-nido-undecaborate(-1) anion to 11-alkyl-2,7-dicarba-nido-undecaborane(13) and to 9-alkyl-7,8-dicarba-nido-undecaborate(-1) anion. Molecular structure of 2,7-Me2-11-PhCH2-2,7-C2B9H10

    International Nuclear Information System (INIS)

    Zakharkin, K.I.; Zhigareva, G.G.; Antonovich, V.A.; Yanovskij, A.I.; Struchkov, Yu.T.

    1986-01-01

    Using the methods of 1 H and 11 B NMR-spectroscopy and X-ray diffraction analysis skeleton polyhedral rearrangements of carboranes are studied. During protonation of anion 8-R-7, 9-R' 2 -7, 9-C 2 B 9 H 9 - the skeleton polyhedral rearrangement in the series of nido-carboranes, resulting in 2,7-R' 2 -11-R-2, 7-C 2 B 9 H 10 (R=Me, PhCH 2 , R'=H, Me) is observed. The rearrangement is reversible. On the detachment of two protons from 2,7-Me 2 -11-PhCH 2 -2,7-C 2 B 9 H 10 and during subsequent protonation the skeleton polyhedral rearrangement with the formation of anion 9-PhCH 2 -7,8-Me 2 -7,8-C 2 B 9 H 9 - takes place

  1. [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.

  2. Quaternary chalcogenides La{sub 3}Sn{sub 0.5}InS{sub 7} and La{sub 3}Sn{sub 0.5}InSe{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Iyer, Abishek K.; Lee, Emma J.; Bernard, Guy M.; Michaelis, Vladimir K.; Mar, Arthur [Department of Chemistry, University of Alberta, Edmonton, AB (Canada); Yin, Wenlong [Department of Chemistry, University of Alberta, Edmonton, AB (Canada); Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang (China)

    2017-12-13

    The quaternary chalcogenides La{sub 3}Sn{sub 0.5}InS{sub 7} and La{sub 3}Sn{sub 0.5}InSe{sub 7} were prepared by reactions of the elements at 1050 C and 950 C, respectively. They adopt noncentrosymmetric structures [hexagonal, space group P6{sub 3}, Z = 2; a = 10.2993(11) Aa, c = 6.0921(6) Aa for La{sub 3}Sn{sub 0.5}InS{sub 7}; a = 10.6533(7) Aa, c = 6.4245(4) Aa for La{sub 3}Sn{sub 0.5}InSe{sub 7}] in which the half-occupancy of Sn atoms within octahedral sites classifies them as belonging to the La{sub 3}Mn{sub 0.5}SiS{sub 7}-type branch of the large family of quaternary rare-earth chalcogenides RE{sub 3}M{sub 1-x}M{sup '}Ch{sub 7}. The site distribution in La{sub 3}Sn{sub 0.5}InCh{sub 7}, with higher-valent Sn atoms occupying octahedral instead of tetrahedral sites, is reversed from the typical situation observed in other RE{sub 3}M{sub 1-x}M{sup '}Ch{sub 7} compounds. The ordered distribution of Sn atoms in octahedral sites and In atoms in tetrahedral sites was evaluated by bond valence sum analyses. Moreover, {sup 119}Sn solid-state nuclear magnetic resonance (NMR) spectroscopy confirms the occupation of Sn{sup 4+} species exclusively within octahedral sites. An optical bandgap of 1.45 eV was found for La{sub 3}Sn{sub 0.5}InS{sub 7}. Band structure calculations on an ordered superstructure model of La{sub 3}Sn{sub 0.5}InS{sub 7} reveal that avoidance of strongly Sn-S antibonding levels is an important driving force for the Sn deficiency. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Characterization of H7 Influenza A Virus in Wild and Domestic Birds in Korea

    Science.gov (United States)

    Kang, Hyun-Mi; Park, Ha-Young; Lee, Kyu-Jun; Choi, Jun-Gu; Lee, Eun-Kyoung; Song, Byung-Min; Lee, Hee-Soo; Lee, Youn-Jeong

    2014-01-01

    During surveillance programs in Korea between January 2006 and March 2011, 31 H7 avian influenza viruses were isolated from wild birds and domestic ducks and genetically characterized using large-scale sequence data. All Korean H7 viruses belonged to the Eurasian lineage, which showed substantial genetic diversity, in particular in the wild birds. The Korean H7 viruses from poultry were closely related to those of wild birds. Interestingly, two viruses originating in domestic ducks in our study had the same gene constellations in all segment genes as viruses originating in wild birds. The Korean H7 isolates contained avian-type receptors (Q226 and G228), no NA stalk deletion (positions 69–73), no C-terminal deletion (positions 218–230) in NS1, and no substitutions in PB2-627, PB1-368, and M2-31, compared with H7N9 viruses. In pathogenicity experiments, none of the Korean H7 isolates tested induced clinical signs in domestic ducks or mice. Furthermore, while they replicated poorly, with low titers (10 0.7–1.3EID50/50 µl) in domestic ducks, all five viruses replicated well (up to 7–10 dpi, 10 0.7–4.3EID50/50 µl) in the lungs of mice, without prior adaptation. Our results suggest that domestic Korean viruses were transferred directly from wild birds through at least two independent introductions. Our data did not indicate that wild birds carried poultry viruses between Korea and China, but rather, that wild-type H7 viruses were introduced several times into different poultry populations in eastern Asia. PMID:24776918

  4. C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings prepared from TiC{sub 0.7}N{sub 0.3} powder using ball milling followed by oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Liang, E-mail: haoliang@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Wang, Zhenwei, E-mail: 1004329228@qq.com [School of Naval Architecture and Ocean Engineering, Harbin Institute of Technology, Weihai, No. 2, Wenhua West Road, Weihai 264209 (China); Zheng, Yaoqing, E-mail: 13612177268@163.com [College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Li, Qianqian, E-mail: 1482471595@qq.com [College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Guan, Sujun, E-mail: sujunguan1221@gmail.com [College of Mechanical Engineering & Graduate School, Chiba University, 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522 (Japan); Zhao, Qian, E-mail: zhaoqian@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Cheng, Lijun, E-mail: chenglijun@tust.edu.cn [Tianjin Key Lab of Integrated Design and On-line Monitoring for Light Industry & Food Machinery and Equipment, Tianjin (China); College of Mechanical Engineering, Tianjin University of Science & Technology, No. 1038 Dagu Nanlu, Hexi District, Tianjin 300222 (China); Lu, Yun, E-mail: luyun@faculty.chiba-u.jp [College of Mechanical Engineering & Graduate School, Chiba University, 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522 (Japan); Liu, Jizi, E-mail: jzliu@njust.edu.cn [Herbert Gleiter Institute of Nanoscience, Nanjing University of Science and Technology, No. 200, Xiaolingwei Street, Nanjing 210094 (China)

    2017-01-01

    Highlights: • TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} coatings were prepared by ball milling followed by oxidation. • In situ co-doping of C and N with simultaneous TiO{sub 2} formation was observed. • Improved photocatalytic activity under UV/visible light was noticed. • Synergism in co-doping and heterojunction formation promoted carrier separation. - Abstract: Ball milling followed by heat oxidation was used to prepared C, N co-doped TiO{sub 2} coatings on the surfaces of Al{sub 2}O{sub 3} balls from TiC{sub 0.7}N{sub 0.3} powder. The as-prepared coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible spectrophotometer (UV–vis). The results show that continuous TiC{sub 0.7}N{sub 0.3} coatings were formed after ball milling. C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings were prepared after the direct oxidization of TiC{sub 0.7}N{sub 0.3} coatings in the atmosphere. However, TiO{sub 2} was hardly formed in the surface layer of TiC{sub 0.7}N{sub 0.3} coatings within a depth less than 10 nm during the heat oxidation of TiC{sub 0.7}N{sub 0.3} coatings in carbon powder. Meanwhile, the photocatalytic activity evaluation of these coatings was conducted under the irradiation of UV and visible light. All the coatings showed photocatalytic activity in the degradation of MB no matter under the irradiation of UV or visible light. The C, N co-doped TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite coatings showed the most excellent performance. The enhancement under visible light irradiation should attribute to the co-doping of carbon and nitrogen, which enhances the absorption of visible light. The improvement of photocatalytic activity under UV irradiation should attribute to the synergistic effect of C, N co-doping, the formation of rutile-anatase mixed phases and the TiO{sub 2}/TiC{sub 0.7}N{sub 0.3} composite microstructure.

  5. 3-(Aminocarbonylpyridinium diaqua-bis(pyridine-2,6-dicarboxylatobismuthate(III monohydrate

    Directory of Open Access Journals (Sweden)

    Janet Soleimannejad

    2012-07-01

    Full Text Available The asymmetric unit of the ionic title compound, (C6H7N2O[Bi(C7H3NO42(H2O2]·H2O or (acpyH[Bi(pydc2(H2O2]·H2O, contains an [Bi(pydc2(H2O2]− anion (where pydcH2 is pyridine-2,6-dicarboxylic acid, a protonated 3-(aminocarbonylpyridine as counter-ion, (acpyH+, and one uncoordinated water molecule. The anion is an eight-coordinate complex with a square-antiprismatic geometry around the BiIII atom. In the crystal, extensive O—H...O and N—H...O hydrogen bonds, as well as ion pairing, C=O...π interactions [O...centroid distance = 3.583 (5 Å], π–π stacking [centroid–centroid distance = 3.864 (3 Å], and C—H...π and C—H...O interactions, play an important role in the formation and stabilization of the three-dimensional supramolecular structure.

  6. catena-Poly[[bis[2-(2,3-dimethylanilinobenzoato-κO]cadmium(II]-di-μ-3-pyridylmethanol-κ2N:O;κ2O:N

    Directory of Open Access Journals (Sweden)

    Tadeusz Lis

    2008-03-01

    Full Text Available In the crystal structure of the title compound, [Cd(C15H14NO22(C6H7NO2]n, the Cd atom displays a distorted octahedral geometry, including two pyridine N atoms and two hydroxyl O from four symmetry-related 3-pyridylmethanol (3-pyme ligands and two carboxylate O atoms from mefenamate [2-(2,3-dimethylanilinobenzoate] anions. The Cd atoms are connected via the bridging 3-pyme ligands into chains, that extend in the a-axis direction. The Cd atom is located on a center of inversion, whereas the 3-pyme ligands and the mefenamate anions occupy general positions.

  7. 7 CFR 1160.101 - Act.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 9 2010-01-01 2009-01-01 true Act. 1160.101 Section 1160.101 Agriculture Regulations... Definitions § 1160.101 Act. Act means the Fluid Milk Promotion Act of 1990, Subtitle H of Title XIX of the Food, Agriculture, Conservation, and Trade Act of 1990, Public Law 101-624, 7 U.S.C. 6401-6417, and any...

  8. Spectroscopy and photophysics of flavin related compounds: Riboflavin and iso-(6,7)-riboflavin

    International Nuclear Information System (INIS)

    Sikorska, Ewa; Khmelinskii, Igor; Komasa, Anna; Koput, Jacek; Ferreira, Luis F.V.; Herance, Jose R.; Bourdelande, Jose L.; Williams, Sian L.; Worrall, David R.; Insinska-Rak, MaIgorzata; Sikorski, Marek

    2005-01-01

    The photochemistry and photophysics of isoalloxazines (10-substituted 2,3,4,10-tetrahydro-benzo[g]pteridine-2,4-diones), and especially flavins (7,8-dimethyl substituted isoalloxazines), are of considerable interest due to the biological relevance of these compounds. In this paper we report data concerning the photophysics of riboflavin and iso-(6,7)-riboflavin (10-(2,3,4,5-tetrahydroxypentyl)-6,7-dimethylbenzo[g]pteridine-2,4(3H,10H) -dione), and correlate the spectroscopic observations with theoretical calculations performed using time-dependent density functional theory. On the basis of these calculations the lowest excited singlet and triplet states are both assigned (π,π*) symmetry, and this result is used to explain the relatively low singlet oxygen quantum yields in comparison with alloxazines. Time-resolved emission studies have indicated 6,7-dimethylalloxazine a photodegradation product of iso-(6,7)-riboflavin

  9. 2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12H-6λ5-dibenzo[d,i][1,3,7,2]dioxazaphosphecin-6-thione

    Directory of Open Access Journals (Sweden)

    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.

  10. Second order magnetic phase transition and scaling analysis in iron doped manganite La{sub 0.7}Ca{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ginting, Dianta [Department of Applied Physics and Institute of Natural Sciences, Kyung Hee University, Yong-in 446-701 (Korea, Republic of); Nanto, Dwi [Physics Education, Syarif Hidayatullah State Islamic University, Jakarta 15412 (Indonesia); Denny, Yus Rama [Department of Electrical Engineering, University of Sultan Ageng Tirtayasa, Banten 42435 (Indonesia); Tarigan, Kontan [Department of Mechanical Engineering, Mercu Buana University, Jakarta-Barat, Jakarta 11650 (Indonesia); Hadi, Syamsul [Department of Mechanical Engineering, State Polytechnic of Malang, East Java 65100 (Indonesia); Ihsan, Mohammad [PSTBM-BATAN, Kawasan Puspiptek Serpong, Tangerang Selatan, Banten 15314 (Indonesia); Institute of Electronic Materials, University of Wollongong, Wollongong NSW 2522 (Australia); Rhyee, Jong-Soo, E-mail: jsrhyee@khu.ac.kr [Department of Applied Physics and Institute of Natural Sciences, Kyung Hee University, Yong-in 446-701 (Korea, Republic of)

    2015-12-01

    We investigated magnetic properties of La{sub 0.7}Ca{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} (x=0.09 and 0.11) compounds in terms of isothermal magnetization analysis and scaling behavior with various critical exponents. From the Landau theory of magnetic phase transition, we found that the paramagnetic to ferromagnetic phase transition in La{sub 0.7}Ca{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3} (x=0.09 and 0.11) compounds is the type of second order magnetic transition (SOMT), which contrary to the first order magnetic transition (FOMT) for low Fe-doped compounds (x<0.09) in previous reports. When we investigate the critical behavior of the compounds near T=T{sub c} by the modified Arrott plot, Kouvel–Fisher plots, and critical isothermal analysis, the estimated critical exponents β, γ, and δ are in between the theoretically predicted values for three-dimensional Heisenberg and mean-field interaction models. It is noteworthy that the scaling relations are obeyed in terms of renormalization magnetization m=ε{sup −β}M(H,ε) and renormalized field h=|ε|{sup β+γ}H. Temperature-dependent effective exponents β{sub eff} and γ{sub eff} correspond to the ones of disordered ferromagnets. It is shown that the magnetic state of the compounds is not fully described by the conventional localized-spin interaction model because the ferromagnetic interaction has itinerant character by increasing Fe-doping concentration. - Highlights: • The ferromagnetic phase transition is of second order in La{sub 0.7}Ca{sub 0.3}Mn{sub 1−x}Fe{sub x}O{sub 3}. • The critical exponents are in between the 3D Heisenberg and mean-field models. • The ferromagnetic interaction becomes more itinerant by Fe-doping.

  11. Avian influenza H7N9/13 and H7N7/13: a comparative virulence study in chickens, pigeons, and ferrets.

    Science.gov (United States)

    Kalthoff, Donata; Bogs, Jessica; Grund, Christian; Tauscher, Kerstin; Teifke, Jens P; Starick, Elke; Harder, Timm; Beer, Martin

    2014-08-01

    Human influenza cases caused by a novel avian H7N9 virus in China emphasize the zoonotic potential of that subtype. We compared the infectivity and pathogenicity of the novel H7N9 virus with those of a recent European avian H7N7 strain in chickens, pigeons, and ferrets. Neither virus induced signs of disease despite substantial replication in inoculated chickens and rapid transmission to contact chickens. Evidence of the replication of both viruses in pigeons, albeit at lower levels of RNA excretion, was also detected. No clear-cut differences between the two H7 isolates emerged regarding replication and antibody development in avian hosts. In ferrets, in contrast, greater replication of the avian H7N9 virus than of the H7N7 strain was observed with significant differences in viral presence, e.g., in nasal wash, lung, and cerebellum samples. Importantly, both viruses showed the potential to spread to the mammal brain. We conclude that efficient asymptomatic viral replication and shedding, as shown in chickens, facilitate the spread of H7 viruses that may harbor zoonotic potential. Biosafety measures are required for the handling of poultry infected with avian influenza viruses of the H7 subtype, independently of their pathogenicity for gallinaceous poultry. This study is important to the field since it provides data about the behavior of the novel H7N9 avian influenza virus in chickens, pigeons, and ferrets in comparison with that of a recent low-pathogenicity H7N7 strain isolated from poultry. We clearly show that chickens, but not pigeons, are highly permissive hosts of both H7 viruses, allowing high-titer replication and virus shedding without any relevant clinical signs. In the ferret model, the potential of both viruses to infect mammals could be demonstrated, including infection of the brain. However, the replication efficiency of the H7N9 virus in ferrets was higher than that of the H7N7 strain. In conclusion, valuable data for the risk analysis of low

  12. Atom-radical reaction dynamics of O(3P)+C3H5→C3H4+OH: Nascent rovibrational state distributions of product OH

    Science.gov (United States)

    Park, Jong-Ho; Lee, Hohjai; Kwon, Han-Cheol; Kim, Hee-Kyung; Choi, Young-Sang; Choi, Jong-Ho

    2002-08-01

    The reaction dynamics of ground-state atomic oxygen [O(3P)] with allyl radicals (C3H5) has been investigated by applying a combination of crossed beams and laser induced fluorescence techniques. The reactants O(3P) and C3H5 were produced by the photodissociation of NO2 and the supersonic flash pyrolysis of precursor allyl iodide, respectively. A new exothermic channel of O(3P)+C3H5→C3H4+OH was observed and the nascent internal state distributions of the product OH (X 2Π:υ″=0,1) showed substantial bimodal internal excitations of the low- and high-N″ components without Λ-doublet and spin-orbit propensities in the ground and first excited vibrational states. With the aid of the CBS-QB3 level of ab initio theory and Rice-Ramsperger-Kassel-Marcus calculations, it is predicted that on the lowest doublet potential energy surface the major reaction channel of O(3P) with C3H5 is the formation of acrolein (CH2CHCHO)+H, which is consistent with the previous bulk kinetic experiments performed by Gutman et al. [J. Phys. Chem. 94, 3652 (1990)]. The counterpart C3H4 of the probed OH product in the title reaction is calculated to be allene after taking into account the factors of reaction enthalpy, barrier height and the number of intermediates involved along the reaction pathway. On the basis of population analyses and comparison with prior calculations, the statistical picture is not suitable to describe the reactive atom-radical scattering processes, and the dynamics of the title reaction is believed to proceed through two competing dynamical pathways. The major low N″-components with significant vibrational excitation may be described by the direct abstraction process, while the minor but extraordinarily hot rotational distribution of high N″-components implies that some fraction of reactants is sampled to proceed through the indirect short-lived addition-complex forming process.

  13. Synthesis and biological activity of some 1,3-dihydro-2H-3-benzazepin-2-ones with a piperazine moiety as bradycardic agents.

    Science.gov (United States)

    Liang, Hong-Yu; Zhang, Deng-Qing; Yue, Yun; Shi, Zhe; Zhao, Sheng-Yin

    2010-02-01

    A series of 1,3-dihydro-2H-3-benzazepin-2-ones with a piperazine moiety were designed and synthesized by treating the common intermediate of 1,3-dihydro-7,8-dimethoxy-3-[3-(1-piperazinyl)propyl]-2H-3-benzazepin-2-ones with a variety of N-aryl-2-chloroacetamides and acyl chlorides. Their structures have been characterized by (1)H-NMR, MS, and elemental analysis. The title compounds were evaluated for their bradycardic activity in vitro. Most of the synthesized compounds exhibited some vasorelaxant activity and heart-rate-reducing activity with bradycardic potency.

  14. Di-μ-chlorido-bis({4-[bis(trimethylsilylamino]-6-chloro-2,2,8,8-tetramethyl-5,7-bis(trimethylsilyl-3,5,7-triaza-4,6-diphospha-2,8-disilanon-3-en-4-ido-κ2P,P′}palladium(II diethyl ether disolvate

    Directory of Open Access Journals (Sweden)

    Martha Höhne

    2016-06-01

    Full Text Available The title compound, [Pd2(C18H54Cl2N4P2Si62Cl2]·2C4H10O, features a dinuclear chloride-bridged palladium complex bearing two equivalents of the novel monoanionic mixed valent (λ3-P—N—(λ5-P ligand. A metal catalyzed coupling of two aminoiminophosphines and a shift of one chlorine from the metal to the phosphorus results in the (λ3-P—N—(λ5-P ligand. The molecule contains a planar bimetallic Pd2Cl2 core with a crystallographic centre of inversion at the mid-point of the Pd...Pd line. The Pd atoms are in a distorted square-planar arrangement, where the P/Pd/P and Cl/Pd/Cl planes are twisted with respect to each other by a dihedral angle of 7.57 (4°. The P—Pd—P bite angle is 71.380 (18°. Intramolecular C—H...Cl interactions are observed. In the crystal, the diethyl ether solvent molecule is disordered over two sites, with an occupancy ratio of 0.788 (5:0.212 (5.

  15. 6-Chloro-3-[5-(3-methoxy-8-methyl-4-quinolyl-1-phenyl-4,5-dihydro-1H-pyrazol-3-yl]-2-methyl-4-phenylquinoline

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2009-11-01

    Full Text Available In the title compound, C36H29ClN4O, the dihydropyrazole ring adopts an envelope conformation. The two quinoline ring systems (r.m.s. deviations = 0.029 and 0.018 Å are oriented at a dihedral angle of 71.43 (4°. One of the quinoline rings makes a dihedral angle of 65.40 (7° with the phenyl substituent. In the crystal, molecules are linked into chains along the b axis by intermolecular C—H...N hydrogen bonds. In addition, C—H...π and π–π [centroid–centroid distance = 3.7325 (8 Å] interactions are observed.

  16. Ba{sub 1.63}La{sub 7.39}Si{sub 11}N{sub 23}Cl{sub 0.42}:Ce{sup 3+} - a nitridosilicate chloride with a zeolite-like structure

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, Peter; Oeckler, Oliver [Institute of Mineralogy, Crystallography and Materials Science, Faculty of Chemistry and Mineralogy, Leipzig University, Scharnhorststrasse 20, 04275 Leipzig (Germany); Durach, Dajana; Schnick, Wolfgang [Department of Chemistry, University of Munich (LMU), Butenandtstrasse 5-13, 81377 Munich (Germany)

    2016-05-15

    The nitridosilicate chloride Ba{sub 1.63}La{sub 7.39}Si{sub 11}N{sub 23}Cl{sub 0.42}:Ce{sup 3+} was synthesized by metathesis reaction starting from LaCl{sub 3}, BaH{sub 2}, CeF{sub 3} and the product of the ammonolysis of Si{sub 2}Cl{sub 6}. The title compound is stable towards air and moisture. Diffraction data of a microcrystal were recorded using microfocused synchrotron radiation. X-ray spectroscopy confirms the chemical composition of the crystal. IR spectra corroborate absence of N-H bonds. The compound is homeotypic to Ba{sub 2}Nd{sub 7}Si{sub 11}N{sub 23} and crystallizes in space group Cmmm with a = 11.009(3), b = 23.243(8), c = 9.706(4) Aa and Z = 4, R{sub 1}(all) = 0.0174. According to bond valence sum calculations, some crystallographic positions show complete occupancy by Ba or La whereas others contain significant amounts of both elements. In contrast to the structure prototype Ba{sub 2}Nd{sub 7}Si{sub 11}N{sub 23}, Ba{sub 1.63}La{sub 7.39}Si{sub 11}N{sub 23}Cl{sub 0.42}:Ce{sup 3+} contains chloride ions in channels of the SiN{sub 4} tetrahedra network, hinting at various substitution possibilities of the complex zeolite-like structure. (Copyright copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. 2,2-Dimethyl-2,3-dihydropyrano[2,3-a]carbazol-4(11H-one

    Directory of Open Access Journals (Sweden)

    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.

  18. N-(3-Chlorophenylmaleamic acid

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    B. Thimme Gowda

    2010-07-01

    Full Text Available In the title compound, C10H8ClNO3, the molecular conformation is stabilized by two intramolecular hydrogen bonds. The first is a short O—H...O hydrogen bond within the maleamic acid unit and the second is a C—H...O hydrogen bond which connects the amide group with the phenyl ring. The maleamic acid unit is essentially planar, with an r.m.s. deviation of 0.044 Å, and makes a dihedral angle of 15.2 (1° with the phenyl ring. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into C(7 chains running [010].

  19. Synthesis of the enantiomers of [3-3H]-2-[[4-[(7-chloro-4-quinolinyl)-amino]pentyl]ethylamino]eth anol, [3-3H]-hydroxychloroquine

    International Nuclear Information System (INIS)

    Ellames, G.J.; Herbert, J.M.; Peace, J.E.; Smith, D.J.; Wedge, K.J.

    1995-01-01

    The enantiomers of [3- 3 H]-2-[[4-[(7-chloro-4-quinolinyl)amino] pentyl]ethylamino]ethanol, [3- 3 H]-hydroxychloroquine, (R)-8 and (S)-8, have been prepared in two steps from the known precursors 4,7-dichloro-3-iodoquinoline, and the enantiomers of 2-[(4-aminopentyl) ethyl-amino]ethanol, (R)-2 and (S)-2, by formation of the enantiomers of 2-[[4-[(7-chloro-3-iodo-4-quinolinyl)amino]pentyl]ethylamino] ethanol, (R)-3 and (S)-3, and subsequent reductive deiodination with tritium gas over 10% palladium on charcoal. (Author)

  20. Identification of a new reactive metabolite of pyrrolizidine alkaloid retrorsine: (3H-pyrrolizin-7-yl)methanol.

    Science.gov (United States)

    Fashe, Muluneh M; Juvonen, Risto O; Petsalo, Aleksanteri; Rahnasto-Rilla, Minna; Auriola, Seppo; Soininen, Pasi; Vepsäläinen, Jouko; Pasanen, Markku

    2014-11-17

    Pyrrolizidine alkaloids (PAs) such as retrorsine are common food contaminants that are known to be bioactivated by cytochrome P450 enzymes to putative hepatotoxic, genotoxic, and carcinogenic metabolites known as dehydropyrrolizidine alkaloids (DHPs). We compared how both electrochemical (EC) and human liver microsomal (HLM) oxidation of retrorsine could produce short-lived intermediate metabolites; we also characterized a toxicologically important metabolite, (3H-pyrrolizin-7-yl)methanol. The EC cell was coupled online or offline to a liquid chromatograph/mass spectrometer (LC/MS), whereas the HLM oxidation was performed in 100 mM potassium phosphate (pH 7.4) in the presence of NADPH at 37 °C. The EC cell oxidation of retrorsine produced 12 metabolites, including dehydroretrorsine (m/z 350, [M + H(+)]), which was degraded to a new reactive metabolite at m/z 136 ([M + H(+)]). The molecular structure of this small metabolite was determined using high-resolution mass spectrometry and NMR spectroscopy followed by chemical synthesis. In addition, we also identified another minor but reactive metabolite at m/z 136, an isomer of (3H-pyrrolizin-7-yl)methanol. Both (3H-pyrrolizin-7-yl)methanol and its minor isomer were also observed after HLM oxidation of retrorsine and other hepatotoxic PAs such as lasiocarpine and senkirkin. In the presence of reduced glutathione (GSH), each isomer formed identical GSH conjugates at m/z 441 and m/z 730 in the negative ESI-MS. Because (3H-pyrrolizine-7-yl)methanol) and its minor isomer subsequently reacted with GSH, it is concluded that (3H-pyrrolizin-7-yl)methanol may be a common toxic metabolite arising from PAs.

  1. Mol 7C/6; Mol 7C/6

    Energy Technology Data Exchange (ETDEWEB)

    Aberle, J.; Schleisiek, K.; Schmuck, I.; Schmidt, L.; Romer, O.; Weih, G.

    1995-08-01

    The Mol 7C/6 coolant blockage experiment in the Belgian BR2 reactor yielded results different from Mol 7C experiments with low burnup pins: At 10% burnup local failure is not self-limiting, but requires active systems for detection and scram. The Mol 7C series was finished in 1991. In each of the test bundles Mol 7C/4, /5 and /6, 30 Mk I pins pre-irradiated in KNK II were used. The central blockage consisted of enriched UO{sub 2} covering 30 percent of the bundle cross-section, with a height of 40 mm. The most important system for timely detection of coolant blockages of the type studied in Mol 7C/6 is based on DND. (orig.)

  2. Hydrolysis of R7T7 nuclear waste glass in dilute media: mechanisms and rate as a function of pH

    International Nuclear Information System (INIS)

    Advocat, T.; Vernaz, E.; Charpentier, H.; Crovisier, J.L.; Ehret, G.

    1990-01-01

    R7T7 nuclear waste glass dissolution in highly dilute aqueous media under static conditions at 90 0 C occurs according to two different mechanisms depending on the solution acidity. In acid media (pH 4.8 and 5.5), preferential extraction of glass network modifiers results in the formation of an alkali metal-depleted surface region on which amorphous and crystallized (phosphate) compounds rich in transition elements precipitate. Steady-state dissolution conditions are not reached, as attested by variable normalized Si, B and Na mass losses. Glass dissolution is stoichiometric in basic media (pH 7 to 10): the strong bonds of the silicated network are broken at a rate that increases with the pH: the glass dissolution rate increases by a factor of 15 between pH 7 and 10. Under these conditions, alteration products at the glass/solution interface do not constitute a short-term kinetic barrier against the release of the major glass components

  3. Photoluminescence and electroluminescence of a tripodal compound containing 7-diethylamino-coumarin moiety

    Energy Technology Data Exchange (ETDEWEB)

    Yu Tianzhi; Zhang Peng; Zhang Hui; Meng Jing; Fan Duowang [Key Laboratory of Opto-Electronic Technology and Intelligent Control (Lanzhou Jiaotong University), Ministry of Education, Lanzhou 730070 (China); Zhao Yuling; Dong Wenkui [School of Chemical and Biological Engineering, Lanzhou Jiaotong University, Lanzhou 730070 (China)], E-mail: ytz823@hotmail.com

    2008-12-07

    A novel tripodal compound, tris[2-(7-diethylamino-coumarin-3-carboxamide)ethyl]amine (Tren-C), was synthesized and characterized by elemental analysis, infrared and {sup 1}H-NMR spectra. The photoluminescent (PL) and electroluminescent properties of Tren-C were investigated. Tren-C exhibits different colour emissions in solid states and solutions. The electroluminescence devices comprising vacuum vapour-deposited films using the compound as a dopant were fabricated, showing blue emissions that are identical to its PL spectrum in chloroform solutions. With the device structure of indium tin oxide (ITO)/4, 4', 4''-tris-N-naphthyl-N-phenylamino-triphenylamine (2-TNATA) (5 nm)/N, N'-bis-(naphthyl)-N, N'-diphenyl-1, 1'-biphenyl-4, 4'-diamine (NPB) (40 nm)/4, 4'-bis(9-carbazolyl) biphenyl (CBP) : Tren-C (0.5 wt%, 30 nm)/2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1, 3, 4-oxadiazole (Bu-PBD) (30 nm)/LiF (1 nm)/Al (100 nm), a maximum external quantum efficiency of 2.85%, a maximum luminous efficiency of 3.85 cd A{sup -1} and a maximum luminance of 1450 cd m{sup -2} are realized.

  4. The Structure and Magnetic Properties of Pr 3MO7 with M = Nb, Ta, and Sb

    Science.gov (United States)

    Vente, J. F.; Helmholdt, R. B.; IJdo, D. J. W.

    1994-01-01

    The crystal structure of the fluorite-related praseodymium compounds with the composition Pr 3MO7, M = Nb, Ta, and Sb, have been determined using Rietveld refinement from X-ray and neutron powder diffraction data at 293 and 4 K. The structure described is orthorhombic with space group Cmcm (No. 63). It is a superstructure of the cubic fluorite structure with unit cell parameters a orth ≈ 2a c, b orth ≈ c orth ≈ a c2, as in La 3NbO 7. This structure consists of chains of corner linked MO 6 octahedra parallel with the c-axis. The magnetic susceptibility was measured between 4 and 300 K. The compounds obey the Curie-Weiss law including a Van Vleck temperature independent term. Pr 3SbO 7 shows a small deviation from this law below 25 K.

  5. 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

    Directory of Open Access Journals (Sweden)

    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.

  6. The 1:1 adduct of caffeine and 2-(1,3-dioxoisoindolin-2-ylacetic acid

    Directory of Open Access Journals (Sweden)

    Moazzam H. Bhatti

    2011-09-01

    Full Text Available In the crystal structure of the title adduct [systematic name: 2-(1,3-dioxoisoindolin-2-ylacetic acid–1,3,7-trimethyl-1,2,3,6-tetrahydro-7H-purine-2,6-dione (1/1], C8H10N4O2·C10H7NO4, the components are linked by an O—H...N hydrogen-bond and no proton transfer occurs.

  7. t-3-Benzyl-r-2,c-6-diphenylpiperidin-4-one oxime

    Directory of Open Access Journals (Sweden)

    R. Arulraj

    2016-12-01

    Full Text Available In the title compound, C24H24N2O [systematic name: (E-3-benzyl-2,6-diphenylpiperidin-4-one oxime], the piperidine ring adopts a slightly distorted chair conformation and the phenyl rings and the benzyl group substituents are attached equatorially. The oxime group makes a dihedral angle of 42.88 (12° with the piperidine ring. The dihedral angle between the phenyl rings is 71.96 (8°. The benzyl ring makes dihedral angles of 63.01 (8 and 59.35 (8° with the two phenyl rings. In the crystal, molecules are linked by O—H...N hydrogen bonds, forming C(7 chains along the c axis. The chains are linked by C—H...π interactions, forming slabs lying parallel to the bc plane.

  8. 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.

  9. Methyl 2-(1a,4a-dimethyl-2,8-dioxo-2,3,4,4a,5,6,7,8-octahydro-1aH-1-oxacyclopropa[d]naphthalen-7-ylacrylate

    Directory of Open Access Journals (Sweden)

    Mohamed Tebbaa

    2012-02-01

    Full Text Available The title compound, C16H20O5, was synthesized from ilicic acid [2-(8-hydroxy-4a,8-dimethyldecahydronaphthalen-2-ylacrylic acid], which was isolated from the chloroform extract of the aerial part of Inula viscose (L Aiton [or Dittrichia viscosa (L Greuter]. The molecule is built up from two fused six-membered rings, the epoxidized six-membered ring adopts a half-chair conformation while the other ring displays a perfect chair conformation. The crystal structure features C—H...O hydrogen bonds.

  10. 3-Phenoxymethyl-6-phenyl-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole

    Directory of Open Access Journals (Sweden)

    Shaaban K. Mohamed

    2016-04-01

    Full Text Available In the title compound, C16H12N4OS, the bicyclic triazolothiadiazole core is approximately planar, with an r.m.s. deviation of 0.018 Å. The phenyl rings are inclined to its mean plane by 7.66 (7 and 71.79 (7°. In the crystal, molecules are linked via a C—H...π interaction and a π–π interaction [intercentroid distance = 3.2942 (9 Å] involving inversion-related triazole rings. These interactions result in the formation of chains propagating along [10-1].

  11. (3-Methylbenzonitrile-1κN-cis-tetrakis(μ-N-phenylacetamidato-1:2κ4N:O;1:2κ4O:N-dirhodium(II(Rh—Rh

    Directory of Open Access Journals (Sweden)

    Cassandra T. Eagle

    2014-08-01

    Full Text Available The complex molecule of the title compound, [Rh2{N(C6H5COCH3}4(NCC7H7], has crystallographically-imposed mirror symmetry. The four acetamide ligands bridging the dirhodium core are arranged in a 2,2-cis manner with two N atoms and two O atoms coordinating to the unique RhII atom cis to one another. The Neq—Rh—Rh—Oeq torsion angles on the acetamide bridge are 0.75 (7 and 1.99 (9°. The axial nitrile ligand completes the distorted octahedral coordination sphere of one RhII atom and shows a nonlinear coordination, with an Rh—N—C bond angle of 162.8 (5°; the N—C bond length is 1.154 (7 Å.

  12. 4,5,6,7-Tetrabromo-1,1,3-trimethyl-3-(2,3,4,5-tetrabromophenylindane

    Directory of Open Access Journals (Sweden)

    Alan J. Lough

    2008-02-01

    Full Text Available The title compound (OctaInd, C18H12Br8, is a commercial brominated flame retardant (BFR. In the molecule, the five-membered ring has a slight envelope conformation, with a deviation of 0.317 (9 Å for the flap C atom from four essentially planar C atoms. The dihedral angle between the two benzene rings is 74.00 (16 Å.

  13. Ab initio/GIAO-CCSD(T) (13)C NMR study of the rearrangement and dynamic aspects of rapidly equilibrating tertiary carbocations, C6H13(+) and C7H15(+).

    Science.gov (United States)

    Olah, George A; Prakash, G K Surya; Rasul, Golam

    2016-01-05

    The rearrangement pathways of the equilibrating tertiary carbocations, 2,3-dimethyl-2-butyl cation (C6H13(+), 1), 2,3,3-trimethyl-2-butyl cation (C7H15(+), 5) and 2,3-dimethyl-2-pentyl cation (C7H15(+), 8 and 9) were investigated using the ab initio/GIAO-CCSD(T) (13)C NMR method. Comparing the calculated and experimental (13)C NMR chemical shifts of a series of carbocations indicates that excellent prediction of δ(13)C could be achieved through scaling. In the case of symmetrical equilibrating cations (1 and 5) the Wagner-Meerwein 1,2-hydride and 1,2-methide shifts, respectively, produce the same structure. This indicates that the overall (13)C NMR chemical shifts are conserved and independent of temperature. However, in the case of unsymmetrical equilibrating cations (8 and 9) the Wagner-Meerwein shift produces different tertiary structures, which have slightly different thermodynamic stabilities and, thus, different spectra. At the MP4(SDTQ)/cc-pVTZ//MP2/cc-pVTZ + ZPE level structure 8 is only 90 calories/mol more stable than structure 9. Based on computed (13)C NMR chemical shift calculations, mole fractions of these isomers were determined by assuming the observed chemical shifts are due to the weighted average of the chemical shifts of the static ions. © 2015 Wiley Periodicals, Inc.

  14. 3-(2-Fluorophenylsulfinyl-2,5,7-trimethyl-1-benzofuran

    Directory of Open Access Journals (Sweden)

    Hong Dae Choi

    2013-06-01

    Full Text Available In the title compound, C17H15FO2S, the benzofuran ring system, being essentially planar, with an r.m.s. deviation from the least-squares plane of 0.009 (2 Å, makes a dihedral angle of 79.02 (5° with the plane of the 2-fluorophenyl group. In the crystal, molecules are linked by pairs of weak C—H...O hydrogen bonds into centrosymmetric dimers.

  15. 4′,5-Dihy­droxy-7-meth­oxy­flavanone dihydrate

    Science.gov (United States)

    Brito, Iván; Bórquez, Jorge; Simirgiotis, Mario; Cárdenas, Alejandro; López-Rodríguez, Matías

    2012-01-01

    The title compound, C16H14O5·2H2O [systematic name: 5-hy­droxy-2-(4-hy­droxy­phen­yl)-7-meth­oxy­chroman-4-one dihydrate], is a natural phytoalexin flavone isolated from the native chilean species Heliotropium taltalense and crystallizes with an organic mol­ecule and two water mol­ecules in the asymmetric unit. The 5-hy­droxy group forms a strong intra­molecular hydrogen bond with the carbonyl group, resulting in a six-membered ring. In the crystal, the components are linked by O—H⋯O hydrogen bonds, forming a three-dimensional network. The 4-hy­droxy­phenyl benzene ring is bonded equatorially to the pyrone ring, which adopts a slightly distorted sofa conformation. The title compound is the hydrated form of a previously reported structure [Shoja (1990 ▶). Acta Cryst. C46, 1969–1971]. There are only slight variations in the mol­ecular geometry between the two compounds. PMID:22259537

  16. Operation and Modulation of H7 Current Source Inverter with Hybrid SiC and Si Semiconductor Switches

    DEFF Research Database (Denmark)

    Wang, Weiqi; Gao, Feng; Yang, Yongheng

    2018-01-01

    This paper proposes an H7 current source inverter (CSI) consisting of a single parallel-connected silicon carbide (SiC) switch and a traditional silicon (Si) H6 CSI. The proposed H7 CSI takes the advantages of the SiC switch to maintain high efficiency, while significantly increasing the switching...... as an all-SiC-switch converter in terms of high performance and high efficiency with reduced DC inductance. It provides a cost-effective solution to addressing the efficiency issue of conventional CSI systems. Simulations and experiments are performed to validate the effectiveness of the proposed H7 CSI...

  17. Design and syntheses of novel N-(benzothiazol-5-yl)-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-dione and N-(benzothiazol-5-yl)isoindoline-1,3-dione as potent protoporphyrinogen oxidase inhibitors.

    Science.gov (United States)

    Jiang, Li-Li; Zuo, Yang; Wang, Zhi-Fang; Tan, Yin; Wu, Qiong-You; Xi, Zhen; Yang, Guang-Fu

    2011-06-08

    Discovery of protoporphyrinogen oxidase (PPO, EC 1.3.3.4) inhibitors has been one of the hottest research areas in the field of herbicide development for many years. As a continuation of our research work on the development of new PPO-inhibiting herbicides, a series of novel N-(benzothiazol-5-yl)-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-diones (1a-p) and N-(benzothiazol-5-yl)isoindoline-1,3-diones (2a-h) were designed and synthesized according to the ring-closing strategy of two ortho-substituents. The bioassay results indicated that some newly synthesized compounds exhibited higher PPO inhibition activity than the control of sulfentrazone. Compound 1a, S-(5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl) O-methyl carbonothioate, was identified as the most potent inhibitor with k(i) value of 0.08 μM, about 9 times higher than that of sulfentrazone (k(i) = 0.72 μM). Further green house assay showed that compound 1b, methyl 2-((5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl)thio)acetate, exhibited herbicidal activity comparable to that of sulfentrazone even at a concentration of 37.5 g ai/ha. In addition, among six tested crops, wheat exhibited high tolerance to compound 1b even at a dosage of 300 g ai/ha. These results indicated that compound 1b might have the potential to be developed as a new herbicide for weed control of wheat field.

  18. 9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4H-thieno[2′,3′:4,5]pyrimidino[1,2-a]pyridin-4-one

    Directory of Open Access Journals (Sweden)

    Khusnutdin M. Shakhidoyatov

    2010-03-01

    Full Text Available The title compound, C17H16N2O2S, was obtained by condensation of 2,3-dimethylthieno[2′,3′:4,5]pyrimidino[1,2-a]pyridin-4-one with furfural in the presence of sodium hydroxide. One of the methylene groups of the tetrahydropyrido ring is disordered over two positions in a 0.87 (1:0.13 (1 ratio. The thieno[2,3-d]pyrimidin-4-one unit and the furan ring are both planar (r.m.s. deviation = 0.535 Å, and coplanar with each other, forming a dihedral angle of 5.4 (1°. Four weak intermolecular hydrogen bonds (C—H...O and C—H...N are observed in the structure, which join molecules into a network parallel to (101.

  19. Proteolytic processing of poliovirus polypeptides: antibodies to polypeptide P3-7c inhibit cleavage at glutamine-glycine pairs

    International Nuclear Information System (INIS)

    Hanecak, R.; Semler, B.L.; Anderson, C.W.; Wimmer, E.

    1982-01-01

    Proteolytic processing of poliovirus polypeptides was examined by the addition of antibodies directed against the viral proteins P3-7c and P2-X to a cell-free translation extract prepared from infected HeLa cells. Antisera to P3-7c specifically inhibited in vitro processing at Gln-Gly pairs. Partial amino acid sequence analysis revealed a second Tyr-Gly pair that is utilized in protein processing. Neither Tyr-Gly cleavage is affected by antibody to P3-7C. Anti-P3-7c antibodies react not only with P3-7c but also with P3-6a and P3-2, two viral polypeptides NH 2 -coterminal with P3-7c. Preimmune and anti-P2-X antibodies had no effect on the processing of poliovirus proteins in vitro. The authors conclude that the activity responsible for processing poliovirus polypeptides at Gln-Gly pairs resides in the primary structure of P3-7c and not in P2-X

  20. Bilateral cervical spondylolysis of C7.

    Science.gov (United States)

    Paik, Nam Chull

    2010-11-01

    Cervical spondylolysis, which is defined as a cleft between the superior and inferior articular facets of the articular pillar, is a rare condition. The sixth cervical vertebra (C6) is the level most commonly affected. Cases involving C2, C3, C4, or C5 have also been reported. However, to date, no case of C7 spondylolysis has been reported. To present a rare case of bilateral spondylolysis of the seventh cervical vertebra (C7) in a 58-year-old man. A case report. A 58-year-old man visited our hospital with chronic posterior neck pain radiating to the left upper extremity. Magnetic resonance imaging (MRI) study revealed left foraminal disc herniations at C5-C6 and C6-C7. Cervical spondylolysis involving C7 was discovered incidentally during computed tomography (CT)-guided transforaminal steroid injection. Plain radiographs, CT images, and MRIs were reviewed thoroughly once again. The patient's symptoms were relieved after he received CT-guided transforaminal steroid injections. Plain radiographs revealed a radiolucent defect in the articular pillar and cleft at the spinous process of C7. Computed tomography confirmed bilateral spondylolysis and spina bifida occulta of the C7 vertebra. Magnetic resonance imaging revealed absence of edema, which was suggestive of a chronic lesion. Involvement of C7 is not exceptional in a case of cervical spondylolysis. Copyright © 2010 Elsevier Inc. All rights reserved.

  1. 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.

  2. Synthesis and crystal structure of a new neodymium(III) selenate-selenite: Nd2(SeO4)(SeO3)2(H2O)2

    International Nuclear Information System (INIS)

    Feng Meiling; Mao Jianggao

    2005-01-01

    The title new neodymium(III) selenate-selenite was obtained by hydrothermal reactions of neodymium(III) oxide, H 2 SeO 4 and 1,10-phenanthroline at 140 o C. Its structure was established by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group C2/c with cell parameters of a = 12.258(2) A, b 7.1024(15) A, c = 13.391(3) A, β = 104.250(2) o . The structure of Nd 2 (SeO 4 )(SeO 3 ) 2 (H 2 O) 2 is isomorphous with that of Er 2 (SeO 4 )(SeO 3 ) 2 (H 2 O) 2 , which was refined in the monoclinic space group C2 with the disordered selenate group. It features an ordered 3D network with channels along b-axis. The selenate or selenite groups alone can form a 2D layer with the Nd(III) ions. IR spectrum, TGA and luminescent studies have also been performed

  3. 4-(9-Anthryl-1-(2-methoxyphenylspiro[azetidin-3,9′-xanthen]-2-one

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The stabilized conformation of the title compound, C36H25NO3, 4-(9-anthryl-1-(2-methoxyphenyl-spiro[azetidin-3,9′-xanthen]-2-one, may be compared with that of the isomeric compound 4-(9-anthryl-1-(4-methoxyphenylspiro[azetidin-3,9′-xanthen]-2-one. In the title isomer, the methoxy group is slightly twisted out of the plane of the attached benzene ring, with a C—O—C—C torsion angle of 31.5 (2°. Its β-lactam ring is essentially planar, with a maximum deviation of −0.021 (1 Å. The β-lactam ring makes dihedral angles of 18.815 (9, 83.33 (7 and 53.62 (8° with the mean planes of the benzene, xanthene and anthracene ring systems, respectively. The structure is stabilized by C—H...π, C—H...N and C—H...O interactions.

  4. Crystal structures of 2-benzylamino-4-(4-bromophenyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile and 2-benzylamino-4-(4-chlorophenyl-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile

    Directory of Open Access Journals (Sweden)

    R. A. Nagalakshmi

    2015-01-01

    Full Text Available In the title compounds, C24H22BrN3, (I, and C24H22ClN3, (II, the 2-aminopyridine ring is fused with a cycloheptane ring, which adopts a half-chair conformation. The planes of the phenyl and benzene rings are inclined to that of the central pyridine ring [r.m.s. deviations = 0.0083 (1 and 0.0093 (1 Å for (I and (II, respectively] by 62.47 (17 and 72.51 (14°, respectively, in (I, and by 71.44 (9 and 54.90 (8°, respectively, in (II. The planes of the aromatic rings are inclined to one another by 53.82 (17° in (I and by 58.04 (9° in (II. In the crystals of both (I and (II, pairs of N—H...Nnitrile hydrogen bonds link the molecules, forming inversion dimers with R22(12 ring motifs. In (I, the resulting dimers are connected through C—H...Br hydrogen bonds, forming sheets parallel to (10-1, and π–π interactions [inter-centroid distance = 3.7821 (16 Å] involving inversion-related pyridine rings, forming a three-dimensional network. In (II, the resulting dimers are connected through π–π interactions [inter-centroid distance = 3.771 (2 Å] involving inversion-related pyridine rings, forming a two-dimensional network lying parallel to (001.

  5. Barium contributions to the valence electronic structure of YBa2Cu3O7-δ, PrBa2Cu3O7-δ, and other barium-containing compounds

    International Nuclear Information System (INIS)

    Mueller, D.R.; Wallace, J.S.; Jia, J.J.; O'Brien, W.L.; Dong, Q.; Callcott, T.A.; Miyano, K.E.; Ederer, D.L.

    1995-01-01

    Monochromatic photon beams were used to excite barium N IV,V soft x-ray emission spectra from YBa 2 Cu 3 O 7-δ , PrBa 2 Cu 3 O 7-δ , BaF 2 , and BaTiO 3 . Near threshold excitation was used to demonstrate that small contributions to the barium N V and N IV emission spectra in the energy region above the 5p→4d core-core transitions do not arise as satellite emission from transitions in multiply excited atoms but rather occur as a result of transitions from the valence states. The emission spectrum of YBa 2 Cu 3 O 7-δ and PrBa 2 Cu 3 O 7-δ reveals a contribution to the electronic density of states at the barium site in the region near the Fermi level. The YBa 2 Cu 3 O 7compound is a superconductor and PrBa 2 Cu 3 O 7-δ is an insulator. It has been proposed that the difference between them is due to mixing of praseodymium and barium among the sites occupied by yttrium and barium, with an accompanying change in electronic structure. However, our measurements indicate that the barium partial density of states for the two compounds are essentially identical

  6. Intranasal immunization of baculovirus displayed hemagglutinin confers complete protection against mouse adapted highly pathogenic H7N7 reassortant influenza virus.

    Directory of Open Access Journals (Sweden)

    Subaschandrabose Rajesh Kumar

    Full Text Available BACKGROUND: Avian influenza A H7N7 virus poses a pandemic threat to human health because of its ability for direct transmission from domestic poultry to humans and from human to human. The wide zoonotic potential of H7N7 combined with an antiviral immunity inhibition similar to pandemic 1918 H1N1 and 2009 H1N1 influenza viruses is disconcerting and increases the risk of a putative H7N7 pandemic in the future, underlining the urgent need for vaccine development against this virus. METHODOLOGY/PRINCIPAL FINDINGS: In this study, we developed a recombinant vaccine by expressing the H7N7-HA protein on the surface of baculovirus (Bac-HA. The protective efficacy of the live Bac-HA vaccine construct was evaluated in a mouse model by challenging mice immunized intranasally (i.n. or subcutaneously (s.c. with high pathogenic mouse adapted H7N7 reassorted strain. Although s.c. injection of live Bac-HA induced higher specific IgG than i.n. immunization, the later resulted in an elevated neutralization titer. Interestingly, 100% protection from the lethal viral challenge was only observed for the mice immunized intranasally with live Bac-HA, whereas no protection was achieved in any other s.c. or i.n. immunized mice groups. In addition, we also observed higher mucosal IgA as well as increased IFN-γ and IL-4 responses in the splenocytes of the surviving mice coupled with a reduced viral titer and diminished histopathological signs in the lungs. CONCLUSION: Our results indicated that protection from high pathogenic H7N7 (NL/219/03 virus requires both mucosal and systemic immune responses in mice. The balance between Th1 and Th2 cytokines is also required for the protection against the H7N7 pathogen. Intranasal administration of live Bac-HA induced all these immune responses and protected the mice from lethal viral challenge. Therefore, live Bac-HA is an effective vaccine candidate against H7N7 viral infections.

  7. 7 CFR 370.3 - Index.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 5 2010-01-01 2010-01-01 false Index. 370.3 Section 370.3 Agriculture Regulations of... AGRICULTURE FREEDOM OF INFORMATION § 370.3 Index. Pursuant to the regulations in § 1.4(b) of this title, APHIS will maintain and make available for public inspection and copying a current index providing...

  8. CeNi{sub 3}-type rare earth compounds: crystal structure of R{sub 3}Co{sub 7}Al{sub 2} (R=Y, Gd–Tm) and magnetic properties of {Gd–Er}{sub 3}Co{sub 7}Al{sub 2}, {Tb, Dy}{sub 3}Ni{sub 8}Si and Dy{sub 3}Co{sub 7.68}Si{sub 1.32}

    Energy Technology Data Exchange (ETDEWEB)

    Morozkin, A.V., E-mail: morozkin@tech.chem.msu.ru [Department of Chemistry, Moscow State University, Leninskie Gory, House 1, Building 3, GSP-1, Moscow 119991 (Russian Federation); Yapaskurt, V.O. [Department of Petrology, Geological Faculty Moscow State University, Leninskie Gory, Moscow 119991 (Russian Federation); Nirmala, R. [Indian Institute of Technology Madras, Chennai 600 036 (India); Quezado, S.; Malik, S.K. [Departamento de Física Teórica e Experimental, Universidade Federal do Rio Grande do Norte, Natal 59082-970 (Brazil)

    2017-03-15

    The crystal structure of new CeNi{sub 3}-type {Y, Gd–Tm}{sub 3}Co{sub 7}Al{sub 2} (P63/mmc. N 194, hP24) compounds has been established using powder X-ray diffraction studies. The magnetism of Tb{sub 3}Ni{sub 8}Si and Dy{sub 3}Ni{sub 8}Si is dominated by rare earth sublattice and the magnetic properties of R{sub 3}Co{sub 7}Al{sub 2} (R =Gd–Er) and Dy{sub 3}Co{sub 7.68}Si{sub 1.32} are determined by both rare earth and cobalt sublattices. Magnetization data indicate ferromagnetic ordering of {Tb, Dy}{sub 3}Ni{sub 8}Si at 32 K and 21 K, respectively. Gd{sub 3}Co{sub 7}Al{sub 2} and Tb{sub 3}Co{sub 7}Al{sub 2} exhibit ferromagnetic ordering at 309 K and 209 K, respectively, whereas Dy{sub 3}Co{sub 7}Al{sub 2}, Ho{sub 3}Co{sub 7}Al{sub 2}, Er{sub 3}Co{sub 7}Al{sub 2} and Dy{sub 3}Co{sub 7.68}Si{sub 1.32} show a field dependent ferromagnetic-like ordering at 166 K, 124 K, 84 K and 226 K, respectively followed by a low temperature transition at 34 K for Dy{sub 3}Co{sub 7}Al{sub 2}, 18 K for Ho{sub 3}Co{sub 7}Al{sub 2}, 56 K for Er{sub 3}Co{sub 7}Al{sub 2}, 155 K and 42 K for Dy{sub 3}Co{sub 7.68}Si{sub 1.32}. Among these compounds, Dy{sub 3}Ni{sub 8}Si shows largest magnetocaloric effect (isothermal magnetic entropy change) of −11.6 J/kg·K at 18 K in field change of 50 kOe, whereas Tb{sub 3}Co{sub 7}Al{sub 2}, Dy{sub 3}Co{sub 7}Al{sub 2} and Dy{sub 3}Co{sub 7.68}Si{sub 1.32} exhibit best permanent magnet properties in the temperature range of 2–5 K with remanent magnetization of 11.95 μ{sub B}/fu, 12.86 μ{sub B}/fu and 14.4 μ{sub B}/fu, respectively and coercive field of 3.0 kOe, 1.9 kOe and 4.4 kOe, respectively. - Highlights: • {Y, Gd–Tm}{sub 3}Co{sub 7}Al{sub 2} compounds crystallize in the CeNi{sub 3}-type structure. • {Gd-Er}{sub 3}Co{sub 7}Al{sub 2} show ferrimagnetic ordering at 309 K, 209 K, 166 K, 124 K and 84 K. • Dy{sub 3}Co{sub 7.68}Si{sub 1.32} exhibits magnetic transitions at 226 K, 155 K and 42 K. • {Tb-Er}{sub 3}Co{sub 7}Al{sub 2

  9. 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].

  10. (R,S-2′-Amino-6′-methyl-2,5′,5′-trioxo-6′H-spiro[indoline-3,4′-pyrano[3,2-c][2,1]benzothiazine]-3′-carbonitrile dimethylformamide monosolvate

    Directory of Open Access Journals (Sweden)

    Svitlana V. Shishkina

    2014-07-01

    Full Text Available The title solvate, C20H14N4O4S·C3H7NO, comprises a stereogenic centre but the centrosymmetric space group causes the presence of the racemate in the crystal. The spiro-joined fragments are almost orthogonal, with a dihedral angle of 86.8 (2° between the mean planes of the pyrane ring and the dihydroindolone ring system. The atoms of the indolinone bicycle are coplanar, with an r.m.s. deviation of 0.005 Å. In the crystal, pairs of N—H...O hydrogen bonds link the molecules into centrosymmetric dimers which are linked to the dimethylformamide solvent molecules by further N—H...O hydrogen bonds. N—H...N hydrogen bonds link neighbouring dimers into [010] chains.

  11. Synthesis, Crystal Structure, DFT Study and Antifungal Activity of 4-(5-((4-Bromobenzyl thio-4-Phenyl-4H-1,2,4-Triazol-3-ylpyridine

    Directory of Open Access Journals (Sweden)

    Jin-Xia Mu

    2015-12-01

    Full Text Available The title compound 4-(5-((4-bromobenzylthio-4-phenyl-4H-1,2,4-triazol-3-ylpyridine (C20H15BrN4S was synthesized, and its structure was confirmed by 1H NMR, MS and elemental analyses and single-crystal X-ray structure determination. It crystallizes in the triclinic space group P-1 with a = 7.717(3, b = 9.210(3, c = 13.370(5 Å, α = 80.347(13, β = 77.471(13, γ = 89.899(16°, V = 913.9(6 Å3, Z = 2 and R = 0.0260 for 3145 observed reflections with I > 2σ(I. A Density functional theory (DFT (B3LYP/6-31G calculation of the title molecule was carried out. The full geometry optimization was carried out using a 6-31G basis set, and the frontier orbital energy. Atomic net charges are discussed. Calculated bond lengths and bond angles were found to differ from experimental values, and the compound exhibits moderate antifungal activity.

  12. Persistence of Escherichia coli O157:H7 in dairy fermentation systems.

    Science.gov (United States)

    Dineen, S S; Takeuchi, K; Soudah, J E; Boor, K J

    1998-12-01

    We examined (i) the persistence of Escherichia coli O157:H7 as a postpasteurization contaminant in fermented dairy products; (ii) the ability of E. coli O157:H7 strains with and without the general stress regulatory protein, RpoS, to compete with commercial starter cultures in fermentation systems; and (iii) the survival of E. coli O157:H7 in the yogurt production process. In commercial products inoculated with 10(3) CFU/ml, E. coli O157:H7 was recovered for up to 12 days in yogurt (pH 4.0), 28 days in sour cream (pH 4.3), and at levels > 10(2) CFU/ml at 35 days in buttermilk (pH 4.1). For the starter culture competition trials, the relative inhibition of E. coli O157:H7 in the experimental fermentation systems was, in decreasing order, thermophilic culture mixture, Lactobacillus delbrueckii subsp. bulgaricus R110 alone, Lactococcus lactis subsp. lactis D280 alone, Lactococcus lactis subsp. cremoris D62 alone, and Streptococcus thermophilus C90 alone showing the least inhibition. Recovery of the rpoS mutant was lower than recovery of its wild-type parent by 72 h or earlier in the presence of individual starter cultures. No E. coli O157:H7 were recovered after the curd formation step in yogurt manufactured with milk inoculated with 10(5) CFU/ml. Our results show that (i) postprocessing entry of E. coli O157:H7 into fermented dairy products represents a potential health hazard; (ii) commercial starter cultures differ in their ability to reduce E. coli O157:H7 CFU numbers in fermentation systems; and (iii) the RpoS protein appears to most effectively contribute to bacterial survival in the presence of conditions that are moderately lethal to the cell.

  13. Construction of Six Coordination Polymers Based on a 5,5′-(1,2-Ethynyl)bis-1,3-benzenedicarboxylic Ligand: Synthesis, Structure, Gas Sorption, and Magnetic Properties

    KAUST Repository

    Zheng, Bing

    2013-03-06

    Six novel coordination polymers based on a multifunctional ligand, 5,5\\'-(1,2-ethynyl)bis-1,3-benzenedicarboxylic (H4EBDC), namely, |(C3H7NO)2(H2O)7(C 2H5OH)3| [Zn2(C18H 6O8)(C10H8N2) 2] (1), |(C3H7NO)3(H2O)30- (CH3CN)2|[Zn 6(C18H6O8)3(C 6H12N2O2)2] (2), |(C 3H7NO)2- (H2O)2(H 3O)2|[Cd3(C18H6O 8)2] (3), |(C3H7NO)|[Mn- (C 18H8O8)(C3H7NO) 2] (4), |(C3H7NO)2(H2O)(C 2H7N)3| [Mn6(C18H 7O8)4(H2O)8] (5), and [Mn2(C18H6O8)(C3H 7NO)2] (6), have been constructed under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction. In these compounds, the ligand, H4EBDC, exhibits different coordination modes and conformations, constructing various architectures by bridging a variety of metal ions or polynuclear clusters. Compound 1 forms a three-dimensional (3D) FSC network constructed from two-dimensional (2D) layer motifs joined by EBDC4- and 4,4\\'-bipyridine bridges. Compound 2 possesses an NbO topology by linking Zn2(CO2)4 units with the ligand, coordinated amine molecules fill the pores, while compound 3 exhibits a 3D FLU network with Cd2+ as the cation and features an infinite framework built from tricadmium clusters. Compound 4 is based on PtS net, constructed of 4-connected rectangular H4EBDC units with tetrahedral monometallic Mn(CO2)4 nodes. Compound 5 is composed of 2D layers with (3,6)-connected KGD topology, and compound 6 consists of a 3D PtS-X network, built by bridging a metal chain with the ligand. The structures of these compounds have been discussed together with their corresponding properties, such as gas storage, separation, and magnetic properties. © 2013 American Chemical Society.

  14. Ethyl 3-[7-eth­oxy-6-(4-meth­oxy­benzene­sulfonamido)-2H-indazol-2-yl]propano­ate

    Science.gov (United States)

    Abbassi, Najat; Oulemda, Bassou; Rakib, El Mostapha; Geffken, Detlef; Zouihri, Hafid

    2012-01-01

    In the title compound, C21H25N3O6S, the dihedral angle between the meth­oxy­benzene and indazole rings is 74.96 (5)°. The crystal packing is stabilized by an N—H⋯O hydrogen bond into a two-dimensional network. In addition, C—H⋯π inter­actions and a π–π contact, with a centroid–centroid distance of 3.5333 (6) Å, are observed. The crystal packing is stabilized by N—H⋯O and C—H⋯O hydrogen bonds. PMID:22589994

  15. Synthesis of both sup 14 C- and sup 3 H- labelled trospectomycin and the assessment of their utility in biological studies

    Energy Technology Data Exchange (ETDEWEB)

    Constable, D A; Dring, L G [Upjohn Ltd., Crawley (UK); Jones, J R [Surrey Univ., Guildford (UK). Dept. of Chemistry

    1990-07-01

    Three radiolabelled forms of trospectomycin (6'-n-propylspectinomycin sulphate hydrate) have been synthesised, namely (8'-{sup 14}C)-, (6',7'-{sup 3}H)-, and (5',6',7'-{sup 3}H)-trospectomycin. Although all three forms of the drug are metabolically stable and therefore suitable for use in animal studies the {sup 14}C compound is produced in poor yield as is the (6',7'-{sup 3}H)trospectomycin. On the other hand, the (5',6',7'-{sup 3}H)-form is produced in good yield and appears to be the labelled form of choice. Following subcutaneous administration of any of the labelled forms to rats, more than 50% of the dose was excreted in the urine as unchanged drug during the first 6h after dosing. Approximately 80% and 10% of the dose appeared in the urine and faeces respectively after 6 days. (author).

  16. 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.

  17. Poly[tetraaqua-μ3-pyridine-3,5-dicarboxylato-strontium(II

    Directory of Open Access Journals (Sweden)

    Shirin Daneshvar

    2008-02-01

    Full Text Available The reaction of strontium(II nitrate with the proton-transfer compound (pdaH2(py-3,5-dc·H2O (where pda = propane-1,3-diamine and py-3,5-dcH2 = pyridine-3,5-dicarboxylic acid leads to the formation of the title polymeric compound, [Sr(C7H3NO4(H2O4]n. The propane-1,3-diaminium cation is not incorporated in this crystal structure. The SrII atom lies on an inversion centre and is eight-coordinated by four O atoms from three py-3,5-dc ligands and four O atoms from four coordinated water molecules. The coordination polyhedron of the SrII atom is a distorted dodecahedron. These binuclear units are connected via the carboxylate O atoms to build a one-dimensional polymeric chain. In the crystal structure, non-covalant interactions consisting of hydrogen bonds (X—H...O, with X = O and C and π–π stacking interactions [3.4604 (19 Å] connect the various components to form a supramolecular structure.

  18. 3-Chloro-4-methyl­quinolin-2(1H)-one

    Science.gov (United States)

    Kassem, Mohamed G.; Ghabbour, Hazem A.; Abdel-Aziz, Hatem A.; Fun, Hoong-Kun; Ooi, Chin Wei

    2012-01-01

    The title compound, C10H8ClNO, is almost planar (r.m.s. deviation for the 13 non-H atoms = 0.023 Å). In the crystal, inversion dimers linked by pairs of N—H⋯O hydrogen bonds generate R 2 2(8) rings. Weak aromatic π–π stacking inter­actions [centroid–centroid distance = 3.7622 (12) Å] also occur. PMID:22589913

  19. 10a-Hydroxy-9-(4-methoxyphenyl-3,4,5,6,7,8a,9,10a-octahydro-1H-xanthene-1,8(2H-dione

    Directory of Open Access Journals (Sweden)

    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.

  20. Crystal structure of 1,3-bis(4-hexyl-5-iodothiophen-2-yl-4,5,6,7-tetrahydro-2-benzothiophene

    Directory of Open Access Journals (Sweden)

    Julian Linshoeft

    2014-10-01

    Full Text Available In the crystal structure of the title compound, C28H36I2S3, a terthiophene monomer, the central thiophene unit is arranged anti-coplanar to the two outer thiophene rings. There are two crystallographically independent molecules in the asymmetric unit, which show different conformations. In one molecule, the dihedral angles between the inner and the two outer thiophene rings are 15.7 (3 and 3.47 (3°, whereas these values are 4.2 (3 and 11.3 (3° for the second molecule. Differences are also found in the arrangement of the hexyl chains: in one of the two molecules, both chains are nearly in plane to the central moiety, whereas in the second molecule, only one chain is in plane and the other one is nearly perpendicular to the central moiety. Some of the C atoms are disordered and were refined using a split model with occupancy ratios of 0.65:0.35 and 0.70:0.30 in the two molecules.

  1. Survival of Escherichia coli O157:H7 in needle-tenderized dry cured Westphalian ham.

    Science.gov (United States)

    Graumann, Gary H; Holley, Richard A

    2007-09-15

    Westphalian ham is a dry cured, ready-to-eat product that is manufactured without a lethal heat treatment. Hams are preserved by a process that involves curing, fermenting, smoking and drying, which may take 3 months or more to complete. The process can be accelerated by tenderizing the meat with solid needles, to increase the rate of cure-salt diffusion throughout muscle tissues. In this study, intact hams were immersed in a solution containing a five strain cocktail of Escherichia coli O157:H7 at 8 log cfu/mL, to determine whether needle treatment before cure application would internalize organisms from the surface. In two trials, the survival of E. coli O157:H7 on external surfaces and within deep tissues after needle treatment was followed during the ripening of hams. The injured E. coli O157:H7 cells were recovered by plating samples on pre-poured Tryptic Soy Agar plates which were incubated for 3 to 4 h at 35 degrees C, overlaid with Sorbitol MacConkey Agar containing cefixime and tellurite and re-incubated at 35 degrees C for 48 to 72 h. Inoculated-injected hams initially carried E. coli O157:H7 at numbers of 7.3 and 4.6 log cfu/g E. coli O157:H7 on the surface and inside, respectively. After 112 d of ripening, which included 79 d of drying, no E. coli O157:H7 were detected at the surface of hams following enrichment, whereas in deep tissue the organism was recovered at numbers of 3.1 log cfu/g. The Westphalian ham ripening procedure evidently was not adequate to eliminate E. coli O157:H7 internalized by needle tenderization.

  2. Crystal and molecular structure of 8-acetoxy-7-aza-6-ethoxycarbonyl-7-formyl-3,4-dihydroxy-3,4-O-isopropylidene-2-oxabicyclo [3.30]octane

    International Nuclear Information System (INIS)

    Holzapfel, C.W.; Koekemoer, J.M.; Kruger, G.J.; Van Dyk, M.S.

    1985-01-01

    The structure and stereochemistry of the title compound, a 11-deoxy-11-azaprostaglandin synthon, has been determined by single-crystal X-ray diffraction methods. The dioxolane and aza-rings are cis-fused on the same side to the central furanose ring. Both the ethoxycarbonyl group on C(5) and the acetoxy-group on C(6) have a β-configuration. The conformation of the solid state structure is compared with that in chloroform solution, as evidenced by 1 H n.m.r. studies

  3. The human polynucleotide kinase/phosphatase (hPNKP) inhibitor A12B4C3 radiosensitizes human myeloid leukemia cells to Auger electron-emitting anti-CD123 111In-NLS-7G3 radioimmunoconjugates

    International Nuclear Information System (INIS)

    Zereshkian, Arman; Leyton, Jeffrey V.; Cai, Zhongli; Bergstrom, Dane; Weinfeld, Michael; Reilly, Raymond M.

    2014-01-01

    Introduction: Leukemia stem cells (LSCs) are believed to be responsible for initiating and propagating acute myeloid leukemia (AML) and for causing relapse after treatment. Radioimmunotherapy (RIT) targeting these cells may improve the treatment of AML, but is limited by the low density of target epitopes. Our objective was to study a human polynucleotide kinase/phosphatase (hPNKP) inhibitor that interferes with DNA repair as a radiosensitizer for the Auger electron RIT agent, 111 In-NLS-7G3, which recognizes the CD123 + /CD131 - phenotype uniquely displayed by LSCs. Methods: The surviving fraction (SF) of CD123 + /CD131 - AML-5 cells exposed to 111 In-NLS-7G3 (33–266 nmols/L; 0.74 MBq/μg) or to γ-radiation (0.25-5 Gy) was determined by clonogenic assays. The effect of A12B4C3 (25 μmols/L) combined with 111 In-NLS-7G3 (16–66 nmols/L) or with γ-radiation (0.25–2 Gy) on the SF of AML-5 cells was assessed. The density of DNA double-strand breaks (DSBs) in the nucleus was measured using the γ-H2AX assay. Cellular dosimetry was estimated based on the subcellular distribution of 111 In-NLS-7G3 measured by cell fractionation. Results: Binding of 111 In-NLS-7G3 to AML-5 cells was reduced by 2.2-fold in the presence of an excess (1 μM) of unlabeled NLS-7G3, demonstrating specific binding to the CD123 + /CD131 - epitope. 111 In-NLS-7G3 reduced the SF of AML-5 cells from 86.1 ± 11.0% at 33 nmols/L to 10.5 ± 3.6% at 266 nmols/L. Unlabeled NLS-7G3 had no significant effect on the SF. Treatment of AML-5 cells with γ-radiation reduced the SF from 98.9 ± 14.9% at 0.25 Gy to 0.03 ± 0.1% at 5 Gy. A12B4C3 combined with 111 In-NLS-7G3 (16–66 nmols/L) enhanced the cytotoxicity up to 1.7-fold compared to treatment with radioimmunoconjugates alone and was associated with a 1.6-fold increase in DNA DSBs in the nucleus. A12B4C3 enhanced the cytotoxicity of γ-radiation (0.25–0.5 Gy) on AML-5 cells by up to 1.5-fold, and DNA DSBs were increased by 1.7-fold. Exposure to

  4. 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.

  5. (E-N′-[(E-3-(4-Hydroxy-3-methoxyphenylallylidene]isonicotinohydrazide

    Directory of Open Access Journals (Sweden)

    H. S. Naveenkumar

    2010-02-01

    Full Text Available In the title compound, C16H15N3O3, the dihedral angle between the pyridine and benzene rings is 7.66 (5°. The crystal packing is consolidated by intermolecular C—H...O and O—H...N interactions, which link the molecules into zigzag chains propagating along [010]. The chains are further linked into a three-dimensional network by N—H...O, C—H...N, C—H...O and C—H...π interactions.

  6. N-(2-Carboxyethyl-2,5-dideoxy-2,5-imino-d-mannonic acid [(3R,4R,5R-1-(2-carboxyethyl-3,4-dihydroxy-5-hydroxymethyl-l-proline

    Directory of Open Access Journals (Sweden)

    David S. Edgeley

    2012-10-01

    Full Text Available The absolute stereochemistry of the title compound, C9H15NO7, was determined from the use of d-glucuronolactone as the starting material. The compound crystallizes as the zwitterion. The five-membered ring adopts an envelope conformation with the –CH2OH-substituted C atom forming the flap. An intramolecular N—H...O hydrogen-bond occurs. In the crystal, the compound exists as a three-dimensional O—H...O intermolecular hydrogen-bonded network with each molecule acting as a donor and acceptor for four hydrogen bonds.

  7. Poly[diaqua(μ5-pyridine-3,5-dicarboxylatostrontium

    Directory of Open Access Journals (Sweden)

    Dan Li

    2012-06-01

    Full Text Available In the structure of the title compound, [Sr(C7H3NO4(H2O2]n, the SrII cation is eight-coordinated in form of a distorted dodecahedron by two water O atoms and by five O atoms and one N atom from five pyridine-3,5-dicarboxylate anions. The bridging mode of the anions leads to the formation of a layered network parallel to (100. O—H...O hydrogen bonding between the coordinating water molecules and the carboxylate groups of adjacent layers consolidates the crystal packing. Weak C—H...O interactions are also observed.

  8. (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

    Directory of Open Access Journals (Sweden)

    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.

  9. Diastereoselective Synthesis of 5-Hydroxy-8-methoxy-1-oxaspiro[5,5]undeca-7,10-diene-9-one

    Directory of Open Access Journals (Sweden)

    Thomas W. Scully

    2013-01-01

    Full Text Available A short five steps synthesis of the title compound from vanillin is described. The racemic spiroether 7 was obtained in 61% yield and in >99% diastereomeric excess (by 1H-NMR from the corresponding phenolic derivative 3 by oxidation with lead (IV acetate.

  10. Synthesis of 3-(4, 5-dihydro-1-phenyl-5-substituted phenyl-1H-pyrazol-3-yl-2H-chromen-2-one derivatives and evaluation of their anticancer activity

    Directory of Open Access Journals (Sweden)

    Nitin Kumar

    2017-05-01

    Full Text Available A novel series of 3-(4, 5-dihydro-1-phenyl-5-substituted phenyl-1H-pyrazol-3-yl-2H-chromen-2-one derivatives were synthesized. In the first step salicylaldehyde was reacted with ethylacetoacetate at room temperature by stirring which gives compound (I. Compound (I when refluxed with substituted benzaldehyde and diethylamine in the presence of n-butanol for 4–5 h gives substituted derivatives (IIa–d. Compounds synthesized in step 2 when refluxed with phenyl hydrazine in the presence of pyridine for 6–7 h gives the title compounds (IIIa–d. All the synthesized compounds were sent to NCI for anticancer activity. Synthesized compounds were tested for anticancer activity against 60 different cell lines. From the data thus obtained it was observed that simple coumarin ring derivatives were more effective in inhibiting the growth of cancerous cell lines, than coumarin-pyrazoline derivatives. Among all the synthesized compounds, irrespective of compounds having simple coumarin ring and coumarin-pyrazoline combination, compounds IIa–c, IIIb and IIId were potent anticancer agents. Compounds were active for the single dose therapeutic program at the dose of 1.00E-5 molar concentration. The main anti cancer activity is assumed to be due to the presence of the lactone structure in coumarin moiety.

  11. 1,4-Dihydroxyquinoxaline-2,3(1H,4H-dione

    Directory of Open Access Journals (Sweden)

    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.

  12. Crystal structure of rac-3-[2,3-bis(phenylsulfanyl-3H-indol-3-yl]propanoic acid

    Directory of Open Access Journals (Sweden)

    Wayland E. Noland

    2015-11-01

    Full Text Available The title compound, C23H19NO2S2, was obtained as an unexpected regioisomer from an attempted synthesis of an intermediate for a substituent-effect study on ergot alkaloids. This is the first report of a 1H-indole monothioating at the 2- and 3-positions to give a 3H-indole. In the crystal, the acid H atom is twisted roughly 180° from the typical carboxy conformation and forms centrosymmetric O—H...N hydrogen-bonded dimers with the indole N atom of an inversion-related molecule. Together with a weak C—H...O hydrogen bond involving the carbonyl O atom, chains are formed along [100].

  13. Selective labelling of 5-HT7 receptor recognition sites in rat brain using [3H]5-carboxamidotryptamine

    International Nuclear Information System (INIS)

    Stowe, R.L.; Barnes, N.M.

    1998-01-01

    The aim of the present study was to establish a radioligand binding assay to selectively label the native 5-HT 7 receptor expressed in rat brain. In rat whole brain (minus cerebellum and striatum) homogenate, (±)-pindolol (10 μM)-insensitive [ 3 H]5-CT ([ 3 H]5-carboxamidotryptamine; 0.5 nM) specific binding (defined by 5-HT, 10 μM) displayed a pharmacological profile similar to the recombinant 5-HT 7 receptor, although the Hill coefficients for competition curves generated by methiothepin, ritanserin, sumatriptan, clozapine and pimozide were significantly less than unity. In homogenates of rat hypothalamus, (±)-pindolol (10 μM)-insensitive [ 3 H]5-CT recognition sites also resembled, pharmacologically, the 5-HT 7 receptor, although pimozide still generated Hill coefficients significantly less than unity. Subsequent studies were performed in the additional presence of WAY100635 (100 nM) to prevent [ 3 H]5-CT binding to residual, possibly, 5-HT 1A sites. Competition for this [ 3 H]5-CT binding indicated the labelling in whole rat brain homogenate of a homogenous population of sites with the pharmacological profile of the 5-HT 7 receptor. Saturation studies also indicated that (±)-pindolol (10 μM)/WAY 100635 (100 nM)-insensitive [ 3 H]5-CT binding to homogenates of whole rat brain was saturable and to an apparently homogenous population of sites which were labelled with nanomolar affinity (B max =33.2±0.7 fmol mg -1 protein, pK d =8.78±0.05, mean±S.E.M., n=3). The development of this 5-HT 7 receptor binding assay will aid investigation of the rat native 5-HT 7 receptor. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  14. 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.

  15. Simple and Efficient One-Pot Synthesis, Spectroscopic Characterization and Crystal Structure of Methyl 5-(4-Chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Imtiaz Khan

    2012-07-01

    Full Text Available A facile one-pot synthesis of methyl 5-(4-chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate (4 is described. The title compound was efficiently synthesized by the reaction of phenyl hydrazine, dimethyl acetylenedicarboxylate and 4-chlorobenzoyl chloride in dichloromethane under reflux in good yield. The structure of the target compound was deduced by modern spectroscopic and analytical techniques and unequivocally confirmed by a single crystal X-ray diffraction analysis. The crystal of the title compound belongs to orthorhombic system, space group P 21 21 21 with cell parameters a = 6.6491(3 Å, b = 7.9627(6 Å, c = 30.621(5 Å, α = β = γ = 90° and Z = 4. The crystal packing of the compound (4 is stabilized by an offset π-stacking between the planar benzoyl-substituted diazole moieties.

  16. Cluster model of A=7 nuclei revisited, and the astrophysical S factors for 3 He(α, γ)7 Be and 3 H(α, γ)7 Li at zero energy

    International Nuclear Information System (INIS)

    Buck, B.; Merchant, A.C.

    1988-10-01

    A elementary cluster model that visualizes an alpha particle interacting with a 3 H of 3 He cluster via a local potential is employed. An assurance is made that the major requirements of the Pauli principle are satisfied by choosing relative motion quantum numbers N (Principal Quantum Number) and L to correspond to the microscopic situation in which the 3 H or 3 He nucleons occupy shell-model orbitals above the (O ) - orbitals filled by the alpha particles. The S o factor for the capture reactions 3 He (α,γ) 7 Be and 3 H (α,γ) 7 Li is calculated by considering only electric dipole capture from incident s-waves as follows. (author)

  17. Two different one-dimensional structural motifs in [catena-{Cu(tacn)}2Pd(CN)4]Br2.[catena-Cu(tacn)Pd(CN)4]2.H2O (tacn is 1,4,7-triazacyclononane).

    Science.gov (United States)

    Kuchár, Juraj; Cernák, Juraj

    2009-07-01

    The title compound, catena-poly[[bis[(triazacyclononane-kappa(3)N,N',N'')copper(II)]-di-mu-cyanido-kappa(4)N:C-palladate(II)-di-mu-cyanido-kappa(4)C:N] dibromide bis[[(triazacyclononane-kappa(3)N,N',N'')copper(II)]-mu-cyanido-kappa(2)N:C-[dicyanidopalladate(II)]-mu-cyanido-kappa(2)C:N] monohydrate], {[Cu(2)Pd(CN)(4)(C(6)H(15)N(3))(2)]Br(2).[Cu(2)Pd(2)(CN)(8)(C(6)H(15)N(3))(2)].H(2)O}(n), (I), was isolated from an aqueous solution containing tacn.3HBr (tacn is 1,4,7-triazacyclononane), Cu(2+) and tetracyanidopalladate(2-) anions. The crystal structure of (I) is essentially ionic and built up of 2,2-electroneutral chains, viz. [Cu(tacn)(NC)-Pd(CN)(2)-(CN)-], positively charged 2,4-ribbons exhibiting the composition {[Cu(tacn)(NC)(2)-Pd(CN)(2)-Cu(tacn)](2n+)}(n), bromide anions and one disordered water molecule of crystallization. The O atom of the water molecule occupies two unique crystallographic positions, one on a centre of symmetry, which is half occupied, and the other in a general position with one-quarter occupancy. One of the tacn ligands also exhibits disorder. The formation of two different types of one-dimensional structural motif within the same structure is a unique feature of this compound.

  18. A novel inorganic-organic compound: Synthesis and structural characterization of tin(II) phenylbis(phosphonate), Sn2(PO3C6H4PO3)

    International Nuclear Information System (INIS)

    Subbiah, Ayyappan; Bhuvanesh, Nattamai; Clearfield, Abraham

    2005-01-01

    A novel tin(II) phenylbis(phosphonate) compound has been synthesized hydrothermally and its structure has been determined by single crystal X-ray diffraction. The structure is monoclinic, space group P2 1 /c (no. 14), a=4.8094(4), b=16.2871(13), c=6.9107(6)A; β=106.292(6) o , V=519.59(7)A 3 , Z=2. The three-dimensional structure consists of 3-coordinated tin and 4-coordinated phosphorus double layers separated (pillared) by phenyl rings. These phenyl rings are placed 4.8A apart along the a-axis in the structure resulting in lower surface area (∼14m 2 /g). The porosity has been increased by replacing phenyl groups by methyl groups (∼31m 2 /g)

  19. Crystal structure of 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl) ethenyl]benzamide: N,N-dimethylformamide (1 : 1)

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, P. [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India); Subbulakshmi, K. N.; Narayana, B. [Mangalore University, Department of Chemistry (India); Sarojini, B. K. [Mangalore University, Industrial Chemistry Division, Department of Studies in Chemistry (India); Kant, R., E-mail: rkant.ju@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India)

    2016-03-15

    The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C{sub 15}H{sub 11}N{sub 3}O{sub 2}S{sub 2} · C{sub 3}H{sub 7}NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.

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

    Directory of Open Access Journals (Sweden)

    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.

  1. Phase diagram of multiferroic KCu3As2O7(OD ) 3

    Science.gov (United States)

    Nilsen, Gøran J.; Simonet, Virginie; Colin, Claire V.; Okuma, Ryutaro; Okamoto, Yoshihiko; Tokunaga, Masashi; Hansen, Thomas C.; Khalyavin, Dmitry D.; Hiroi, Zenji

    2017-06-01

    The layered compound KCu3As2O7(OD ) 3 , comprising distorted kagome planes of S =1 /2 Cu2 + ions, is a recent addition to the family of type-II multiferroics. Previous zero-field neutron diffraction work has found two helically ordered regimes in KCu3As2O7(OD ) 3 , each showing a distinct coupling between the magnetic and ferroelectric order parameters. Here, we extend this work to magnetic fields up to 20 T using neutron powder diffraction, capacitance, polarization, and high-field magnetization measurements, hence determining the H -T phase diagram. We find metamagnetic transitions in both low-temperature phases around μ0Hc˜3.7 T, which neutron powder diffraction reveals to correspond to rotations of the helix plane away from the easy plane, as well as a small change in the propagation vector. Furthermore, we show that the sign of the ferroelectric polarization is reversible in a magnetic field, although no change is observed (or expected on the basis of the magnetic structure) due to the transition at 3.7 T. We finally justify the temperature dependence of the polarization in both zero-field ordered phases by a symmetry analysis of the free energy expansion, and attempt to account for the metamagnetic transition by adding anisotropic exchange interactions to our existing model for KCu3As2O7(OD ) 3 .

  2. Reactions of recoil tritium generated by the 3He(n,p)3H reaction with aromatic compounds -intramolecular tritium distribution and radiochemical yield

    International Nuclear Information System (INIS)

    Nogawa, N.; Morikawa, Naotake; Oohashi, Kunio; Matuoka, H.; Moki, T.; Moriya, T.

    1986-01-01

    Reactions of recoil tritium with benzoic acid, acetanilide and β-phenethyl alcohol were studied using the 3 He(=n,p) 3 H reaction. The tritium distribution in the aromatic ring is approximately uniform in all the irradiated compounds and the tritium activity per C-H bond in the methyl and ethylene groups is 7 to 8 relative to that of the corresponding ring as standard. These findings are substantially the same as those obtained previously by the 6 Li(n,α) 3 H reactions, suggesting the same mechanism of tritiation for both recoil reactions. The tritiated parent compounds were obtained in high radiochemical yields: 45% for benzoic acid, 30% for acetanilide, 12% for β-phenethyl alcohol. (author)

  3. Antitumor properties of (5E,7E) analogs of vitamin D3.

    Science.gov (United States)

    Filip, B; Milczarek, M; Wietrzyk, J; Chodyński, M; Kutner, A

    2010-07-01

    Geometric isomers (5E,7E) of major active metabolites of vitamin D3 [1alpha,25(OH)2D3 and (24R)-1,24(OH)2D3] were synthesized by a new convenient procedure. Vitamin D triene system of the metabolites was first derivatized as a Diels-Alder adduct. Removal of the triene protecting group, in a key synthetic step, yielded the title compounds PRI-2208 and PRI-2209, respectively. The analogs were examined for their antiproliferative activity in vitro against human breast cancer cells (MCF-7) and promyelocytic leukemia (HL-60) cells. The activity was compared with one of the parent compounds. Both analogs examined revealed similar or higher antiproliferative activity compared to 1alpha,25(OH)2D3 or to (24R)-1,24(OH)2D3. The studies of calcemic activity in vivo showed that analogs PRI-2208 and PRI-2209 did not influence the serum calcium level in doses, in which 1alpha,25(OH)2D3 or (24R)-1,24(OH)2D3 significantly increased this level. The antitumor activity of these analogs in the LLC mice tumor model was studied. Analog PRI-2208 was found to be more active in inhibiting LLC tumor growth than 1alpha,25(OH)2D3, as well as than PRI-2191 and PRI-2209. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

  4. Poly[(6-carboxypicolinato-κ3O2,N,O6(μ3-pyridine-2,6-dicarboxylato-κ5O2,N,O6:O2′:O6′dysprosium(III

    Directory of Open Access Journals (Sweden)

    Xu Li

    2009-11-01

    Full Text Available In the title complex, [Dy(C7H3NO4(C7H4NO4]n, one of the ligands is fully deprotonated while the second has lost only one H atom. Each DyIII ion is coordinated by six O atoms and two N atoms from two pyridine-2,6-dicarboxylate and two 6-carboxypicolinate ligands, displaying a bicapped trigonal-prismatic geometry. The average Dy—O bond distance is 2.40 Å, some 0.1Å longer than the corresponding Ho—O distance in the isotypic holmium complex. Adjacent DyIII ions are linked by the pyridine-2,6-dicarboxylate ligands, forming a layer in (100. These layers are further connected by π–π stacking interactions between neighboring pyridyl rings [centroid–centroid distance = 3.827 (3 Å] and C—H...O hydrogen-bonding interactions, assembling a three-dimensional supramolecular network. Within each layer, there are other π–π stacking interactions between neighboring pyridyl rings [centroid–centroid distance = 3.501 (2 Å] and O—H...O and C—H...O hydrogen-bonding interactions, which further stabilize the structure.

  5. Growth and Characterization of Organic Based Marine Dye NLO Material: 7-Bromo-6-chloro-3-[3-[(2R, 3S)-3-hydroxy-2-piperidyl]-2-oxopropyl]-4(3H)-quinazolinone

    OpenAIRE

    M. Jayandran; V. Balasubramanian

    2011-01-01

    An organic marine dye compound (7-bromo-6-chloro-3-[3-[(2R, 3S)-3-hydroxy-2-piperidyl]-2-oxopropyl]-4(3H)-quinazolinone) was synthesized. The characteristics of this dye is soluble in water. The organic compound was made into a crystal by slow evaporation technique. The grown crystals were characterized by single crystal x-ray diffraction (XRD) analysis, FTIR studies and UV-visible transmittance studies and the NLO activity of the grown crystal has been checked by second harmonic generation (...

  6. African Heath Sciences Vol 7 No 4.p65

    African Journals Online (AJOL)

    FOMCS2

    no evidence of significant associative interactions between Hib-CRM197 and MenC-CRM197 in saline-based buffers, pH 7.2. African ... aggregation of vaccine saccharide or protein components. 17, 18 ... chromatography and for analysis of the generated data. .... protein would be expected to elute after the main MenC-.

  7. 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

  8. Synthesis of the enantiomers of [3-{sup 3}H]-2-[[4-[(7-chloro-4-quinolinyl)-amino]pentyl]ethylamino]eth anol, [3-{sup 3}H]-hydroxychloroquine

    Energy Technology Data Exchange (ETDEWEB)

    Ellames, G.J.; Herbert, J.M.; Peace, J.E.; Smith, D.J.; Wedge, K.J. [Sterling Winthrop Research Centre, Alnwick (United Kingdom). Pharmaceuticals Research Div.

    1995-01-01

    The enantiomers of [3-{sup 3}H]-2-[[4-[(7-chloro-4-quinolinyl)amino] pentyl]ethylamino]ethanol, [3-{sup 3}H]-hydroxychloroquine, (R)-8 and (S)-8, have been prepared in two steps from the known precursors 4,7-dichloro-3-iodoquinoline, and the enantiomers of 2-[(4-aminopentyl) ethyl-amino]ethanol, (R)-2 and (S)-2, by formation of the enantiomers of 2-[[4-[(7-chloro-3-iodo-4-quinolinyl)amino]pentyl]ethylamino] ethanol, (R)-3 and (S)-3, and subsequent reductive deiodination with tritium gas over 10% palladium on charcoal. (Author).

  9. Oxonium ions substituting cesium ions in the structure of the new high-pressure borate HP-Cs{sub 1-x}(H{sub 3}O){sub x}B{sub 3}O{sub 5} (x=0.5-0.7)

    Energy Technology Data Exchange (ETDEWEB)

    Sohr, Gerhard; Heymann, Gunter; Wurst, Klaus; Huppertz, Hubert [Institut fuer Allgemeine, Anorganische und Theoretische Chemie, Leopold-Franzens-Universitaet Innsbruck (Austria); Neumair, Stephanie C. [Tyrolit Schleifmittelwerke Swarovski K.G., Schwaz (Austria); Schmedt auf der Guenne, Joern [Department fuer Chemie und Biologie, Universitaet Siegen (Germany)

    2014-04-07

    The new high-pressure borate HP-Cs{sub 1-x}(H{sub 3}O){sub x}B{sub 3}O{sub 5} (x=0.5-0.7) was synthesized under high-pressure/high-temperature conditions of 6 GPa/900 C in a Walker-type multianvil apparatus. The compound crystallizes in the monoclinic space group C2/c (Z=8) with the parameters a=1000.6(2), b=887.8(2), c=926.3(2) pm, β=103.1(1) , V=0.8016(3) nm{sup 3}, R1=0.0452, and wR2=0.0721 (all data). The boron-oxygen network is analogous to those of the compounds HP-MB{sub 3}O{sub 5}, (M=K, Rb) and exhibits all three structural motifs of borates - BO{sub 3} groups, corner-sharing BO{sub 4} tetrahedra, and edge-sharing BO{sub 4} tetrahedra - at the same time. Channels inside the boron-oxygen framework contain the cesium and oxonium ions, which are disordered on a specific site. Estimating the amount of hydrogen by solid-state NMR spectroscopy and X-ray diffraction led to the composition HP-Cs{sub 1-x}(H{sub 3}O){sub x}B{sub 3}O{sub 5} (x=0.5-0.7), which implies a nonzero phase width. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Crystal structure of (E-4,4,4-trifluoro-3-phenylbut-2-enoic acid

    Directory of Open Access Journals (Sweden)

    Alexey Barkov

    2015-12-01

    Full Text Available In the title compound, C10H7F3O2, the dihedral angle between the benzene ring and the ethylene plane is 76.34 (11°. In the crystal, O—H...O hydrogen bonds link the molecules into C(4 chains propagating in [010].

  11. 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)

  12. (3R,5S,7R,8R,9S,10S,12S,13R,14S-10,13-Dimethyl-17-[5-oxo-5-(prop-2-yn-1-yloxypentan-2-yl]hexadecahydro-1H-cyclopenta[a]phenanthrene-3,7,12-triyl triacetate

    Directory of Open Access Journals (Sweden)

    T. Kavitha

    2017-03-01

    Full Text Available In the title compound, C33H48O8, four terminal H atoms of cholic acid are replaced by three acetyl and one terminal alkyne group. All the acetyl residues are twisted with respect to the rings (A, B and C to which they are attached. The cyclopentane ring D adopts an envelope conformation with the methyl-substituted C atom as the flap. Rings A, B and C have chair conformations. The dihedral angle between the mean planes of rings C and D is 4.70 (11°. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a three-dimensional structure.

  13. 2S protein Ara h 7.0201 has unique epitopes compared to other Ara h 7 isoforms and is comparable to 2S proteins Ara h 2 and 6 in basophil degranulation capacity.

    Science.gov (United States)

    Hayen, S M; Ehlers, A M; den Hartog Jager, C F; Garssen, J; Knol, E F; Knulst, A C; Suer, W; Willemsen, L E M; Otten, H G

    2018-07-01

    Screening for specific IgE against 2S albumin proteins Ara h 2 and 6 has good positive predictive value in diagnosing peanut allergy. From the third 2S member Ara h 7, 3 isoforms have been identified. Their allergenicity has not been elucidated. This study investigated the allergenicity of Ara h 7 isoforms compared to Ara h 2 and 6. Sensitization of 15 DBPCFC-confirmed peanut-allergic patients to recombinant Ara h 2.0201, Ara h 6.01 and isoforms of recombinant Ara h 7 was determined by IgE immunoblotting strips. A basophil activation test (BAT) was performed in 9 patients to determine IgE-cross-linking capacities of the allergens. Sensitivity to the allergens was tested in 5 patients who were sensitized to at least 1 Ara h 7 isoform, by a concentration range in the BAT. 3D prediction models and sequence alignments were used to visualize differences between isoforms and to predict allergenic epitope regions. Sensitization to Ara h 7.0201 was most frequent (80%) and showed to be equally potent as Ara h 2.0201 and 6.01 in inducing basophil degranulation. Sensitization to Ara h 7.0201 together with Ara h 2.0201 and/or 6.01 was observed, indicating the presence of unique epitopes compared to the other 2 isoforms. Differences between the 3 Ara h 7 isoforms were observed in C-terminal cysteine residues, pepsin and trypsin cleavage sites and 3 single amino acid substitutions. The majority of peanut-allergic patients are sensitized to isoform Ara h 7.0201, which is functionally as active as Ara h 2.0201 and 6.01. Unique epitopes are most likely located in the C-terminus or an allergenic loop region which is a known allergenic epitope region for Ara h 2.0201 and 6.01. Due to its unique epitopes and allergenicity, it is an interesting candidate to improve the diagnostic accuracy for peanut allergy. © 2018 The Authors. Clinical & Experimental Allergy Published by John Wiley & Sons Ltd.

  14. Behavior of Escherichia coli O157:H7 and Listeria monocytogenes during fermentation and storage of camel yogurt.

    Science.gov (United States)

    Al-Nabulsi, Anas A; Olaimat, Amin N; Osaili, Tareq M; Ayyash, Mutamed M; Abushelaibi, Aisha; Jaradat, Ziad W; Shaker, Reyad; Al-Taani, Mahmoud; Holley, Richard A

    2016-03-01

    In addition to its nutritional and therapeutic properties, camel milk has the ability to suppress the growth of a wide range of foodborne pathogens, but there is a lack of information regarding the behavior of these pathogens in products such as yogurt produced from camel milk. The objective of the current study was to investigate the behavior of Listeria monocytogenes and Escherichia coli O157:H7 during manufacture and storage of camel yogurt. Camel milk inoculated with L. monocytogenes and E. coli O157:H7 was fermented at 43° C for 5h using freeze-dried lactic acid bacteria (LAB) starter cultures (Streptococcus thermophilus and Lactobacillus bulgaricus) and stored at 4 or 10 °C for 14 d. Camel milk inoculated with L. monocytogenes and E. coli O157:H7 without starter culture was also prepared. During fermentation, the numbers of L. monocytogenes and E. coli O157:H7 increased 0.3 and 1.6 log cfu/mL, respectively, in the presence of LAB, and by 0.3 and 2.7 log cfu/mL in the absence of LAB. During storage at 4 or 10 °C, L. monocytogenes increased 0.8 to 1.2 log cfu/mL by 14 d in camel milk without LAB, but in the presence of LAB, the numbers of L. monocytogenes were reduced by 1.2 to 1.7 log cfu/mL by 14 d. Further, E. coli O157:H7 numbers in camel milk were reduced by 3.4 to 3.5 log cfu/mL in the absence of LAB, but E. coli O157:H7 was not detected (6.3 log cfu/mL reduction) by 7d in camel yogurt made with LAB and stored at either temperature. Although camel milk contains high concentrations of natural antimicrobials, L. monocytogenes was able to tolerate these compounds in camel yogurt stored at refrigerator temperatures. Therefore, appropriate care should be taken during production of yogurt from camel milk to minimize the potential for postprocess contamination by this and other foodborne pathogens. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  15. 2-Ethoxy-4-[2-(3-nitrophenylhydrazonomethyl]phenol

    Directory of Open Access Journals (Sweden)

    Jun-Qiang Chen

    2009-10-01

    Full Text Available The title Schiff base compound, C15H15N3O4, was prepared from a condensation reaction of 3-ethoxy-4-hydroxybenzaldehyde and 3-nitrophenylhydrazine. The molecule is nearly planar; the dihedral angle between the hydroxybenzene ring and the nitrobenzene ring is 6.57 (7°. O—H...O, O—H...N and C—H...O hydrogen bonding helps to stabilize the crystal structure.

  16. Chiral Silver-Lanthanide Metal-Organic Frameworks Comprised of One-Dimensional Triple Right-Handed Helical Chains Based on [Ln73-OH)8]13+ Clusters.

    Science.gov (United States)

    Guo, Yan; Zhang, Lijuan; Muhammad, Nadeem; Xu, Yan; Zhou, Yunshan; Tang, Fang; Yang, Shaowei

    2018-02-05

    Three new isostructural chiral silver-lanthanide heterometal-organic frameworks [Ag 3 Ln 73 -OH) 8 (bpdc) 6 (NO 3 ) 3 (H 2 O) 6 ](NO 3 )·2H 2 O [Ln = Eu (1), Tb (2, Sm (3); H 2 bpdc = 2,2'-bipyridine-3,3'-dicarboxylic acid] based on heptanuclear lanthanide clusters [Ln 73 -OH) 8 ] 13+ comprised of one-dimensional triple right-handed helical chains were hydrothermally synthesized. Various means such as UV-vis spectroscopy, IR spectroscopy, elemental analysis, powder X-ray diffraction, and thermogravimetric/differential thermal analysis were used to characterize the compounds, wherein compound 3 was crystallographically characterized. In the structure of compound 3, eight μ 3 -OH - groups link seven Sm 3+ ions, forming a heptanuclear cluster, [Sm 73 -OH) 8 ] 13+ , and the adjacent [Sm 73 -OH) 8 ] 13+ clusters are linked by the carboxylic groups of bpdc 2- ligands, leading to the formation of a one-dimensional triple right-handed helical chain. The adjacent triple right-handed helical chains are further joined together by coordinating the pyridyl N atoms of the bpdc 2- ligands with Ag + , resulting in a chiral three-dimensional silver(I)-lanthanide(III) heterometal-organic framework with one-dimensional channels wherein NO 3 - anions and crystal lattice H 2 O molecules are trapped. The compounds were studied systematically with respect to their photoluminescence properties and energy-transfer mechanism, and it was found that H 2 bpdc (the energy level for the triplet states of the ligand H 2 bpdc is 21505 cm -1 ) can sensitize Eu 3+ luminescence more effectively than Tb 3+ and Sm 3+ luminescence because of effective energy transfer from bpdc 2- to Eu 3+ under excitation in compound 1.

  17. Synthesis and characterization of diphenyltin (IV) dithiocarbamate compounds

    International Nuclear Information System (INIS)

    Amirah Faizah Abdul Muthalib; Ibrahim Baba; Yang Farina; Mohd Wahid Samsudin

    2011-01-01

    Ten compounds of diphenyltin(IV) with N-dialkyl dithiocarbamate were successfully prepared using in situ methods. Elemental analysis data (C, H, N and S) showed an agreement with the general formula of (C 6 H 5 ) 2 Sn[S 2 CNR 1 R 2 ] (R 1 = CH 3 , C 2 H 5 , C 7 H 7 ; R 2 = C 2 H 5 , C 4 H 9 , C 6 H 1 1, iC 3 H 7 , C 7 H 7 ). The structures of these compounds have been examined by infrared spectroscopy, ultraviolet, 1 H, 13 C and 119 Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these compounds showed three important peaks for v(C...N), v(C...S) and v(C...S) bands that appeared in the region of 1474 -1499, 969 - 995 and 324 - 335 cm -1 respectively. Data for 13 C NMR spectroscopy showed an important peak in the region of 198 - 200 ppm that corresponded to the NCS 2 group. Single crystal X-ray diffraction studies showed (C 6 H 5 ) 2 Sn[S 2 CN(C 2 H 5 )(CH 3 )] 2 (1) is six coordinated and adopted a monoclinic system with space group C2/c, while (C 6 H 5 ) 2 SnCl[S 2 CN(C 7 H 7 )(iC 3 H 7 )] (2) is five coordinated, crystallized in monoclinic system with space group Pb 1 /n. Meanwhile, six coordinated (C 6 H 5 ) 2 Sn[S 2 CN(CH 3 )(iC 3 H 7 )] 2 (3) adopted a orthorhombic system with a space group Pbcn. (author)

  18. Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by 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

    Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group$P\\bar 1$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) Å3of compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) Å3of compound (2). Structural analyses reveal that the title compounds are isostructural.

  19. meso-[5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-1(14,7-diene]nickel(II dibromide dihydrate

    Directory of Open Access Journals (Sweden)

    Feifei Shi

    2010-06-01

    Full Text Available The asymmetric unit of the title complex, [Ni(C16H32N4]Br2·2H2O, contains two [Ni(C16H32N4]2+ cations, four Br− anions and four uncoordinated H2O molecules. The Ni atoms are in a slightly distorted square-planar coordination by the four macrocyclic N atoms, which are almost coplanar [N—N—N—N torsion angles of 2.97 (6 and 3.12 (7°]. In the crystal, a network of N—H...Br, O—H...Br and N—H...O hydrogen bonds leads to the formation of a chain structure.

  20. Cs[FeSe{sub 2}], Cs{sub 3}[FeSe{sub 2}]{sub 2}, and Cs{sub 7}[Fe{sub 4}Se{sub 8}]. Missing links of known chalcogenido ferrate series

    Energy Technology Data Exchange (ETDEWEB)

    Stueble, Pirmin; Roehr, Caroline [Institut fuer Anorganische und Analytische Chemie, Universitaet Freiburg (Germany)

    2017-11-17

    The three cesium selenido ferrate title compounds with an Se:Fe ratio of 2:1 were synthesized from stoichiometric samples reacting elemental Cs either (A) with Fe and Se in a double-crucible setup (Cs[FeSe{sub 2}], Cs{sub 3}[FeSe{sub 2}]{sub 2}) or (B) with previously prepared FeSe{sub 2} (Cs{sub 3}[FeSe{sub 2}]{sub 2}, Cs{sub 7}[Fe{sub 4}S{sub 8}]) (T{sub max} = 800-1000 C). The pure Fe{sup III} ferrate Cs[FeSe{sub 2}] crystallizes in the Tl[FeSe{sub 2}] type [monoclinic, space group C2/m, a = 1392.95(10), b = 564.43(3), c = 737.44(6) pm, β = 119.163(5) , Z = 4, R{sub 1} = 0.0550]. It is thus not isotypic to all other alkali ferrates(III) A[FeS{sub 2}] and A[FeSe{sub 2}] containing chains of edge-sharing tetrahedra, but crystallizes in a t2 subgroup of the Immm structure of Cs[FeS{sub 2}]. The mixed-valent chain compound Cs{sub 3}[FeSe{sub 2}]{sub 2} is isotypic to its sulfido analogue [orthorhombic, space group Pnma, a = 777.88(6), b = 1151.02(6), c = 1341.61(7) pm, Z = 4, R{sub 1} = 0.0470]. In contrast to the isopunctal Na{sub 3}[FeSe{sub 2}]{sub 2} type K/Rb compounds the chains are only slightly corrugated. The monoclinic, likewise mixed-valent Fe{sup II/III} selenido ferrate Cs{sub 7}[Fe{sub 4}Se{sub 8}] [monoclinic, space group C2/c, a = 1953.79(10), b = 879.71(5), c = 1717.03(10) pm, β = 117.890(2) , Z = 4, R{sub 1} = 0.0816] is isostructural both to the cesium sulfido and tellurido compound. The structure contains oligomeric moieties of four edge sharing [FeSe{sub 4}] tetrahedra forming slightly distorted tetrahedral clusters [Fe{sub 4}Se{sub 8}]{sup 7-}, which are surrounded by a cube of 26 Cs cations. Based on a structure map, the crystal chemistry of the three title compounds is discussed together with all chain/cluster ferrates of the general series A{sub 1+x}[Fe{sup III}{sub 1-x}Fe{sup II}{sub x}Q{sub 2}] (x = 0-1; A = Na, K, Rb, Cs; Q = S, Se, Te). (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. 2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate

    Directory of Open Access Journals (Sweden)

    Guoquan Zhou

    2012-04-01

    Full Text Available The title compound, C6H7O2S3+·BF4−, consists of a planar 2-thioxo-1,3-dithiol-4,5-yl unit [maximum deviation from the ring plane = 0.020 (3 Å], with an ethylenedioxy group fused at the 4,5-positions; the ethylenedioxy C atoms are disordered over two positions with site-occupancy factors of 0.5. The 1,4-dioxine ring has a twist-chair conformation. Weak cation–anion S...F interactions [3.022 (4–3.095 (4 Å] and an S...O [3.247 (4 Å] interaction are present.

  2. Synthesis and crystal structure of new uranyl selenite(IV)-selenate(VI) [C5H14N][(UO2)3(SeO4)4(HSeO3)(H2O)](H2SeO3)(HSeO4)

    International Nuclear Information System (INIS)

    Krivovichev, S.V.; Tananaev, I.G.; Myasoedov, B.F.; Kalenberg, V.

    2006-01-01

    Crystals of new uranyl selenite(IV)-selenate(VI) [C 5 H 14 N][(UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)](H 2 SeO 3 )(HSeO 4 ) are obtained by the method of evaporation from aqueous solutions. Compound has triclinic lattice, space group P1-bar, a=11.7068(9), b=14.8165(12), c=16.9766(15), α=73.899(6), β=76.221(7), γ=89.361(6) Deg, V=2743.0(4) A 3 , Z=2. Laminated complexes (UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)] 3- are the basis of the structure. [HSe(VI)O 4 ] - , [H 2 Se(IV)O 3 ] complexes and protonated methylbutylamine cations are disposed between layers [ru

  3. Quinolinium 8-hydroxy-7-iodoquinoline-5-sulfonate 0.8-hydrate

    Directory of Open Access Journals (Sweden)

    Graham Smith

    2012-12-01

    Full Text Available In the crystal structure of the title hydrated quinolinium salt of ferron (8-hydroxy-7-iodoquinoline-5-sulfonic acid, C9H7N+·C9H5INO4S−·0.8H2O, the quinolinium cation is fully disordered over two sites (occupancy factors fixed at 0.63 and 0.37 lying essentially within a common plane and with the ferron anions forming π–π-associated stacks down the b axis [minimum ring centroid separation = 3.462 (6 Å]. The cations and anions are linked into chains extending along c through hydroxy O—H...O and quinolinium N—H...O hydrogen bonds to sulfonate O-atom acceptors which are also involved in water O—H...O hydrogen-bonding interactions along b, giving a two-dimensional network.

  4. Crystal structure of poly[N,N-diethyl-2-hy-droxy-ethan-1-aminium [μ3-cyanido-κ(3) C:C:N-di-μ-cyanido-κ(4) C:N-dicuprate(I)

    Science.gov (United States)

    Corfield, Peter W R; Cleary, Emma; Michalski, Joseph F

    2016-07-01

    In the title compound, {(C6H16NO)[Cu2(CN)3]} n , the cyanide groups link the Cu(I) atoms into an open three-dimensional anionic network, with the mol-ecular formula Cu2(CN)3 (-). One Cu(I) atom is tetra-hedrally bound to four CN groups, and the other Cu(I) atom is bonded to three CN groups in an approximate trigonal-planar coordination. The tetra-hedrally coordinated Cu(I) atoms are linked into centrosymmetric dimers by the C atoms of two end-on bridging CN groups which bring the Cu(I) atoms into close contact at 2.5171 (7) Å. Two of the cyanide groups bonded to the Cu(I) atoms with trigonal-planar surrounding link the dimeric units into columns along the a axis, and the third links the columns together to form the network. The N,N-di-ethyl-ethano-lamine mol-ecules used in the synthesis have become protonated at the N atoms and are situated in cavities in the network, providing charge neutrality, with no covalent inter-actions between the cations and the anionic network.

  5. {2-[Bis(2,4-di-tert-butylphenoxyphosphanyloxy-κP]-3,5-di-tert-butylphenyl-κC1}[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I toluene monosolvate

    Directory of Open Access Journals (Sweden)

    Detlef Selent

    2012-02-01

    Full Text Available The reaction of (η3-allyl[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I with tris(2,4-di-tert-butylphenylphosphite in toluene produces the title compound, [Rh(C42H62O3P(C8H12]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2 and 0.190 (2.

  6. The effects of H+ implants on YBa2Cu3O7 superconducting materials

    International Nuclear Information System (INIS)

    Luo Chenglin; Pan Guoqiang; Han Ming; Wang Guanghou

    1993-09-01

    The variations of microstructure and electrical properties of Y-Ba-Cu O with and without H + implantation have been studied by scanning electron microscope, X-ray diffraction and IR spectrum techniques. The results have shown that these variations are directly relative to the intrinsic quality of YBa 2 Cu 3 O 7 . Microstructural change is responsible for the variations of electrical properties of YBa 2 Cu 3 O 7 superconductor. The Cu H bond formed by H + implanted into YBa 2 Cu 3 O 7 is not a key factor for these variations

  7. (2E-1-(3-Chlorophenyl-3-(4-chlorophenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Jerry P. Jasinski

    2009-11-01

    Full Text Available The title compound, C15H10Cl2O, is a chalcone with 3-chlorophenyl and 4-chlorophenyl substituents bonded at the opposite ends of a propenone group, the biologically active region. The dihedral angle between mean planes of these two chloro-substituted benzene rings is 46.7 (7° compared to 46.0 (1 and 32.4 (1° in similar published sructures. The angles between the mean plane of the prop-2-en-1-one group and the mean planes of the 3-chlorophenyl and 4-chlorophenyl rings are 24.1 (2 and 29.63°, respectively. While no classical hydrogen bonds are present, weak intermolecular C—H...π-ring interactions are observed, which contribute to the stability of crystal packing.

  8. Production and characterization of compounds based on MgB4O7 for application in dosimetry

    International Nuclear Information System (INIS)

    Souza, Luiza Freire de

    2016-01-01

    Many materials with luminescent properties are used for ionizing radiation dosimetry through the thermoluminescence (TL) and optically stimulated luminescence (OSL) techniques. Detectors based on lithium fluoride (LiF), calcium sulphate (CaSO 4 ) and aluminum oxide (Al 2 O 3 ), doped or codoped with various elements, are the TL or OSL commercial dosimeters most widely used currently. However, several researches are focused to the development of new TL /OSL materials in intention to enhance the dosimetric properties, in view that no TL/OSL dosimeter has all the ideal characteristics for monitoring the radiation. In this context, magnesium tetraborate (MgB 4 O 7 ), which has been presented in the literature as a material for dosimetry TL, was investigated in this work. As there are no reports on the structural characterization of this material or regarding to its applicability on OSL dosimetry, the proposal of the present work was to develop compounds based on MgB 4 O 7 , with different doping, by solid state synthesis. It was made the structural, optical, TL and OSL characterization of the compound to verify it feasibility for application on radiation dosimetry. Initially, it was determined the calcination temperature and time for MgB 4 O 7 formation, with the use of thermal analyses and x ray diffraction. The ideal calcination was found at 900 °C for 7 hours. It were produced , in powder form, the compounds: MgB 4 O 7 , MgB 4 O 7 :Dy, MgB 4 O 7 :Dy,Li, MgB 4 O 7 :Ce, MgB 4 O 7 :Ce,Li, MgB 4 O 7 :Nd and MgB 4 O 7 :Nd,Li. For TL and OSL analyses it were produced pellets sintering at 950 °C for 2 hours. The radioluminescence (RL) analyses of MgB 4 O 7 :Dy and MgB 4 O 7 :Dy,Li shows wavelength emissions at 490, 590, 670 and 760 nm. For MgB 4 O 7 :Ce and MgB 4 O 7 :Ce,Li RL was observed wide emission band in the ultraviolet region. For the MgB 4 O 7 :Nd and MgB 4 O 7 :Nd,Li RL were not observed emission from the ultraviolet to infrared. With the results obtained from

  9. Internal Friction of Li7La3Zr2O12 Based Lithium Ionic Conductors

    Directory of Open Access Journals (Sweden)

    Wang X.P.

    2016-03-01

    Full Text Available The diffusion mechanisms of lithium ions in tetragonal phase as well as in Al and Nb stabilized cubic Li7La3Zr2O12 compounds were investigated by low-frequency internal friction technique. In the cubic Li7La3Zr2O12 phase, a remarkable relaxation-type internal friction peak PC with a peak height up to 0.12 was observed in the temperature range from 15°C to 60°C. In the tetragonal phase however, the height of the PT peak dropped to 0.01. The obvious difference of the relaxation strength between the cubic and tetragonal phases is due to the different distribution of lithium ions in lattice, ordered in the tetragonal phase and disordered in the cubic phase. Based on the crystalline structure of the cubic garnet-type Li7La3Zr2O12 compound, it is suggested that the high internal friction peak in the cubic phase may be attributed to two diffusion processes of lithium ions: 96h↔96h and 96h↔24d.

  10. 7 CFR 1927.53 - Costs of title clearance and closing of transactions.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 12 2010-01-01 2010-01-01 false Costs of title clearance and closing of transactions... and Loan Closing § 1927.53 Costs of title clearance and closing of transactions. The borrower or the... payment of all costs of title clearance and closing of the transaction and will arrange for payment before...

  11. New borohydride anion B6H7-

    International Nuclear Information System (INIS)

    Kuznetsov, I.Yu.; Vinitskij, D.M.; Solntsev, K.A.

    1985-01-01

    The [Ni(Bipy) 3 ] (B 6 H 7 ) 2 , (Ph 4 P)B 6 H 7 , [Ni(Phen) 3 ](B 6 H 7 ) 2 crystals (where Bipy = bipyridine, Phen = phenathroline, Ph = phenyl) are obtained via the exchange reaction with a subsequent recrystallization from aqua-acetonic and acetonic solutions. The structure is studied of a new borohydride anion B 6 H 7 - possessing a four-valence bond unique for polyhedral borohydride anions. A triangular face of boride skeleton coordinating a hydrogen atom is considerably larger than other faces, and the electron density on this hydrogen atom is evidently much higher than at the end hydride hydrogen atoms. The trend of B 6 H 7 - anion to form statistically disordered structurs testifies to a rather slight effect of the seventh hydrogen atom position on the structure pattern of the ionic crystal lattice

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

    Directory of Open Access Journals (Sweden)

    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.

  13. NMR structural studies of the ionizing radiation adduct 7-hydro-8-oxodeoxyguanosine (8-oxo-7H-dG) opposite deoxyadenosine in a DNA duplex. 8-oxo-7H-dG(syn)·dA(anti) alignment at lesion site

    International Nuclear Information System (INIS)

    Kouchakdjian, M.; Patel, D.J.; Bodepudi, V.; Shibutani, S.; Eisenberg, M.; Johnson, F.; Grollman, A.P.

    1991-01-01

    Proton NMR studies are reported on the complementary d(C1-C2-A3-C4-T5-A6-oxo-G7-T8-C9-A10-C11-C12)·d(G13-G14-T15-G16-A17-A18-T19-A20-G21-T22-G23-G24) dodecanucleotide duplex (designated 8-oxo-7H-dG·dA 12-mer), which contains a centrally located 7-hydro-8-oxodeoxyguanosine (8-oxo-7H-dG) residue, a group commonly found in DNA that has been exposed to ionizing radiation or oxidizing free radicals. From the NMR spectra it can be deduced that this moiety exists as two tautomers, or gives rise to two DNA conformations, that are in equilibrium and that exchange slowly. The present study focuses on the major component of the equilibrium that originates in the 6,8-dioxo tautomer of 8-oxo-7H-dG. The authors have assigned the exchangeable NH1, NH7, and NH 2 -2 base protons located on the Watson-Crick and Hoogsteen edges of 8-oxo-7H-dG7 in the 8-oxo-7H-dG·dA 12-mer duplex, using an analysis of one- and two-dimensional nuclear Overhauser enhancement (NOE) data in H 2 O solution. They were able to detect a set of intra- and interstrand NOEs between protons (exchangeable and nonexchangeable) on adjacent residues in the d(A6-oxo-G7-T8)·d(A17-A18-T19) trinucleotide segment centered about the lesion site that establishes stacking of the oxo-dG7(syn)·dA(anti) pair between stable Watson-Crick dA6·dT19 and dT8·A17 base pairs with minimal perturbation of the helix. The structural studies demonstrate that 8-oxo-7H-dG(syn)·dA(anti) forms a stable pair in the interior of the helix, providing a basis for the observed incorporation of dA opposite 8-oxo-7H-dG when readthrough occurs past this oxidized nucleoside base

  14. Synthesis, Characterization, and Antimicrobial Activity of a Novel Trisazo Dye from 3-Amino-4H-thieno[3,4-c][1]benzopyran-4-one

    Science.gov (United States)

    Tsemeugne, Joseph; Rohand, Taoufik; Ngongang, Arnaud Djintchui; Sondengam, Beibam Luc

    2018-01-01

    A new trisazo dye has been synthesized by coupling the diazonium ion of 3-amino-4H thieno[3,4-c][1]benzopyran-4-one with 2-tert-butyl-4-methoxyphenol. The newly prepared trisazo dye was characterized by its physical, elemental, and spectroscopic data. 2D-NMR (COSY, HSQC, and HMBC) techniques were used to secure the structural assignments. The new trisazo dye (compound 7) along with precursors 3, 4, and 6 was screened by microdilution susceptibility assay for antibacterial and antifungal activities towards eight bacterial strains and three yeasts selected on the basis of their relevance as human pathogens. The results showed that compound 7 (MIC = 2–128 μg/mL) was the most active as compared with its precursors. The most resistant microorganisms were V. cholerae NB2 and V. cholerae SG24, whereas the most sensitive microorganism was C. neoformans. The overall results of this study indicated that compound 7 had the greatest potential value against both yeasts and multidrug-resistant bacteria, so further investigation is warranted. PMID:29484208

  15. Synthesis, Characterization, and Antimicrobial Activity of a Novel Trisazo Dye from 3-Amino-4H-thieno[3,4-c][1]benzopyran-4-one

    Directory of Open Access Journals (Sweden)

    Joseph Tsemeugne

    2018-01-01

    Full Text Available A new trisazo dye has been synthesized by coupling the diazonium ion of 3-amino-4H thieno[3,4-c][1]benzopyran-4-one with 2-tert-butyl-4-methoxyphenol. The newly prepared trisazo dye was characterized by its physical, elemental, and spectroscopic data. 2D-NMR (COSY, HSQC, and HMBC techniques were used to secure the structural assignments. The new trisazo dye (compound 7 along with precursors 3, 4, and 6 was screened by microdilution susceptibility assay for antibacterial and antifungal activities towards eight bacterial strains and three yeasts selected on the basis of their relevance as human pathogens. The results showed that compound 7 (MIC = 2–128 μg/mL was the most active as compared with its precursors. The most resistant microorganisms were V. cholerae NB2 and V. cholerae SG24, whereas the most sensitive microorganism was C. neoformans. The overall results of this study indicated that compound 7 had the greatest potential value against both yeasts and multidrug-resistant bacteria, so further investigation is warranted.

  16. Synthesis, spectral characterization and X-ray crystal structure studies of 3-(benzo[d][1,3]dioxol-5-yl)-5-(3-methylthiophen-2-yl)-4,5-dihydro-1H-pyrazole-1-carboxamide: Hirshfeld surface, DFT and thermal analysis

    Science.gov (United States)

    Kumara, Karthik; Dileep Kumar, A.; Naveen, S.; Ajay Kumar, K.; Lokanath, N. K.

    2018-06-01

    A novel pyrazole derivative, 3-(benzo[d][1,3]dioxol-5-yl)-5-(3-methylthiophen-2-yl)-4,5-dihydro-1H-pyrazole-1-carboxamide was synthesized and characterized by elemental analysis, FT-IR, NMR (1H and 13C), MS, UV-visible spectra and finally the structure was confirmed by the single crystal X-ray diffraction studies. The title compound (C16H15N3O3S) crystallized in the triclinic crystal system, with the space group Pī. A dihedral angle of 65.84(1)° between the pyrazole and the thiophene rings confirms the twisted conformation between them. The X-ray structure revealed that the pyrazole ring adopts an E-form and an envelope conformation on C7 atom. The crystal and molecular structure of the title compound is stabilized by inter molecular hydrogen bonds. The compound possesses three dimensional supramolecular self-assembly, in which Csbnd H⋯O and Nsbnd H⋯O chains build up two dimensional arrays, which are extended to 3D network through Csbnd H···Cg and Csbnd O···Cg interactions. The structure also exhibits intramolecular hydrogen bonds of the type Nsbnd H⋯N and π···π stacking interactions, which contributes to the crystal packing. Further, Hirshfeld surface analysis was carried out for the graphical visualization of several short intermolecular interactions on the molecular surface while the 2D finger-print plot provides percentage contribution of each individual atom-to-atom interactions. The thermal decomposition of the compound has been studied by thermogravimetric analysis. The molecular geometries and electronic structures of the compounds were fully optimized, calculated with ab-initio methods by HF, DFT/B3LYP functional in combination of different basis set with different solvent environment and the structural parameters were compared with the experimental data. The Mulliken atomic charges and molecular electrostatic potential on molecular van der Waals (vdW) surface were calculated to know the electrophilic and nucleophilic regions

  17. 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.

  18. Overexpression of MfPIP2-7 from Medicago falcata promotes cold tolerance and growth under NO3 (-) deficiency in transgenic tobacco plants.

    Science.gov (United States)

    Zhuo, Chunliu; Wang, Ting; Guo, Zhenfei; Lu, Shaoyun

    2016-06-14

    Plasma membrane intrinsic proteins (PIPs), which belong to aquaporins (AQPs) superfamily, are subdivided into two groups, PIP1 and PIP2, based on sequence similarity. Several PIP2s function as water channels, while PIP1s have low or no water channel activity, but have a role in water permeability through interacting with PIP2. A cold responsive PIP2 named as MfPIP2-7 was isolated from Medicago falcata (hereafter falcata), a forage legume with great cold tolerance, and transgenic tobacco plants overexpressing MfPIP2-7 were analyzed in tolerance to multiple stresses including freezing, chilling, and nitrate reduction in this study. MfPIP2-7 transcript was induced by 4 to 12 h of cold treatment and 2 h of abscisic acid (ABA) treatment. Pretreatment with inhibitor of ABA synthesis blocked the cold induced MfPIP2-7 transcript, indicating that ABA was involved in cold induced transcription of MfPIP2-7 in falcata. Overexpression of MfPIP2-7 resulted in enhanced tolerance to freezing, chilling and NO3 (-) deficiency in transgenic tobacco (Nicotiana tabacum L.) plants as compared with the wild type. Moreover, MfPIP2-7 was demonstrated to facilitate H2O2 diffusion in yeast. Higher transcript levels of several stress responsive genes, such as NtERD10B, NtERD10C, NtDREB1, and 2, and nitrate reductase (NR) encoding genes (NtNIA1, and NtNIA2) were observed in transgenic plants as compared with the wild type with dependence upon H2O2. In addition, NR activity was increased in transgenic plants, which led to alterations in free amino acid components and concentrations. The results suggest that MfPIP2-7 plays an important role in plant tolerance to freezing, chilling, and NO3 (-) deficiency by promoted H2O2 diffusion that in turn up-regulates expression of NIAs and multiple stress responsive genes.

  19. Expression of the costimulatory molecule B7-H3 is associated with prolonged survival in human pancreatic cancer

    International Nuclear Information System (INIS)

    Loos, Martin; Hedderich, Dennis M; Ottenhausen, Malte; Giese, Nathalia A; Laschinger, Melanie; Esposito, Irene; Kleeff, Jörg; Friess, Helmut

    2009-01-01

    Costimulatory signaling has been implicated as a potential regulator of antitumor immunity in various human cancers. In contrast to the negative prognostic value of aberrant B7-H1 expression by pancreatic cancer cells, the role of B7-H3 is still unknown. Therefore, we investigated the expression pattern and clinical significance of B7-H3 expression in human pancreatic cancer. B7-H3 expression was evaluated by immunohistochemistry in 68 patients with pancreatic cancer who underwent surgical tumor resection. Expression data was correlated with clinicopathologic features and with the number of tumor-infiltrating T cells. B7-H3 expression was significantly upregulated in pancreatic cancer compared to normal pancreas (p < 0.05). In 60 of 68 examined tumors B7-H3 protein was detectable in pancreatic cancer cells. Patients with high tumor B7-H3 levels had a significantly better postoperative prognosis than patients with low tumor B7-H3 levels (p = 0.0067). Furthermore, tumor B7-H3 expression significantly correlated with the number of tumor-infiltrating CD8+ T cells (p = 0.018). We demonstrate for the first time that B7-H3 is abundantly expressed in pancreatic cancer and that tumor-associated B7-H3 expression significantly correlates with prolonged postoperative survival. Our findings suggest that B7-H3 might play an important role as a potential stimulator of antitumor immune response in pancreatic cancer

  20. Growth and Characterization of Organic Based Marine Dye NLO Material: 7-Bromo-6-chloro-3-[3-[(2R, 3S-3-hydroxy-2-piperidyl]-2-oxopropyl]-4(3H-quinazolinone

    Directory of Open Access Journals (Sweden)

    M. Jayandran

    2011-01-01

    Full Text Available An organic marine dye compound (7-bromo-6-chloro-3-[3-[(2R, 3S-3-hydroxy-2-piperidyl]-2-oxopropyl]-4(3H-quinazolinone was synthesized. The characteristics of this dye is soluble in water. The organic compound was made into a crystal by slow evaporation technique. The grown crystals were characterized by single crystal x-ray diffraction (XRD analysis, FTIR studies and UV-visible transmittance studies and the NLO activity of the grown crystal has been checked by second harmonic generation (SHG test.

  1. Indolo[3,2-c]cinnolines with antiproliferative, antifungal, and antibacterial activity.

    Science.gov (United States)

    Barraja, P; Diana, P; Lauria, A; Passannanti, A; Almerico, A M; Minnei, C; Longu, S; Congiu, D; Musiu, C; La Colla, P

    1999-08-01

    A series of indolo[3,2-c]cinnoline derivatives was prepared and tested to evaluate their biological activity. Most of them inhibited the proliferation of leukemia, lymphoma and solid tumor-derived cell lines at micromolar concentrations, whereas none of the compounds were active against HIV-1. With the exception of 7g, all title compounds showed antibacterial activity against gram-positive bacteria, being up to 200 times more potent than the reference drug streptomycin. Some of the indolo[3,2-c]cinnolines were also endowed with good antifungal activity, particularly against Criptococcus neoformans.

  2. Crystal structure of diethyl 2-amino-6-[(thiophen-3-ylethynyl]azulene-1,3-dicarboxylate

    Directory of Open Access Journals (Sweden)

    Sebastian Förster

    2015-03-01

    Full Text Available The title compound, C22H19NO4S, has an almost planar geometry supported by intramolecular N—H...O and C—H...O hydrogen bonds. The thiophene ring is inclined to the azulene ring by 4.85 (16°, while the ethoxycarbonyl groups are inclined to the azulene ring by 7.0 (2 and 5.7 (2°. 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 via C—H...π interactions, forming sheets parallel to (10-1.

  3. Metal ion displacements in noncentrosymmetric chalcogenides La{sub 3}Ga{sub 1.67}S{sub 7}, La{sub 3}Ag{sub 0.6}GaCh{sub 7} (Ch=S, Se), and La{sub 3}MGaSe{sub 7} (M=Zn, Cd)

    Energy Technology Data Exchange (ETDEWEB)

    Iyer, Abishek K. [Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G2G2 (Canada); Yin, Wenlong [Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G2G2 (Canada); Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621900 (China); Rudyk, Brent W. [Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G2G2 (Canada); Lin, Xinsong [Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G2G2 (Canada); Centre for Oil Sands Sustainability, Northern Alberta Institute of Technology, Edmonton, Alberta, Canada T6N1E5 (Canada); Nilges, Tom [Department of Chemistry, Technical University of Munich, 85748 Garching b. München (Germany); Mar, Arthur, E-mail: arthur.mar@ualberta.ca [Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G2G2 (Canada)

    2016-11-15

    The quaternary Ga-containing chalcogenides La{sub 3}Ag{sub 0.6}GaS{sub 7}, La{sub 3}Ag{sub 0.6}GaSe{sub 7}, La{sub 3}ZnGaSe{sub 7}, and La{sub 3}CdGaSe{sub 7}, as well as the related ternary chalcogenide La{sub 3}Ga{sub 1.67}S{sub 7}, were prepared by reactions of the elements at 950 °C. They adopt noncentrosymmetric hexagonal structures (space group P6{sub 3}, Z=2) with cell parameters (a=10.2 Å, c=6.1 Å for the sulfides; a=10.6 Å, c=6.4 Å for the selenides) that are largely controlled by the geometrical requirements of one-dimensional stacks of Ga-centered tetrahedra separated by the La atoms. Among these compounds, which share the common formulation La{sub 3}M{sub 1–x}GaCh{sub 7} (M=Ga, Ag, Zn, Cd; Ch=S, Se), the M atoms occupy sites within a stacking of trigonal antiprisms formed by Ch atoms. The location of the M site varies between extremes with trigonal antiprismatic (CN6) and trigonal planar (CN3) geometry. Partial occupation of these sites and intermediate ones accounts for the considerable versatility of these structures and the occurrence of large metal displacement parameters. The site occupations can be understood in a simple way as being driven by the need to satisfy appropriate bond valence sums for both the M and Ch atoms. Band structure calculations rationalize the substoichiometry observed in the Ag-containing compounds (La{sub 3}Ag{sub 0.6}GaS{sub 7}, La{sub 3}Ag{sub 0.6}GaSe{sub 7}) as a response to overbonding. X-ray photoelectron spectroscopy supports the presence of monovalent Ag atoms in these compounds, which are not charge-balanced. - Graphical abstract: Partial occupation of metal atoms in multiple sites accounts for versatility in Ga-containing chalcogenides La{sub 3}M{sub 1–x}GaCh{sub 7} with noncentrosymmetric hexagonal structures. - Highlights: • La{sub 3}M{sub 1–x}GaCh{sub 7} (M =Ga, Ag, Zn, Cd; Ch =S, Se) adopt related hexagonal structures. • Large displacements of M atoms originate from partial occupation of multiple

  4. (-)-P7C3-S243 Protects a Rat Model of Alzheimer's Disease From Neuropsychiatric Deficits and Neurodegeneration Without Altering Amyloid Deposition or Reactive Glia.

    Science.gov (United States)

    Voorhees, Jaymie R; Remy, Matthew T; Cintrón-Pérez, Coral J; El Rassi, Eli; Khan, Michael Z; Dutca, Laura M; Yin, Terry C; McDaniel, Latisha N; Williams, Noelle S; Brat, Daniel J; Pieper, Andrew A

    2017-11-06

    In addition to cognitive deficits, Alzheimer's disease (AD) is associated with other neuropsychiatric symptoms, including severe depression. Indeed, depression often precedes cognitive deficits in patients with AD. Unfortunately, the field has seen only minimal therapeutic advances, underscoring the critical need for new treatments. P7C3 aminopropyl carbazoles promote neuronal survival by enhancing nicotinamide adenine dinucleotide flux in injured neurons. Neuroprotection with P7C3 compounds has been demonstrated in preclinical models of neurodegeneration by virtue of promoting neuronal survival independently of early disease-specific pathology, resulting in protection from cognitive deficits and depressive-like behavior. We hypothesize that P7C3 compounds might be uniquely applicable to patients with AD, given the comorbid presentation of depression and cognitive deficits. Aging male and female wild-type and TgF344-AD rats, a well-characterized preclinical AD model, were administered (-)-P7C3-S243 daily for 9 and 18 months, beginning at 6 months of age. Behavioral phenotypes related to cognition and depression were assessed at 15 and 24 months, and brain pathology and biochemistry were assessed at 24 months. (-)-P7C3-S243 safely protected aging male and female wild-type and TgF344-AD rats from cognitive deficits and depressive-like behavior. Depressive-like behavior occurred earlier than cognitive deficits in TgF344-AD rats, consistent with AD in many patients. Treatment with (-)-P7C3-S243 blocked neurodegeneration in TgF344-AD rats, without altering amyloid deposition or indicators of neuroinflammation. Neuronal cell death-specific treatment approaches, such as P7C3 compounds, may represent a new treatment approach for patients experiencing the combination of cognitive deficits and depression associated with AD. Published by Elsevier Inc.

  5. Dissociation dynamics of 3- and 4-nitrotoluene radical cations: Coherently driven C-NO2 bond homolysis

    Science.gov (United States)

    Ampadu Boateng, Derrick; Gutsev, Gennady L.; Jena, Puru; Tibbetts, Katharine Moore

    2018-04-01

    Monosubstituted nitrotoluenes serve as important model compounds for nitroaromatic energetic molecules such as trinitrotoluene. This work investigates the ultrafast nuclear dynamics of 3- and 4-nitrotoluene radical cations using femtosecond pump-probe measurements and the results of density functional theory calculations. Strong-field adiabatic ionization of 3- and 4-nitrotoluene using 1500 nm, 18 fs pulses produces radical cations in the ground electronic state with distinct coherent vibrational excitations. In both nitrotoluene isomers, a one-photon excitation with the probe pulse results in NO2 loss to form C7H7+, which exhibits out-of-phase oscillations in yield with the parent molecular ion. The oscillations in 4-nitrotoluene with a period of 470 fs are attributed to the torsional motion of the NO2 group based on theoretical results showing that the dominant relaxation pathway in 4-nitrotoluene radical cations involves the rotation of the NO2 group away from the planar geometry. The distinctly faster oscillation period of 216 fs in 3-nitrotoluene is attributed to an in-plane bending motion of the NO2 and CH3 moieties based on analysis of the normal modes. These results demonstrate that coherent nuclear motions determine the probability of C-NO2 homolysis in the nitrotoluene radical cations upon optical excitation within several hundred femtoseconds of the initial ionization event.

  6. Crystal structures of the dioxane hemisolvates of N-(7-bromomethyl-1,8-naphthyridin-2-ylacetamide and bis[N-(7-dibromomethyl-1,8-naphthyridin-2-ylacetamide

    Directory of Open Access Journals (Sweden)

    Robert Rosin

    2017-10-01

    Full Text Available The syntheses and crystal structures of N-(7-bromomethyl-1,8-naphthyridin-2-ylacetamide dioxane hemisolvate, C11H10BrN3O·0.5C4H8O2, (I, and bis[N-(7-dibromomethyl-1,8-naphthyridin-2-ylacetamide] dioxane hemisolvate, 2C11H9Br2N3O·0.5C4H8O2, (II, are described. The molecules adopt a conformation with the N—H hydrogen pointing towards the lone electron pair of the adjacent naphthyridine N atom. The crystals of (I are stabilized by a three-dimensional supramolecular network comprising N—H...N, C—H...N and C—H...O hydrogen bonds, as well as C—Br...π halogen bonds. The crystals of compound (II are stabilized by a three-dimensional supramolecular network comprising N—H...N, C—H...N and C—H...O hydrogen bonds, as well as C—H...π contacts and C—Br...π halogen bonds. The structure of the substituent attached in the 7-position of the naphthyridine skeleton has a fundamental influence on the pattern of intermolecular noncovalent bonding. While the Br atom of (I participates in weak C—Br...Oguest and C—Br...π contacts, the Br atoms of compound (II are involved in host–host interactions via C—Br...O=C, C—Br...N and C—Br...π bonding.

  7. Bis[μ-1,2-bis(1H-imidazol-1-ylmethylbenzene-κ2N3:N3′]disilver(I 3-carboxylato-4-hydroxybenzenesulfonate methanol solvate trihydrate

    Directory of Open Access Journals (Sweden)

    Hong-Mei Sun

    2009-09-01

    Full Text Available In the title compound, [Ag2(C14H14N42](C7H4O6S·CH3OH·3H2O, the complex dication has a binuclear structure in which each AgI ion is two-coordinated in a slightly distorted linear coordination geometry. The two AgI atoms are bridged by two 1,2-bis[(1H-imidazol-1-ylmethyl]benzene (IBI ligands, forming a 22-membered ring. In the dication, π–π interactions are observed between the imidazole rings with centroid–centroid distances of 3.472 (3 and 3.636 (3 Å. In the crystal, the uncoordinated water molecules, anions and methanol solvent molecules are linked into chains along the b axis by O—H...O hydrogen bonds. In addition, π–π interactions are observed between the benzene rings of the IBI ligands, with a centroid–centroid distance of 3.776 (2 Å. The sulfonate group is disordered over two orientations with occupancies of 0.676 (12 and 0.324 (12.

  8. Copper interactions in TlCu7S4 and TlCu7Se4

    International Nuclear Information System (INIS)

    Noren, L.; Delaplane, R.G.; Berger, R.

    1999-01-01

    Complete text of publication follows. The copper chalcogenides ACu 7 S 4 (A=NH 4 + , Tl + , Rb + ) are quasi-one-dimensional metals at ambient and higher temperatures which is due to the high mobility of copper in these structures. TlCu 7 S 4 and TlCu 7 Se 4 are isostructural compounds, space group I4/m, which can be described on the basis of a TlX 8 cube with two different Cu sites, Cu(1) and Cu(2). Cu(2)-Cu(2) zigzag chains run along the c axis with only 3/4 occupation of the Cu(2) sites. However, these two compounds differ in behaviour on cooling. The sulphide shows a polymorphic first-order transition to the CsAg 7 S 4 type (P4/n) owing to ordering of the vacancies in the Cu(2)-Cu(2) chains. In order to study the nature of the Cu(2) order/disorder in the two title compounds, a series of neutron diffraction measurements (both Bragg and diffuse scattering) were made at several temperatures from 40 to 713 K on the instrument SLAD at Studsvik. The structure at each temperature was modelled using RMC techniques. The resulting configuration show that as the temperature increases, there is a marked increase in the mobility of the Cu atoms in the Cu(2)-Cu(2) chains for TlCu 7 S 4 but not for TlCu 7 Se 4 . This is due to the initial difference in the Cu(2)-Cu(2) distances, only 2.2A for the thiocuprate, but 2.7A in the selenocuprate which explains the relative ease for Cu(2) ordering in the latter case. (author)

  9. Crystal structure of bis{μ2-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diylbis(methylene]bis(4-oxo-4H-pyran-3-olato}dicobaltcalcium bis(perchlorate 1.36-hydrate

    Directory of Open Access Journals (Sweden)

    Patrizia Rossi

    2017-12-01

    Full Text Available The title compound, [CaCo2(C22H30N4O62](ClO42·1.36H2O or {Ca[Co(H–2L1]2}·2ClO4·1.36H2O {where L1 is 4,10-bis[(3-hydroxy-4-pyron-2-ylmethyl]-1,7-dimethyl-1,4,7,10-tetraazacyclododecane}, is a trinuclear complex whose asymmetric unit comprises a quarter of the {Ca[Co(H–2L1]2}2+ trinuclear complex, half of a perchlorate ion and 0.34-water molecules. In the neutral [Co(H–2L1] moiety, the cobalt ion is hexacoordinated in a trigonal–prismatic fashion by the surrounding N4O2 donor set. A Ca2+ cation holds together two neutral [Co(H–2L1] moieties and is octacoordinated in a distorted trigonal–dodecahedral fashion by the surrounding O atoms belonging to the deprotonated oxide and carbonyl groups of two [Co(H–2L1] units. The coordination of the CoII cation preorganizes L1 and an electron-rich area forms, which is able to host hard metal ions. The comparison between the present structure and the previously published ones suggests a high versatility of this ligand; indeed, hard metal ions with different nature and dimensions lead to complexes having different stoichiometry (mono- and dinuclear monomers and trinuclear dimers or even a polymeric structure. The heterotrinuclear CoII–CaII–CoII complexes are connected in three dimensions via weak C—H...O hydrogen bonds, which are also responsible for the interactions with the perchlorate anions and the lattice water molecules. The perchlorate anion is disordered about a twofold rotation axis and was refined giving the two positions a fixed occupancy factor of 0.5. The crystal studied was refined as a two-component inversion twin [BASF parameter = 0.14 (4].

  10. 57Fe Moessbauer and magnetization study of the Th7Fe3 and the hydride Th7Fe3H/sub n/

    International Nuclear Information System (INIS)

    Viccaro, P.J.; Shenoy, G.K.; Dunlap, B.D.; Westlake, D.G.; Malik, S.K.; Wallace, W.E.

    1978-01-01

    Th 7 Fe 3 is known to be a Pauli paramagnet and to undergo a superconducting transition at 1.86K. Its hydride Th 7 Fe 3 H/sub n/ is shown to possess magnetic ordering. The 57 Fe saturated hyperfine field in the hydride is estimated to be aproximately 20kG. A positive isomer shift of 0.30 +- 0.02 mm/s at 300 K relative to Th 7 Fe 3 would be consistent with an increase in d-like electrons on Fe. Preliminary magnetization results indicate a magnetic moment of about 0.5 μ/sub B/ for the hydride and a transition temperature near 300 K

  11. (1R,4R,6S,7R-5,5-Dibromo-1,4,8,8-tetramethyltricyclo[5.4.1.04,6]dodecan-12-one

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    Mohamed Zaki

    2014-05-01

    Full Text Available The title compound, C16H24Br2O, was synthesized from the reaction of β-himachalene (3,5,5,9-tetramethyl-2,4a,5,6,7,8-hexahydro-1H-benzocycloheptene, which was isolated from Atlas cedar (Cedrus atlantica. The asymmetric unit contains two independent molecules with similar conformations. Each molecule is built up from two fused seven-membered rings and an additional three-membered ring. In both molecules, one of the seven-membered rings has a chair conformation, whereas the other displays a screw-boat conformation.

  12. Poly[[[[1-ethyl-6,8-difluoro-7-(3-methylpiperazin-1-yl-4-oxo-1,4-dihydroquinoline-3-carboxylato]cadmium]-μ-benzene-1,4-dicarboxylato] trihydrate

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    Xin-Ping Kang

    2010-11-01

    Full Text Available In the title layered coordination polymer, {[Cd(C17H18F2N3O3(C8H4O4]·3H2O}n, the CdII atom exhibits a very distorted CdO6 octahedral geometry defined by one O3,O4-bidentate 1-ethyl-6,8-difluoro-7-(3-methylpiperazin-1-yl-4-oxo-1,4-dihydroquinoline-3-carboxylate (lome ligand, one O,O′-bidentate benzene-1,4-dicarboxylate (bdc dianion and two O-monodentate bdc dianions. Both the bdc species in the asymmetric unit are completed by crystallographic inversion symmetry. The bridging bdc dianions link the cadmium nodes into a rectangular grid lying parallel to (01overline{1}. A network of N—H...O and O—H...O hydrogen bonds helps to establish the packing.

  13. (E-Methyl 3-(3,4-dimethoxyphenyl-2-[(1,3-dioxoisoindolin-2-ylmethyl]acrylate

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    D. Kannan

    2012-04-01

    Full Text Available In the title compound, C21H19NO6, the isoindole ring system is essentially planar [maximum deviation = 0.019 (2 Å for the N atom] and is oriented at a dihedral angle of 51.3 (1° with respect to the benzene ring. The two methoxy groups are almost coplanar with the attached benzene ring [C—O—C—C = 3.7 (4 and 4.3 (4°]. The molecular conformation is stabilized by an intramolecular C—H...O hydrogen bond, which generates an S(9 ring motif. In the crystal, molecules are linked through bifurcated C—H...(O,O hydrogen bonds having R12(5 ring motifs, forming chains along the b-axis direction. The crystal packing is further stabilzed by π–π interactions [centriod–centroid distance = 3.463 (1 Å].

  14. Novel 2,3-Dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones: Synthesis and Biological Evaluation

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    Malose J. Mphahlele

    2016-12-01

    Full Text Available Herein we describe the synthesis and evaluation of a series of novel 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones for in vitro cytotoxicity against three human cancer cell lines as well as for potential antimalarial activity against the chloroquine-sensitive strain 3D7 of Plasmodium falciparum. The title compounds were prepared via PdCl2-mediated endo-dig cyclization of 2-aryl-8-(arylethynyl-6-bromo-2,3-dihydroquinazolin-4(1H-ones. The latter were prepared, in turn, via initial Sonogashira cross-coupling of 2-amino-5-bromo-3-iodobenzamide with aryl acetylenes followed by boric acid-mediated cyclocondensation of the intermediate 2-amino-3-(arylethynyl-5-bromobenzamides with benzaldehyde derivatives. The 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones 4a–k were evaluated for potential in vitro cytotoxicity against the breast (MCF-7, melanoma (B16 and endothelioma (sEnd.2 cell lines. All of the compounds except 4h and 4i were found to be inactive against the three cancer cell lines. Compound 4h substituted with a 4-methoxyphenyl and 4-fluorophenyl groups at the 3- and 5-positions was found to exhibit significant cytotoxicity against the three cancer cell lines. The presence of phenyl and 3-chlorophenyl groups at the 3- and 5-posiitons of the pyrroloquinazolinone 4i, on the other hand, resulted in significant cytotoxicity against vascular tumour endothelial cells (sEnd.2, but reduced activity against the melanoma (B16 and breast cancer (MCF-7 cells except at higher concentrations. The 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones 4a–l were found to be inactive against the chloroquine sensitive 3D7 strain of Plasmodium falciparum.

  15. Design and syntheses of hybrid metal-organic materials based on K3[M(C2O4)33H2O [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)33H2O [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.

  16. Ethyl 2-[4-(benzyloxyanilino]-4-oxo-4,5-dihydrofuran-3-carboxylate

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    S. Sriman Narayanan

    2008-12-01

    Full Text Available In the title compound, C20H19NO5, the dihydrofuran ring is almost planar [maximum deviation of 0.021 (2°] and makes dihedral angles of 28.1 (7 and 54.5 (5° with the benzyl and phenylamino rings, respectively. The molecular packing is stabilized by intramolecular N—H...O hydrogen bonds and intermolecular C—H...O interactions.

  17. 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.

  18. Fatores perinatais associados a recém-nascidos de termo com pH<7,1 na artéria umbilical e índice de Apgar <7,0 no 5º minuto Perinatal factors associated with pH<7.1 in umbilical artery and Apgar 5 min <7.0 in term newborn

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    Patrícia de Moraes De Zorzi

    2012-08-01

    Full Text Available OBJETIVO: Avaliar os fatores perinatais associados a recém-nascidos de termo com pHPURPOSE: To assess perinatal factors associated with term newborns with pH<7.1 in the umbilical artery and 5th min Apgar score<7,0. METHODS: Retrospective case-control study carried out after reviewing the medical records of all births from September/1998 to March/2008, that occurred at the General Hospital of Caxias do Sul. The inclusion criterion was term newborns who presented a 5th min Apgar score <7.0 and umbilical artery pH<7.10. In the univariate analysis, we used the Student's t-test and the Mann-Whitney test for continuous variables, the c² test for dichotomous variables and risk estimation by the odds ratio (OR. The level of significance was set at p<0.05. RESULTS: Of a total of 15,495 consecutive births, 25 term neonates (0.16% had pH<7.1 in the umbilical artery and a 5th min Apgar score <7.0. Breech presentation (OR=12.9, p<0.005, cesarean section (OR=3.5, p<0.01 and modified intrapartum cardiotocography (OR=7.8, p<0.02 presented a significant association with the acidosis event. Among the fetal characteristics, need for hospitalization in the neonatal intensive care unit (OR=79.7, p <0.0001, need for resuscitation (OR=12.2, p <0.0001 and base deficit were associated with the event (15.0 versus -4.5, p<0.0001. CONCLUSION: Low Apgar score at the 5th min of life associated with pH<7.1 in the umbilical artery can predict adverse neonatal outcomes.

  19. Effect of whey goat milk kefir on hydrophobicity of E. coli O157:H7, S. typhi bacteria and C. albicans

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    Dedi Fardiaz

    2012-03-01

    Full Text Available The hydrophobicity of bacteria. was determined using BATH (Bacteria adhesion to hydrocarbon test. All bacteria showed that 0,9 ml n-octane exposure gave a positive response and indicating that E. coli O157:H7 was categorized as moderate hydrophobic bacteria,  while S.  typhi  and C. albicans were catagorized as  highly hydrophobic bacteria. Goat Milk Kefir increased hydrophobicity of E.  coli O157:H7 by 24.40, however, decreased hydrophobicity of S. typhi by 47.56  and C. albicans by 70.14 percent, respectively. This finding showed that one of the inhibition mechanism may be caused by  an interaction  of  organic acid and peptide  compounds with cell membrane, in which hydrophobic sites of component  modified the hydrophobicity of the bacteria cell surface. The hydrophobicity modification in bacterial  cell wall might result inhibition of adhetion bacteria at cell host. Key words : Enterophatogenic bacteria, hidrophobisitas bacteria

  20. Identification and analytical characterization of six synthetic cannabinoids NNL-3, 5F-NPB-22-7N, 5F-AKB-48-7N, 5F-EDMB-PINACA, EMB-FUBINACA, and EG-018.

    Science.gov (United States)

    Liu, Cuimei; Jia, Wei; Hua, Zhendong; Qian, Zhenhua

    2017-08-01

    Clinical and forensic toxicology laboratories are continuously confronted by analytical challenges when dealing with the new psychoactive substances phenomenon. The number of synthetic cannabinoids, the chemical diversity, and the speed of emergence make this group of compounds particularly challenging in terms of detection, monitoring, and responding. Three indazole 7N positional isomer synthetic cannabinoids, two ethyl 2-amino-3-methylbutanoate-type synthetic cannabinoids, and one 9H-carbazole substituted synthetic cannabinoid were identified in seized materials. These six synthetic cannabinoid derivatives included: 1H-benzo[d] [1,2,3]triazol-1-yl 1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate (NNL-3, 1), quinolin-8-yl 1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate (5F-NPB-22-7N, 2), N-((1 s,3 s)-adamantan-1-yl)-1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxamide (5F-AKB-48-7N, 3), ethyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate (5F-EDMB-PINACA, 4), ethyl 2-(1-(4-fluorobenzyl)-1H-indazole-3-carboxamido)-3-methylbutanoate (EMB-FUBINACA, 5), and naphthalen-1-yl(9-pentyl-9H-carbazol-3-yl)methanone (EG-018, 6). The identification was based on ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry (UHPLC-QTOF-MS), gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance spectroscopy (NMR). The analytical characterization of these six synthetic cannabinoids was described, so as to assist forensic laboratories in identifying these compounds or other substances with similar structure in their case work. To our knowledge, no analytical data about the compounds 1-5 have appeared until now, making this the first report on these compounds. The GC-MS data of 6 has been reported, but this study added the LC-MS, NMR, and Fourier transform infrared (FTIR), data to render the analytical data collection process more complete. Copyright © 2017 John Wiley & Sons, Ltd

  1. Effect of interstitial nitrogen on magnetism and entropy change of LaFe11.7Si1.3 compound

    International Nuclear Information System (INIS)

    Balli, M.; Rosca, M.; Fruchart, D.; Gignoux, D.

    2009-01-01

    Crystal structure, magnetism and magnetocaloric properties of LaFe 11.7 Si 1.3 N y (y=0, 1.3) compounds have been studied by X-ray diffraction and magnetic measurements. The LaFe 11.7 Si 1.3 N y compounds present a cubic NaZn 13 -type structure. Insertion of 1.3 nitrogen atoms per LaFe 11.7 Si 1.3 formula increases the lattice parameter and Curie temperature from 11.467 to 11.733 A and from 190 to ∼230 K, respectively. Besides, the absorption of nitrogen drives drastically the magnetic transition from first to second order and accordingly strongly decreases the magnetocaloric effect compared to the parent alloy. Under an external field change of 5 T, the value of isothermal entropy change -ΔS is about 28 and 3.5 J/kg K for LaFe 11.7 Si 1.3 and LaFe 11.7 Si 1.3 N 1.3 , respectively, close to their Curie temperature. However, the relative cooling power RCP(S) of the nitride is about half that of the parent alloy

  2. 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.

  3. Carvacrol and p-cymene inactivate Escherichia coli O157:H7 in apple juice

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    Roller Sibel

    2005-06-01

    Full Text Available Abstract Background Outbreaks of food poisoning associated with drinking un-pasteurised apple juice contaminated with enterohaemorrhagic Escherichia coli O157:H7 are a cause of serious illness and occasionally death. Whilst a well-established heat process (pasteurisation will readily eliminate the pathogen, some consumers are demanding more fresh-like foods that have not been subjected to processing methods that are perceived as severe and may lead to loss of flavour and vitamins. Therefore, alternative methods are being investigated to replace pasteurisation and improve the safety of minimally-processed juices. The addition of natural antimicrobial substances such as the phenolic substances carvacrol and p-cymene (derived from the essential oils of herbs and spices provides a potential new route to assure safety and extend the shelf-life of raw fruit juices. The aim of this study was to evaluate the addition of very low concentrations (0.25–1.25 mM of carvacrol and p-cymene both individually and in combination as a novel means of controlling Escherichia coli O157:H7 in un-pasteurised apple juice. Results When inoculated at a level of 4 log CFU/ml into un-pasteurised apple juice (pH 3.20 ± 0.06, Escherichia coli O157:H7 survived for up to 3 and 19 days at 25° and 4°C, respectively. Treatment of the juice with 1.25 mM carvacrol or p-cymene reduced the numbers of E. coli O157:H7 to undetectable levels within 1–2 days at both storage temperatures. The effective concentrations of carvacrol could be reduced even further by combining it at 0.5 mM with cymene at 0.25 mM. The phenolic compounds were biocidal against both spoilage yeasts and E. coli O157:H7 thereby increasing the shelf-life and improving the safety of un-pasteurised apple juice, particularly when stored at chill temperatures. Conclusion The results showed that the natural antimicrobial compounds carvacrol and p-cymene could potentially be used to extend the shelf life and improve

  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. Anomalous misfit strain relaxation in ultrathin YBa2Cu3O7-δ epitaxial films

    International Nuclear Information System (INIS)

    Kamigaki, K.; Terauchi, H.; Terashima, T.; Bando, Y.; Iijima, K.; Yamamoto, K.; Hirata, K.; Hayashi, K.; Nakagawa, I.; Tomii, Y.

    1991-01-01

    Ultrathin YBa 2 Cu 3 O 7-δ epitaxial films were successfully grown in situ on (001) SrTiO 3 and MgO substrates by means of ozone-incorporating activated reactive evaporation. The x-ray-diffraction study was carefully examined to determine the structural properties of the grown films. Excellent crystallinity with no interfacial disorders was revealed by the appearance of the Laue oscillations. It was found that in a well lattice-matched YBa 2 Cu 3 O 7-δ /SrTiO 3 system, the crystallinity was deteriorated due to defect introduction at the critical layer thickness h c ( ∼ 130 A). Interestingly, also in a poorly lattice-matched YBa 2 Cu 3 O 7-δ /MgO system, excellent crystallinity was revealed even at above h c ( 2 Cu 3 O 7-δ /MgO system. In such a system, no crystal imperfection of the MgO substrate caused by defect introduction was elucidated by the grazing incidence x-ray scattering, which indicated that the MgO substrate did not contribute to the anomalous misfit relaxation. The anomalous growth manner was also found in YBa 2 Cu 3 O 7-δ /MgO according to surface morphology investigations. Below 40 A( > h c ), island nucleation growth was found. Above 40 A, it was observed that an atomically smooth surface was obtained and the crystallinity was simultaneously improved. It is suggested that YBa 2 Cu 3 O 7-δ possesses an anomalous misfit relaxation mechanism, and that especially in the growth on MgO, it couples with the characteristic growth behavior at the initial stage

  6. Minimum Requirements of Flagellation and Motility for Infection of Agrobacterium sp. Strain H13-3 by Flagellotropic Bacteriophage 7-7-1

    Science.gov (United States)

    Yen, Jiun Y.; Broadway, Katherine M.

    2012-01-01

    The flagellotropic phage 7-7-1 specifically adsorbs to Agrobacterium sp. strain H13-3 (formerly Rhizobium lupini H13-3) flagella for efficient host infection. The Agrobacterium sp. H13-3 flagellum is complex and consists of three flagellin proteins: the primary flagellin FlaA, which is essential for motility, and the secondary flagellins FlaB and FlaD, which have minor functions in motility. Using quantitative infectivity assays, we showed that absence of FlaD had no effect on phage infection, while absence of FlaB resulted in a 2.5-fold increase in infectivity. A flaA deletion strain, which produces straight and severely truncated flagella, experienced a significantly reduced infectivity, similar to that of a flaB flaD strain, which produces a low number of straight flagella. A strain lacking all three flagellin genes is phage resistant. In addition to flagellation, flagellar rotation is required for infection. A strain that is nonmotile due to an in-frame deletion in the gene encoding the motor component MotA is resistant to phage infection. We also generated two strains with point mutations in the motA gene resulting in replacement of the conserved charged residue Glu98, which is important for modulation of rotary speed. A change to the neutral Gln caused the flagellar motor to rotate at a constant high speed, allowing a 2.2-fold-enhanced infectivity. A change to the positively charged Lys caused a jiggly motility phenotype with very slow flagellar rotation, which significantly reduced the efficiency of infection. In conclusion, flagellar number and length, as well as speed of flagellar rotation, are important determinants for infection by phage 7-7-1. PMID:22865074

  7. 2-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]indane-1,3-dione

    Directory of Open Access Journals (Sweden)

    Abdullah M. Asiri

    2011-02-01

    Full Text Available The title compound 2-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-indane-1,3-dione (3 was synthesized in high yield by reaction of 3,5-dimethyl-1-phenyl-pyrazole-4-carbaldehyde and indane-1,3-dione in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H NMR, 13C NMR and GC-MS spectral analysis.

  8. Solvent-Dependent Delamination, Restacking, and Ferroelectric Behavior in a New Charge-Separated Layered Compound: [NH4 ][Ag3 (C9 H5 NO4 S)2 (C13 H14 N2 )2 ]⋅8 H2 O.

    Science.gov (United States)

    Sushrutha, Sringeri Ramesh; Mohana, Shivanna; Pal, Somnath; Natarajan, Srinivasan

    2017-01-03

    A new anionic coordination polymer, [NH 4 ][Ag 3 (C 9 H 5 NO 4 S) 2 (C 13 H 14 N 2 ) 2 ]⋅8 H 2 O, with a two-dimensional structure, has been synthesized by a reaction between silver nitrate, 8-hydroxyquinoline-5-sulfonic acid (HQS), and 4,4'-trimethylene dipyridine (TMDP). The compound stabilizes in a noncentrosymmetric space group, and the lattice water molecules and the charge-compensating [NH 4 ] + group occupy the inter-lamellar spaces. The lattice water molecules can be fully removed and reinserted, which is accompanied by a crystalline-amorphous-crystalline transformation. This transformation resembles the collapse/delamination and restacking of the layers. To the best of our knowledge, this is the first observation of delamination and restacking in an inorganic coordination polymer that contains silver. The presence of a natural dipole (the anionic framework and cationic ammonium ions) along with the noncentrosymmetric space group gives rise to the room-temperature ferroelectric behavior of the compound. The ferroelectric behavior is also water-dependent and exhibits a ferroelectric-paraelectric transformation. The temperature-dependent dielectric measurements indicate that the ferroelectric/ paraelectric transformation occurs at 320 K. This transformation has also been investigated by using in-situ IR spectroscopy and PXRD studies. The second-harmonic generation (SHG) study indicated values that are comparable to some of the known SHG solids, such as potassium dihydrogen phosphate (KDP) and urea. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Thermal reactivity of some nitro- and nitroso-compounds derived from 1,3,5,7-tetraazabicyclo[3.3.1]nonane at contamination by ammonium nitrate.

    Science.gov (United States)

    Zeman, Svatopluk; Shu, Yuanjie; Friedl, Zdenek; Vágenknecht, Jirí

    2005-05-20

    Thermal reactivity of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT), 3,7-dinitroso-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DNPT), 1,3,5-trinitroso-1,3,5-triazinane (TMTA or R-salt), 1,3,5-trinitro-1,3,5-triazinane (hexogen or RDX), 1,5-diacetyl-3,7-dinitro-1,3,5,7-tetrazocane (DADN), alpha-modification of the 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (octogen or HMX) and of their mixtures with 2wt.% of ammonium nitrate (AN) has been examined by means of non-isothermal differential thermal analysis. The resulting data were analyzed according to the Kissinger method. The reactivity was expressed as the E(a)R(-1) slopes of the Kissinger relationship. A relatively high reactivity has been found with mixtures of DPT and DNPT with AN. Electronic charges q(N) at nitrogen atoms in molecules of the compounds studied were calculated by means of ab initio DFT B3LYP/6-31G** method. The relationships were confirmed between the slopes E(a)R(-1) and the q(N) values for the nitrogen atoms primarily undergoing reaction. On the basis of these relationships it is stated that the destabilizing effect of AN is due to acidolytic attack of nitric acid (resulting from dissociation of ammonium nitrate) at the nitrogen atoms with the most negative q(N) values in the molecules of the compounds studied.

  10. Search for resonant states in 10C and 11C and their impact on the primordial 7Li abundance

    Science.gov (United States)

    Hammache, F.; Coc, A.; de Séréville, N.; Stefan, I.; Roussel, P.; Assié, M.; Audouin, L.; Beaumel, D.; Franchoo, S.; Fernandez-Dominguez, B.; Fox, S.; Hamadache, C.; Kiener, J.; Laird, A.; Le Crom, B.; Lefebvre-Schuhl, A.; Lefebvre, L.; Matea, I.; Matta, A.; Mavilla, G.; Mrazek, J.; Morfouace, P.; de Oliveira Santos, F.; Parikh, A.; Perrot, L.; Sanchez-Benitez, A. M.; Suzuki, D.; Tatischeff, V.; Ujic, P.; Vandebrouck, Marine

    2018-01-01

    The cosmological 7Li problem arises from the significant discrepancy of about a factor 3 between the predicted primordial 7Li abundance and the observed one. The main process for the production of 7Li during Big-Bang nucleosynthesis is the decay of 7Be. Many key nuclear reactions involved in the production and destruction of 7Be were investigated in attempt to explain the 7Li deficit but none of them led to successful conclusions. However, some authors suggested recently the possibility that the destruction of 7Be by 3He and 4He may reconcile the predictions and observations if missing resonant states in the compound nuclei 10C and 11C exist. Hence, a search of these missing resonant states in 10C and 11C was investigated at the Orsay Tandem-Alto facility through 10B(3He,t)10C and 11B(3He,t)11C charge-exchange reactions respectively. After a short overview of the cosmological 7Li problem from a nuclear physics point of view, a description of the Orsay experiment will be given as well as the obtained results and their impact on the 7Li problem.

  11. Synthesis, crystal structure and characterization of a 1D polyoxometalate-based compound: {l_brace}[Pr(H{sub 2}O){sub 7}][CrMo{sub 6}H{sub 6}O{sub 24}]{r_brace} . 4H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Lijie; Shen Shuchang; Yu Haiming [Qiqihar Univ., HL (China). Dept. of Chemistry and Chemical Engineering

    2008-07-15

    A novel polyoxometalated-based compound, {l_brace}[Pr(H{sub 2}O){sub 7}][CrMo{sub 6}H{sub 6}O{sub 24}]{r_brace} . 4H{sub 2}O, was prepared and characterized by elemental analysis, infrared and ultraviolet spectroscopy, TG measurement and single crystal X-ray diffraction. A chain-like coordination polymer is formed from a heteropolyanion [CrMo{sub 6}H{sub 6}O{sub 24}]{sup 3} as a building unit and [Pr(H{sub 2}O){sub 7}]{sup 3+} cations as linker. The chains are linked into an extensive three-dimensional supramolecular network through hydrogen bonding. The synthesis of 1 is accomplished only from pre-synthesized Anderson clusters, but not from simple starting materials. (orig.)

  12. Crystal structure of a diaryl carbonate: 1,3-phenylene bis(phenyl carbonate

    Directory of Open Access Journals (Sweden)

    Marina A. Solomos

    2017-12-01

    Full Text Available The whole molecule of the title compound, C20H14O6, is generated by mirror symmetry, the mirror bisecting the central benzene ring. The carbonate groups adopt an s-cis-s-cis conformation, with torsion angles of 58.7 (2 and 116.32 (15°. The crystal structure of 1,3-phenylene bis(phenyl carbonate contains no strong hydrogen bonds, though weak C—H...O and offset π–π interactions are observed, forming layers parallel to the ac plane.

  13. Synthesis of R-(+)- and S-(-)-8-hydroxy-2-(N,N-dipropylamino)-2[2-3H]tetralin. HCl (8-OH-DPAT) a 5HT1A receptor agonist

    International Nuclear Information System (INIS)

    Ackland, M.J.; Dring, L.G.; Jones, J.R.

    1991-01-01

    The title compounds were synthesised in 7 steps from 1,7-dihydroxynaphthalene as follows: 1,7-dihydroxynaphthalene was methylated and subjected to a Birch reduction to yield 8-methoxy-2-tetralone. Reductive amination with sodium cyanoboro[ 3 H]hydride and n-propylamine gave 8-methoxy-2-(n-propylamino)-[2- 3 H]tetralin which was acylated and reduced to give (±)8-methoxy-2-(N,N-dipropylamino)-[2 3 H]tetralin. Treatment with conc.HC1 gave (±)-8-hydroxy-2-(N,N-dipropylamino)-[2- 3 H]tetralin. The racemate was then resolved by chiral mobile phase chromatography. (author)

  14. Novel compound heterozygous mutations in MYO7A Associated with Usher syndrome 1 in a Chinese family.

    Science.gov (United States)

    Gao, Xue; Wang, Guo-Jian; Yuan, Yong-Yi; Xin, Feng; Han, Ming-Yu; Lu, Jing-Qiao; Zhao, Hui; Yu, Fei; Xu, Jin-Cao; Zhang, Mei-Guang; Dong, Jiang; Lin, Xi; Dai, Pu

    2014-01-01

    Usher syndrome is an autosomal recessive disease characterized by sensorineural hearing loss, age-dependent retinitis pigmentosa (RP), and occasionally vestibular dysfunction. The most severe form is Usher syndrome type 1 (USH1). Mutations in the MYO7A gene are responsible for USH1 and account for 29-55% of USH1 cases. Here, we characterized a Chinese family (no. 7162) with USH1. Combining the targeted capture of 131 known deafness genes, next-generation sequencing, and bioinformatic analysis, we identified two deleterious compound heterozygous mutations in the MYO7A gene: a reported missense mutation c.73G>A (p.G25R) and a novel nonsense mutation c.462C>A (p.C154X). The two compound variants are absent in 219 ethnicity-matched controls, co-segregates with the USH clinical phenotypes, including hearing loss, vestibular dysfunction, and age-dependent penetrance of progressive RP, in family 7162. Therefore, we concluded that the USH1 in this family was caused by compound heterozygous mutations in MYO7A.

  15. Novel compound heterozygous mutations in MYO7A Associated with Usher syndrome 1 in a Chinese family.

    Directory of Open Access Journals (Sweden)

    Xue Gao

    Full Text Available Usher syndrome is an autosomal recessive disease characterized by sensorineural hearing loss, age-dependent retinitis pigmentosa (RP, and occasionally vestibular dysfunction. The most severe form is Usher syndrome type 1 (USH1. Mutations in the MYO7A gene are responsible for USH1 and account for 29-55% of USH1 cases. Here, we characterized a Chinese family (no. 7162 with USH1. Combining the targeted capture of 131 known deafness genes, next-generation sequencing, and bioinformatic analysis, we identified two deleterious compound heterozygous mutations in the MYO7A gene: a reported missense mutation c.73G>A (p.G25R and a novel nonsense mutation c.462C>A (p.C154X. The two compound variants are absent in 219 ethnicity-matched controls, co-segregates with the USH clinical phenotypes, including hearing loss, vestibular dysfunction, and age-dependent penetrance of progressive RP, in family 7162. Therefore, we concluded that the USH1 in this family was caused by compound heterozygous mutations in MYO7A.

  16. 45 CFR 7.3 - Determination as to domestic rights.

    Science.gov (United States)

    2010-10-01

    ... 45 Public Welfare 1 2010-10-01 2010-10-01 false Determination as to domestic rights. 7.3 Section 7.3 Public Welfare DEPARTMENT OF HEALTH AND HUMAN SERVICES GENERAL ADMINISTRATION EMPLOYEE INVENTIONS..., title, and interest in and to an invention which is or may be patentable, made by a Government employee...

  17. Selective labelling of 5-HT{sub 7} receptor recognition sites in rat brain using [{sup 3}H]5-carboxamidotryptamine

    Energy Technology Data Exchange (ETDEWEB)

    Stowe, R.L.; Barnes, N.M. [Department of Pharmacology, The Medical School, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)

    1998-12-01

    The aim of the present study was to establish a radioligand binding assay to selectively label the native 5-HT{sub 7} receptor expressed in rat brain. In rat whole brain (minus cerebellum and striatum) homogenate, ({+-})-pindolol (10 {mu}M)-insensitive [{sup 3}H]5-CT ([{sup 3}H]5-carboxamidotryptamine; 0.5 nM) specific binding (defined by 5-HT, 10 {mu}M) displayed a pharmacological profile similar to the recombinant 5-HT{sub 7} receptor, although the Hill coefficients for competition curves generated by methiothepin, ritanserin, sumatriptan, clozapine and pimozide were significantly less than unity. In homogenates of rat hypothalamus, ({+-})-pindolol (10 {mu}M)-insensitive [{sup 3}H]5-CT recognition sites also resembled, pharmacologically, the 5-HT{sub 7} receptor, although pimozide still generated Hill coefficients significantly less than unity. Subsequent studies were performed in the additional presence of WAY100635 (100 nM) to prevent [{sup 3}H]5-CT binding to residual, possibly, 5-HT{sub 1A} sites. Competition for this [{sup 3}H]5-CT binding indicated the labelling in whole rat brain homogenate of a homogenous population of sites with the pharmacological profile of the 5-HT{sub 7} receptor. Saturation studies also indicated that ({+-})-pindolol (10 {mu}M)/WAY 100635 (100 nM)-insensitive [{sup 3}H]5-CT binding to homogenates of whole rat brain was saturable and to an apparently homogenous population of sites which were labelled with nanomolar affinity (B{sub max}=33.2{+-}0.7 fmol mg{sup -1} protein, pK{sub d}=8.78{+-}0.05, mean{+-}S.E.M., n=3). The development of this 5-HT{sub 7} receptor binding assay will aid investigation of the rat native 5-HT{sub 7} receptor. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  18. (3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione

    Directory of Open Access Journals (Sweden)

    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.

  19. Synthesis of Novel 2-(Substituted aminoalkylthiopyrimidin-4(3H-ones as Potential Antimicrobial Agents

    Directory of Open Access Journals (Sweden)

    Mohamed I. Attia

    2013-12-01

    Full Text Available 5-Alkyl-6-(substituted benzyl-2-thiouracils 3a,c were reacted with (2-chloroethyl diethylamine hydrochloride to afford the corresponding 2-(2-diethylaminoethylthiopyrimidin- 4(3H-ones 4a,b. Reaction of 3a–c with N-(2-chloroethylpyrrolidine hydrochloride and/or N-(2-chloroethylpiperidine hydrochloride gave the corresponding 2-[2-(pyrrolidin-1-ylethyl]-thiopyrimidin-4(3H-ones 5a–c and 2-[2-(piperidin-1-ylethyl]thiopyrimidin-4(3H-ones 6a,b, respectively. Treatment of 3a–d with N-(2-chloroethylmorpholine hydrochloride under the same reaction conditions formed the corresponding 2-[2-(morpholin-4-ylethyl]thiopyrimidines 6c–f. On the other hand, 3a,b were reacted with N-(2-bromoethylphthalimide and/or N-(3-bromopropylphthalimide to furnish the corresponding 2-[2-(N-phthalimidoethyl]-pyrimidines 7a,b and 2-[3-(N-phthalimido-propyl]pyrimidines 7c,d, respectively. Compounds 3a–d, 4a,b, 5a–c, 6a–f and 7a–d were screened against Gram-positive bacteria (Staphylococcus aureus ATCC 29213, Bacillus subtilis NRRL 4219 and Bacillus cereus, yeast-like pathogenic fungus (Candida albicans ATCC 10231 and a fungus (Aspergillusniger NRRL 599. The best antibacterial activity was displayed by compounds 3a, 3b, 4a, 5a, 5b, 6d, 6f, 7b and 7d, whereas compounds 4b, 5b, 5c, 6a, 6b and 6f exhibited the best antifungal activity.

  20. Functionalized Fullerene Targeting Human Voltage-Gated Sodium Channel, hNav1.7.

    Science.gov (United States)

    Hilder, Tamsyn A; Robinson, Anna; Chung, Shin-Ho

    2017-08-16

    Mutations of hNa v 1.7 that cause its activities to be enhanced contribute to severe neuropathic pain. Only a small number of hNa v 1.7 specific inhibitors have been identified, most of which interact with the voltage-sensing domain of the voltage-activated sodium ion channel. In our previous computational study, we demonstrated that a [Lys 6 ]-C 84 fullerene binds tightly (affinity of 46 nM) to Na v Ab, the voltage-gated sodium channel from the bacterium Arcobacter butzleri. Here, we extend this work and, using molecular dynamics simulations, demonstrate that the same [Lys 6 ]-C 84 fullerene binds strongly (2.7 nM) to the pore of a modeled human sodium ion channel hNa v 1.7. In contrast, the fullerene binds only weakly to a mutated model of hNa v 1.7 (I1399D) (14.5 mM) and a model of the skeletal muscle hNa v 1.4 (3.7 mM). Comparison of one representative sequence from each of the nine human sodium channel isoforms shows that only hNa v 1.7 possesses residues that are critical for binding the fullerene derivative and blocking the channel pore.