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Sample records for title compound c22h17no3s

  1. (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.

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

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    Islam Ullah Khan

    2012-07-01

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

  3. (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.

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

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    Makuteswaran Sridharan

    2008-11-01

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

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

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    Peng Zhang

    2008-02-01

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

  6. 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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  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

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    Goverdhan Mehta

    2012-12-01

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

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

    Science.gov (United States)

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

    2017-02-01

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

  10. 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.

  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. Low-temperature heat capacities and standard molar enthalpy of formation of N-methylnorephedrine C211H17NO(s)

    Institute of Scientific and Technical Information of China (English)

    Di You-Ying; Wang Da-Qi; Shi Quan; Tan Zhi-Cheng

    2008-01-01

    This paper reports that low-temperature heat capacities of N-methylnorephedrine C11H17NO(s) have been mea- sured by a precision automated adiabatic calorimeter over the temperature range from T=78 K to T=400 K. A solid to liquid phase transition of the compound was found in the heat capacity curve in the temperature range of T=342- 364 K. The peak temperature, molar enthalpy and entropy of fusion of the substance were determined. The experimental values of the molar heat capacities in the temperature regions of T=78-342 K and T=364-400 K were fitted to two poly- nomial equations of heat capacities with the reduced temperatures by least squares method. The smoothed molar heat capacities and thermodynamic functions of N-methylnorephedrine C11H17NO(s) relative to the standard refer- ence temperature 298.15 K were calculated based on the fitted polynomials and tabulated with an interval of 5 K. The constant-volume energy of combustion of the compound at T=298.15 K was measured by means of an isoperibol preci- sion oxygen-bomb combustion calorimeter. The standard molar enthalpy of combustion of the sample was calculated. The standard molar enthalpy of formation of the compound was determined from the combustion enthalpy and other auxiliary thermodynamic data through a Hess thermochemical cycle.

  13. [(4S,5S-2,2-Dimethyl-1,3-dioxolane-4,5-diyl]bis[N-(thiophen-2-ylmethylidenemethanamine

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    Yan Jiang

    2012-02-01

    Full Text Available In the title compound, C17H20N2O2S2, the five-membered heterocycle exhibits an envelope conformation and the molecular chirality and configuration are well preserved from l-tartaric acid. The dihedral angle between the two thiophene rings is 17.0 (2°. In the crystal, molecules are linked by C—H...O and C—H...S hydrogen interactions, which are effective in the stabilization of the crystal structure.

  14. 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.

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

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    Dai Jing

    2009-06-01

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

  16. 1-Methyl-1H-2,1-benzothiazin-4(3H-one 2,2-dioxide

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    Muhammad Nadeem Arshad

    2008-03-01

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

  17. 3H-1,2-Benzodithiole-3-thione

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    Khaled Boukebbous

    2016-10-01

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

  18. Crystal structures of bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocobaltate and tetrachloridocuprate

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    Eric Gauchat

    2017-01-01

    Full Text Available (9S,13S,14S-3-Methoxy-17-methylmorphinan (dextromethorphan forms two isostructural salts with (a tetrachloridocobaltate, namely bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocobaltate, (C18H26NO2[CoCl4], and (b tetrachloridocuprate, namely bis[(9S,13S,14S-3-methoxy-17-methylmorphinanium] tetrachloridocuprate, (C18H26NO2[CuCl4]. The distorted tetrahedral anions are located on twofold rotational axes. The dextromethorphan cation can be described as being composed of two ring systems, a tetrahydronaphthalene system A+B and a decahydroisoquinolinium subunit C+D, that are nearly perpendicular to one another: the angle between mean planes of the A+B and C+D moieties is 78.8 (1° for (a and 79.0 (1° for (b. Two symmetry-related cations of protonated dextromethorphan are connected to the tetrachloridocobaltate (or tetrachloridocuprate anions via strong N—H...Cl hydrogen bonds, forming neutral ion associates. These associates are packed in the (001 plane with no strong attractive bonding between them. Both compounds are attractive crystalline forms for unambiguous identification of the dextromethorphan and, presumably, of its optical isomer, levomethorphan.

  19. (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°.

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

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    Andrii I. Buvailo

    2012-12-01

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

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

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    Peter G. Jones

    2010-01-01

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

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

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    Muhammad Hafeez

    2013-12-01

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

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

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    Hakima Chicha

    2014-06-01

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

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

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    Krzysztof Lyczko

    2013-01-01

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

  5. 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.

  6. 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.

  7. 2,2-Dimethyl-2,3-dihydro-1H-perimidine

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    Sarah Maloney

    2013-02-01

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

  8. 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.

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

    Institute of Scientific and Technical Information of China (English)

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

    2011-01-01

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

  10. 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)

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

    Directory of Open Access Journals (Sweden)

    Jing Zhao

    2012-06-01

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

  12. 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

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

    Directory of Open Access Journals (Sweden)

    Vijayan Viswanathan

    2017-05-01

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

  14. /sup 13/C, /sup 17/O, and /sup 33/S NMR spectra of alkyl phenyl sulfones C/sub 6/H/sub 5/SO/sub 2/Alk

    Energy Technology Data Exchange (ETDEWEB)

    Bzhezovskii, V.M.; Valeev, R.B.; Kalabin, G.A.; Aliev, I.A.

    1987-06-20

    The /sup 13/C, /sup 17/O, and /sup 33/S NMR spectra of alkyl phenyl sulfones C/sub 6/H/sub 5/SO/sub 2/Alk were obtained. The changes in the screening of the /sup 13/C, /sup 17/O, and /sup 33/S nuclei in these compounds are determined by the effect of the alkyl substituents, which alternates in sign and decreases along the chain of atoms in the order: CH/sub 3/, C/sub 2/H/sub 5/, iso-C/sub 3/H/sub 7/, and tert-C/sub 4/H/sub 9/. In the alkyl phenyl sulfides C/sub 6/H/sub 5/SAlk the additional effect of disruption in the p,..pi.. interaction between the sulfur atom and the benzene ring as a result of conformational changes is superimposed on the screening of the /sup 13/C/sup ortho/ nuclei. For the changes in the screening of the /sup 13/C/sup para/ nuclei in C/sub 6/H/sub 5/SAlk the steric disruption of the p,..pi.. conjugation by the alkyl substituents is determining.

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

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    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.

  16. 1,4-Dihydroxyquinoxaline-2,3(1H,4H-dione

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    Wolfgang Frey

    2008-03-01

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

  17. 3-Ethyl-4-[(E-(4-fluorobenzylideneamino]-1H-1,2,4-triazole-5(4H-thione

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    Alphonsus D'souza

    2012-05-01

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

  18. N-[(2S-4-Chloro-2-(l-menthyloxy-5-oxo-2,5-dihydro-3-furyl]-l-alanine

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    Kai Yang

    2009-05-01

    Full Text Available The title compound, C17H26ClNO5, was prepared via a tandem asymmetric Michael addition–elimination reaction of (5S-3,4-dichloro-5-(l-menthyloxyfuran-2(5H-one and l-alanine in the presence of potassium hydroxide. The five-membered furanone ring is approximately planar while the six-membered menthyloxy ring adopts a chair conformation. The crystal packing is stabilized by intermolecular O—H...O and N—H...O hydrogen bonds.

  19. 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.

  20. DFT studies on the mechanism of the reaction of C2H5S with NO2

    Science.gov (United States)

    Tang, Yi-Zhen; Sun, Hao; Pan, Ya-Ru; Pan, Xiu-Mei; Wang, Rong-Shun

    The mechanisms for the reaction of C2H5S with NO2 are investigated at the QCISD(T)/6-311++G(d, p)//B3LYP/6-311++G(d, p) level on both single and triple potential energy surfaces. The geometries, vibrational frequencies and zero-point energy (ZPE) corrections of all stationary points involved in the title reaction are calculated at the B3LYP/6-311++G(d, p) level. The results show that the reaction is more predominant on the single potential energy surface, while it is negligible on the triple potential energy surface. Without barrier height in the whole process, the major channel is R ? C2H5SONO (IM1 and IM2) ? P1 (C2H5SO+NO). With much heat released in the formation of C2H5SNO2 (IM3) and the transition state involved in the subsequent step more stable than reactants, P4 (CH3CHS + t-HONO) is subdominant product energetically.

  1. Crystal structure of 2-(4-chlorophenyl-3-(4-methoxyphenyl-3-(methylsulfanylacrylonitrile

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    Shamantha Kumar

    2014-11-01

    Full Text Available In the title compound, C17H14ClNOS, the aromatic rings are inclined to one another by 64.22 (9°. The acrylonitrile group (C=C—C[triple-bond]N is planar to within 0.003 (2 Å, with the S atom and the methyl C atom displaced from this plane by 0.2317 (6 and −0.637 (2 Å, respectively. In the crystal, molecules are linked via pairs of C—H...π interactions, forming inversion dimers. There are no other significant intermolecular interactions present.

  2. 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.

  3. 22 CFR 17.3 - Fault.

    Science.gov (United States)

    2010-04-01

    ... 22 Foreign Relations 1 2010-04-01 2010-04-01 false Fault. 17.3 Section 17.3 Foreign Relations...) § 17.3 Fault. A recipient of an overpayment is without fault if he or she performed no act of... agency may have been at fault in initiating an overpayment will not necessarily relieve the individual...

  4. (Carbonyl-1κC)bis-[2,3(η)-cyclo-penta-dien-yl][μ(3)-(S-methyl trithio-carbonato)methylidyne-1:2:3κC,S'':C:C](triphenyl-phosphine-1κP)(μ(3)-sulfido-1:2:3κS)dicobalt(II)iron(II) trifluoro-methane-sulfonate.

    Science.gov (United States)

    Manning, Anthony R; McAdam, C John; Palmer, Anthony J; Simpson, Jim

    2008-04-10

    The asymmetric unit of the title compound, [FeCo(2)(C(5)H(5))(2)(C(3)H(3)S(3))S(C(18)H(15)P)(CO)]CF(3)SO(3), consists of a triangular irondicobalt cluster cation and a trifluoro-methane-sulfonate anion. In the cation, the FeCo(2) triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithio-carbonate residue that bridges the Fe-C bond. Each Co atom carries a cyclo-penta-dienyl ligand while the Fe atom coordinates to one carbonyl and one triphenyl-phosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C-H⋯O and C-H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) inter-actions. The structure is further stabilized by additional inter-molecular C-H⋯O, C-H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) inter-action (S⋯centroid distance = 3.385 Å), generating an extended network.

  5. Crystal structure of (1S,3R,8R,10S-2,2-dichloro-10-hydroxy-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodecan-9-one

    Directory of Open Access Journals (Sweden)

    Ahmed Benzalim

    2016-05-01

    Full Text Available The asymmetric unit of the title compound, C16H24Cl2O2, contains two independent molecules (A and B which are built from three fused rings, viz. a seven-membered heptane ring, a six-membered cyclohexyl ring bearing a ketone and an alcohol group, and a cyclopropane ring bearing two Cl atoms. In the crystal, the two molecules are linked via two O—H...O hydrogen bonds, forming an A–B dimer with an R22(10 ring motif. The A molecules of these dimers are linked via a C—H...O hydrogen bond, forming chains propagating along the a-axis direction. Both molecules have the same absolute configuration, i.e. 1S,3R,8R,10S, which is based on the synthetic pathway and further confirmed by resonant scattering [Flack parameter = 0.03 (5].

  6. (4S)-4-(3,4-Dichloro?phen?yl)-1?-methyl-4?-phenyl-3,4-dihydronaphthalene-2-spiro-3?-pyrrolidine-2?-spiro-1??-acenaphthyl?ene-1,2??(2H,1??H)-dione

    OpenAIRE

    Murugan, R.; Gunasekaran, B.; Narayanan, S. Sriman; Manivannan, V.

    2008-01-01

    In the title compound, C37H27Cl2NO2, the 3,4-dichloro?phenyl ring makes a dihedral angle of 46.66?(6)? with the phenyl ring. The mol?ecular structure is stabilized by weak intra?molecular C?H?O inter?actions and the crystal structure is stabilized by weak inter?molecular C?H?O inter?actions. The C?C?C?C?C five-membered ring is planar, while the C?C?C?C?N five-membered ring adopts a half-chair conformation.

  7. 2-(2-Pyridylpyridinium (2,2′-bipyridine-κ2N,N′tetrakis(nitrato-κ2O,O′bismuthate(III

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    Shu-Shen Zhang

    2011-10-01

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

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

    Directory of Open Access Journals (Sweden)

    T. Thanh Van Tran

    2016-05-01

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

  9. 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.

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

    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.

  11. Dipropyl 3,6-diphenyl-1,2-dihydro-1,2,4,5-tetrazine-1,2-dicarboxylate.

    Science.gov (United States)

    Rao, Guo-Wu; Hu, Wei-Xiao

    2003-05-01

    The title compound, C(22)H(24)N(4)O(4), was prepared from propyl chloroformate and 3,6-diphenyl-1,2-dihydro-s-tetrazine. This reaction yields the title compound rather than dipropyl 3,6-diphenyl-1,4-dihydro-s-tetrazine-1,4-dicarboxylate. The 2,3-diazabutadiene group in the central six-membered ring is not planar; the C=N double-bond length is 1.285 (2) A, and the average N-N single-bond length is 1.401 (3) A, indicating a lack of conjugation. The ring has a twist conformation, in which adjacent N atoms lie +/- 0.3268 (17) A from the plane of the ring. The molecule has twofold crystallographic symmetry.

  12. 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.

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

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    Zhe An

    2009-04-01

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

  14. 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

  15. 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.

  16. (2-Oxo-2H-benzo[h]chromen-4-ylmethyl morpholine-4-carbodithioate

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    Rajni Kant

    2012-04-01

    Full Text Available In the title compound, C19H17NO3S2, the morpholine ring is in a chair conformation. In the coumarin ring system, the dihedral angle between the benzene and pyran rings is 3.9 (1°. In the crystal, weak C—H...O interactions link the molecules into corrugated layers parallel to (102. The crystal packing also exhibits π–π interactions, with distances of 3.644 (1 and 3.677 (1 Å between the centroids of the benzene rings of neighbouring molecules.

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

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    Wolfgang Holzer

    2010-09-01

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

  18. 4-{(E-[2-(4-Iodobutoxybenzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one

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    Hoong-Kun Fun

    2010-07-01

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

  19. (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.

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

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    Eyad Mallah

    2015-01-01

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

  1. (E-5,6-Dimethoxy-2-(pyridin-4-ylmethylidene-2,3-dihydro-1H-inden-1-one

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    Mohamed Ashraf Ali

    2010-11-01

    Full Text Available The molecule of the title compound, C17H15NO3, is slightly twisted, with a dihedral angle of 12.12 (3° between the dihydroindenone group and the pyridine ring. In the crystal, molecules are connected into layers parallel to the ab plane via intermolecular C—H...O hydrogen bonds. Weak π–π [centroid–centroid distance = 3.5680 (6 Å] interactions are also observed.

  2. 2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide

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    B. Narayana

    2013-01-01

    Full Text Available In the crystal structure of the title compound, C19H17Cl2N3O2, the molecules form dimers of the R22(10 type through N—H...O hydrogen bonding. As a result of steric repulsion, the amide group is rotated with respect to both the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 80.70 (13 and 64.82 (12°, respectively. The dihedral angle between the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings is 48.45 (5° while that between the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings is 56.33 (6°.

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

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    Tara Shahani

    2011-02-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  5. 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.

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

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    Omar bin Shawkataly

    2010-08-01

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

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

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    Narsimha Reddy Penthala

    2009-08-01

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

  8. 9-Benzyl-6-benzylsulfanyl-9H-purin-2-amine

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    Maywan Hariono

    2014-03-01

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

  9. Novel 2D or 3D alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand

    Science.gov (United States)

    Du, Zi-Yi; Wen, He-Rui; Xie, Yong-Rong

    2008-11-01

    Three novel alkaline-earth metal sulfonate-phosphonates based on [O 3S-C 2H 4-PO 3H] 2- ligand, namely, [Ca(O 3SC 2H 4PO 3H)(H 2O) 2] ( 1), [Sr(O 3SC 2H 4PO 3H)] ( 2) and [Ba 2(O 3SC 2H 4PO 3H) 2] ( 3), have been synthesized by hydrothermal reactions. They represent the first structurally characterized alkaline-earth metal complexes of phosphonic acid attached with a sulfonate group. The structure of compound 1 features a 2D layer based on 1D chains of [Ca 2(PO 3) 2] bridged by -CH 2-CH 2-SO 3- groups. Compounds 2 and 3 show pillar-layer architecture based on two different inorganic layers linked by -CH 2-CH 2- groups. The inorganic layer in compound 2 features a 1D chain of edge-sharing SrO 8 polyhedra whereas that in compound 3 features an edge-sharing Ba 2O 14 di-polyhedral unit which is further corner-shared with four neighboring ones. The [O 3S-C 2H 4-PO 3H] 2- ligand shows diverse coordination modes in the three alkaline-earth metal sulfonate-phosphonates.

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

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    Mohammed El Fal

    2014-09-01

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

  11. (3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione

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    Garima Sharma

    2012-09-01

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

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

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    Hong-Mian Wu

    2008-05-01

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

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

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    Jing Xu

    2009-08-01

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

  14. 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}].

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

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    Aliou H. Barry

    2003-12-01

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

  16. Dicyclohexylammonium (S-2-azido-3-phenylpropanoate

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    Sebastian J. Petrik

    2012-07-01

    Full Text Available The asymmetric unit of the title compound, C12H24N+·C9H8N3O2−, consists of two dicyclohexylammonium cations linked to two (S-2-azido-3-phenylpropanoate anions by four short N—H...O hydrogen bonds with N...O distances in the range 2.712 (3–2.765 (3 Å. The dicyclohexylammonium cations and the aryl and carboxylate groups of the anion are related by a pseudo-inversion centre, with overall crystallographic inversion symmetry for the structure broken by the chirality of the α-C atoms of the anions.

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

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    Rika Obata

    2015-05-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  19. 17 CFR 402.2d - Appendix D-Modification of § 240.15c3-1d of this title, relating to satisfactory subordination...

    Science.gov (United States)

    2010-04-01

    ... 17 Commodity and Securities Exchanges 3 2010-04-01 2010-04-01 false Appendix D-Modification of § 240.15c3-1d of this title, relating to satisfactory subordination agreements, for purposes of § 402.2...—Modification of § 240.15c3-1d of this title, relating to satisfactory subordination agreements, for purposes of...

  20. 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.

  1. 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

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

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    Joseph Nirmala

    2009-08-01

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

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

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    Tara Shahani

    2010-06-01

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

  4. 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

  5. (R-3-(tert-Butoxycarbonyl-5-methyl-1,2,3-oxathiazolidine 2,2-dioxide

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    Gerhard Laus

    2017-06-01

    Full Text Available The chiral title compound, C8H15NO5S, was obtained by cyclization of (R-1-(tert-butoxycarbonylamino-2-propanol with thionyl chloride and subsequent oxidation with sodium metaperiodate/ruthenium(IV oxide. It crystallizes with two independent molecules in the asymmetric unit. In the crystal, C—H...O interactions link the molecules into a three-dimensional network.

  6. EPR study of gamma irradiated N-methyl taurine (C 3H 9NO 3S) and sodium hydrogen sulphate monohydrate (NaHSO 3·H 2O) single crystals

    Science.gov (United States)

    Yıldırım, İlkay; Karabulut, Bünyamin

    2011-03-01

    EPR study of gamma irradiated C 3H 9NO 3S and NaHSO 3.H 2O single crystals have been carried out at room temperature. There is one site for the radicals in C 3H 9NO 3S and two magnetically distinct sites for the radicals in NaHSO 3. The observed lines in the EPR spectra have been attributed to the species of SO3- and RH radicals for N-methyl taurine, and to the SO3- and OH radicals for sodium hydrogen sulfate monohydrate single crystals. The principal values of the g for SO3-, the hyperfine values of RH and OH proton splitting have been calculated and discussed.

  7. 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.

  8. The crystal structure of Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Winkler, Verena; Schlosser, Marc; Pfitzner, Arno [Regensburg Univ. (Germany). Inst. fuer Anorganische Chemie

    2016-08-01

    A reinvestigation of the alkali metal thiosulfates has led to the new phase Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O. At first cesium thiosulfate monohydrate was obtained as a byproduct of the synthesis of Cs{sub 4}In{sub 2}S{sub 5}. Further investigations were carried out using the traditional synthesis reported by J. Meyer and H. Eggeling. Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O crystallizes in transparent, colorless needles. The crystal structure of the title compound was determined by single crystal X-ray diffraction at room temperature: space group C2/m (No. 12), unit cell dimensions: a = 11.229(4), b = 5.851(2), c = 11.260(5) Aa, β = 95.89(2) , with Z = 4 and a cell volume of V = 735.9(5) Aa{sup 3}. The positions of all atoms including the hydrogen atoms were located in the structure refinement. Cs{sub 2}S{sub 2}O{sub 3}.H{sub 2}O is isotypic with Rb{sub 2}S{sub 2}O{sub 3}.H{sub 2}O. Isolated tetrahedra [S{sub 2}O{sub 3}]{sup 2-} are coordinated by the alkali metal cations, and in addition they serve as acceptors for hydrogen bonding. For both Cs atoms the shortest distances are observed to oxygen atoms of the S{sub 2}O{sub 3}{sup 2-} anions whereas the terminating sulfur atom has its shortest contacts to the water hydrogen atoms. Thus, an extended hydrogen bonding network is formed. The title compound has also been characterized by IR spectroscopy. IR spectroscopy reveals the vibrational bands of the water molecules at 3385 cm{sup -1}. They show a red shift in the OH stretching and bending modes as compared to free water. This is due both to the S..H hydrogen bonding and to the coordination of H{sub 2}O molecules to the cesium atoms.

  9. 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

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    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.

  10. 23 CFR 505.17 - Applicability of Title 23, U.S. Code.

    Science.gov (United States)

    2010-04-01

    ... 23 Highways 1 2010-04-01 2010-04-01 false Applicability of Title 23, U.S. Code. 505.17 Section 505... INFRASTRUCTURE MANAGEMENT PROJECTS OF NATIONAL AND REGIONAL SIGNIFICANCE EVALUATION AND RATING § 505.17 Applicability of Title 23, U.S. Code. Funds made available to carry out this section shall be available for...

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

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    Lorenzo C. Visentin

    2011-01-01

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

  12. 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

  13. (1S,3S,4S-tert-Butyl N-[1-benzyl-3-hydroxy-5-phenyl-4-(picolinamidopentyl]carbamate

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    Jian-Feng Zheng

    2008-07-01

    Full Text Available The title compound, C29H35N3O4, was obtained by the reaction of (2S,4S,5S-tert-butyl N-(4-amino-1-benzyl-3-hydroxy-5-phenylpentylcarbamate and picolinic acid using oxalyl chloride as a chlorinating reagent to activate the carboxyl group. In the crystal structure there are two molecules in the asymmetric unit, which are aligned edge-to-face. In one molecule, the pyridyl ring forms a dihedral angle of 22.0 (1° with the phenyl ring of the terminal benzyl group and 14.3 (1° with the other phenyl ring; in the other molecule, the corresponding angles are 12.1 (1 and 10.6 (1°, respectively. The packing is stabilized by intermolecular hydrogen bonds and C—H...π interactions.

  14. N-Cyclohexyl-2-(5-fluoro-1H-indol-3-yl-2-oxoacetamide

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    Dan-Li Tian

    2011-07-01

    Full Text Available In title compound, C16H17FN2O2, the cyclohexane ring adopts a chair conformation.. The crystal packing is stabilized by weak π–π stacking interactions [centroid–centroid distance = 3.503 (5 Å] and intermolecular C—H...O, N—H...O and N—H...F hydrogen-bond interactions.

  15. 17 CFR 270.22c-1 - Pricing of redeemable securities for distribution, redemption and repurchase.

    Science.gov (United States)

    2010-04-01

    ... 17 Commodity and Securities Exchanges 3 2010-04-01 2010-04-01 false Pricing of redeemable securities for distribution, redemption and repurchase. 270.22c-1 Section 270.22c-1 Commodity and Securities... 1940 § 270.22c-1 Pricing of redeemable securities for distribution, redemption and repurchase. (a) No...

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

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    Rodrigo Abonia

    2016-12-01

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

  17. 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.

  18. (S-Methyl 2-benzamido-3-(3,4-dimethoxyphenylpropanoate

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    Tricia Naicker

    2012-01-01

    Full Text Available The dimethoxypbenzene ring in the title compound, C19H21NO5, is gauche to the amide group and anti to the ester group. The chirality was confirmed to be S from two-dimensional NMR spectroscopy. In the crystal, N—H...O and C—H...O hydrogen bonds and several short-contact interactions (2.07–3.45 Å create chains parallel to [110]. The phenyl ring is disordered over two orientations in a 0.54 (2:0.46 (2 ratio.

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

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    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.

  20. 5-Imino-3,4-diphenyl-1H-pyrrol-2-one

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    Evgeny Bulatov

    2014-02-01

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

  1. [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

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    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.

  2. 1,1′,4,5-Tetrahydrotrispiro[1,3,2-diazaphosphole-2,2′-[1,3,5,2,4,6]triazatriphosphinine-4′,6′′-dibenzo[d,f][1,3,2]dioxaphosphepine-6′,6′′′-dibenzo[d,f][1,3,2]dioxaphosphepine] acetone monosolvate

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    Krystal R. Fontenot

    2013-09-01

    Full Text Available The title compound, C26H22N5O4P3·C3H6O, has been achieved in a two-step synthesis that does not require chromatography. This molecule contains a seven-membered spirocyclic ring at two P-atom positions and a five-membered ring containing new P—N bonds at the other P-atom position. Endocyclic torsion angles about the central biphenyl C—C bonds are −41.5 (3 and −44.4 (3°, and P—N bonds of the central P3N3 ring are within the range 1.5665 (17–1.6171 (17 Å, while the P—O distances are in the range 1.5940 (14–1.6041 (14 Å. One N—H group makes an intermolecular N—H...N hydrogen bond, forming centrosymmetric dimers, while the other N—H group makes an N—H...O hydrogen bond to the acetone solvent molecule. The crystal was a two-component non-merohedral twin with ratio 0.811/0.189.

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

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    Ming-Jian Li

    2009-09-01

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

  4. 2-{N-[(2,3,4,9-Tetrahydro-1H-carbazol-3-ylmethyl]methylsulfonamido}ethyl methanesulfonate

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    Mustafa Göçmentürk

    2014-01-01

    Full Text Available In the title compound, C17H24N2O5S2, the indole ring system is nearly planar [maximum deviation = 0.032 (1 Å] and the cyclohexene ring has a half-chair conformation. In the crystal, N—H...O hydrogen bonds link the molecules into a chain running along the b-axis direction. Weak C—H...O hydrogen bonds and weak C—H...π interactions are observed between the chains.

  5. 3-Benzyl-6-bromo-2-(2-furyl-3H-imidazo[4,5-b]pyridine

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    Younès Ouzidan

    2010-07-01

    Full Text Available In the title molecule, C17H12BrN3O, the imidazopyridine ring system is almost coplanar with the furan ring [dihedral angle = 2.0 (3°]. The benzyl phenyl ring is oriented at dihedral angles of 85.2 (2 and 85.5 (1°, respectively, with respect to the furan ring and the imidazopyridine ring system. In the crystal, molecules are linked into chains propagating along the b axis by C—H...N hydrogen bonds. Adjacent chains are linked via short Br...Br contacts [3.493 (1 Å].

  6. (3R,4Z-1,3-Diethyl-4-(2-oxopropylidene-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one

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    Laila El Foujji

    2018-04-01

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

  7. 2-[1-(1-Naphthyl-1H-1,2,3-triazol-4-yl]pyridine

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    Ulrich S. Schubert

    2009-05-01

    Full Text Available In the crystal structure of the title compound, C17H12N4, the angle between the naphthalene and 1H-1,2,3-triazole ring systems is 71.02 (4° and that between the pyridine and triazole rings is 8.30 (9°.

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

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    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].

  9. 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].

  10. 2-[2-Chloro-5-(trifluoromethylphenyl]hexahydropyrimidine monohydrate

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    Reza Kia

    2008-09-01

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

  11. 1-Benzyl-2-(1H-indol-3-yl-5-oxopyrrolidine-2-carbonitrile

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    Raymond Schinazi

    2008-02-01

    Full Text Available In the title compound, C20H17N3O, a potential anti-human immunodeficiency virus type 1 (HIV-1 non-nucleoside reverse-transcriptase inhibitor, the pyrrolidine ring has an envelope conformation. In the crystal structure, adjacent molecules are connected into infinite chains via an N—H...O hydrogen bond.

  12. 1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one

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    Hualing Zhu

    2011-07-01

    Full Text Available In the title compound, C21H21N3O2, an intramolecular N—H...O interaction generates an S(6 ring, which stablizes the enamine–keto tautomer. The S(6 ring makes dihedral angles of 33.07 (7, 56.50 (8 and 38.59 (8°, respectively, with the benzoylacetone benzene ring and the antipyrine pyrazole and benzene rings.

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

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    Chin Wei Ooi

    2012-08-01

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

  14. 2,2′-Dimethyl-1,1′-[2,2-bis(bromomethylpropane-1,3-diyl]dibenzimidazole hemihydrate

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    Yong-Sheng Yan

    2012-03-01

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

  15. 2-[3-(4-Methoxyphenyl-1-phenyl-1H-pyrazol-5-yl]phenol

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    2009-03-01

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

  16. 2-Benzyl-6-chloro-1-(4-methylphenyl-1H-indole-3-carbonitrile

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    Qiao Yan

    2011-12-01

    Full Text Available In the title compound, C23H17ClN2, the dihedral angle between the indole ring and the attached tolyl ring is 86.97 (8°. Weak C—H...N(nitrile hydrogen bonding, and C—H...π(aromatic and short Cl...π(aromatic [3.628 (1 Å] interactions consolidate the crystal packing.

  17. 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.

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

    Science.gov (United States)

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

    2012-01-01

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

  19. (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.

  20. 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.

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

    Directory of Open Access Journals (Sweden)

    Ravell Bengiat

    2016-07-01

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

  3. 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.

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

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    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].

  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. 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.

  7. (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.

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

    Science.gov (United States)

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

    2017-04-01

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

  9. 1-(1-Hydroxy-9H-carbazol-2-yl-3-methylbut-2-en-1-one

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    Matthias Zeller

    2010-02-01

    Full Text Available The title compound, C17H15NO2, was prepared as one of two products of the AlCl3/POCl3-catalysed reaction of 9-carbazol-1-ol with 3,3-dimethyacrylic acid. It crystallizes with two crystallographically independent molecules, A and B, which are virtually superimposable but not related by any translational or other pseudosymmetry. Both independent molecules are almost planar [r.m.s. deviations from planarity = 0.053 (1 and 0.079 (1 Å in A and B, respectively] and contain an intramolecular O—H...O hydrogen bond. Each type of molecules is connected via pairs of N—H...O hydrogen bonds, forming centrosymmetric A2 and B2 dimers which are, in turn, arranged in offset π-stacks extending along the a-axis direction. The offset of the dimers and the tilt angle of the molecules allows the formation of alternating C—H...π interactions between A and B molecules of parallel stacks.

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

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    Mehmet Akkurt

    2014-06-01

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

  11. (2S-1,1-Dichloro-2-(2-chlorophenyl-2-(4-chlorophenylethane

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    Lars Eriksson

    2009-02-01

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

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

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    Andrii I. Buvailo

    2008-01-01

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

  13. 2-[4-(Dimethylaminophenyl]-3,3-difluoro-3H-naphtho[1,2-e][1,3,2]oxazaborinin-2-ium-3-uide

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    Błażej Dziuk

    2017-08-01

    Full Text Available In the title compound, C19H17BF2N2O, a twist about the N—C single bond is observed, making the cross conjugation not as efficient as in the case of a planar structure. The borone complex has tetrahedral geometry. In the crystal, molecules are conected by weak C—H...F hydrogen bonds.

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

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    Ankur Trigunait

    2010-08-01

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

  15. 5-(4-Methoxyphenyl-4-methyl-1-phenyl-3-p-tolyl-1H-pyrazole

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    Yahya Ben Soumane

    2017-11-01

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

  16. (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.

  17. 3,5-Bis(4-methoxyphenyl-1-phenyl-4,5-dihydro-1H-pyrazole

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    Zeliha Baktır

    2011-02-01

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

  18. (Carbonyl-1κC)bis­[2,3(η5)-cyclo­penta­dien­yl][μ3-(S-methyl trithio­carbonato)methylidyne-1:2:3κ4 C,S′′:C:C](triphenyl­phosphine-1κP)(μ3-sulfido-1:2:3κ3 S)dicobalt(II)iron(II) trifluoro­methane­sulfonate

    Science.gov (United States)

    Manning, Anthony R.; McAdam, C. John; Palmer, Anthony J.; Simpson, Jim

    2008-01-01

    The asymmetric unit of the title compound, [FeCo2(C5H5)2(C3H3S3)S(C18H15P)(CO)]CF3SO3, consists of a triangular irondicobalt cluster cation and a trifluoro­methane­sulfonate anion. In the cation, the FeCo2 triangle is symmetrically capped on one face by an S atom and on the other by a C atom linked to a methyl trithio­carbonate residue that bridges the Fe—C bond. Each Co atom carries a cyclo­penta­dienyl ligand while the Fe atom coordinates to one carbonyl and one triphenyl­phosphine ligand. In the crystal structure, the cation is linked to the anion by a number of weak non-classical C—H⋯O and C—H⋯F hydrogen bonds and weak S⋯O (3.317 Å) and S⋯F (3.198 Å) inter­actions. The structure is further stabilized by additional inter­molecular C—H⋯O, C—H⋯F and O⋯O (2.942 Å) contacts, together with an unusual S⋯π(Cp) inter­action (S⋯centroid distance = 3.385 Å), generating an extended network. PMID:21202187

  19. 1,3-Dibenzyl-6-bromo-1H-imidazo[4,5-b]pyridin-2(3H-one

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    S. Dahmani

    2010-04-01

    Full Text Available The imidazopyridine fused-ring in the title compound, C20H16BrN3O, is planar (r.m.s. deviation = 0.011 Å. The phenyl rings of the benzyl substitutents twist away from the central five-membered ring in opposite directions; the rings are aligned at 61.3 (1 and 71.2 (1° with respect to this ring.

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

    Science.gov (United States)

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

    2002-11-01

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

  1. N-Benzyl-1,3-dideoxy-1,3-imino-l-xylitol

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    Sarah F. Jenkinson

    2011-09-01

    Full Text Available The structure determination confirms the stereochemistry of the title compound, C12H17NO3, which contains a four-membered azetidine ring system. The absolute configuration was determined by the use of d-glucose as the starting material. In the crystal, O—H...O and O—H...N hydrogen bonds link the molecules into layers in the ab plane.

  2. 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 groupS0885715617001105_inline1' mime-subtype='gif' type='simple'/>$P\\bar 1$,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.

  3. 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)

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

    NARCIS (Netherlands)

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

    1982-01-01

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

  5. (E-3-Methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone

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    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.

  6. 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.

  7. 12,12′-[2,2′-Oxybis(ethane-2,1-diylbis(oxy]bis[(Rp-4-bromo[2.2]paracyclophane

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    Bing Hong

    2011-04-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  9. 3,5-Bis(4-meth-oxy-phen-yl)-1-phenyl-4,5-dihydro-1H-pyrazole.

    Science.gov (United States)

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

    2011-01-12

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

  10. 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.

  11. 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.

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

    Science.gov (United States)

    2015-04-27

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

  13. (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

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    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].

  14. 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".

  15. 4-Hydroxy-6-methyl-3-[3-(thiophen-2-ylacryloyl]-2H-pyran-2-one

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    Salima Thabti

    2013-04-01

    Full Text Available The title compound, C13H10O4S, crystallizes with two molecules in the asymmetric unit in which the rings make dihedral angles of 3.9 (1 and 6.0 (1°; this planarity is due in part to the presence of an intramolecular O—H...O hydrogen bond, which generates an S(6 ring in each molecule. Both molecules represent E isomers with respect to the central C=C bond. In the crystal, molecules are linked by C—H...O interactions into a three-dimensional network.

  16. 5-[(E-(2-Hydroxybenzylideneamino]-1H-1,3-benzimidazole-2(3H-thione

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    Hoong-Kun Fun

    2011-01-01

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

  17. 1-Methoxy-3-o-tolylbicyclo[2.2.2]oct-5-ene-2,2-dicarbonitrile

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    Orhan Büyükgüngör

    2009-09-01

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

  18. HFE gene C282Y, H63D and S65C mutations frequency in the Transylvania region, Romania.

    Science.gov (United States)

    Trifa, Adrian P; Popp, Radu A; Militaru, Mariela S; Farcaş, Marius F; Crişan, Tania O; Gana, Ionuţ; Cucuianu, Andrei; Pop, Ioan V

    2012-06-01

    HFE-associated haemochromatosis is one of the most frequent autosomal recessive disorders in the Caucasian population. Although most of the cases are homozygous individuals for the C282Y mutation, another two mutations, H63D and S65C, have been reported to be associated with milder forms of the disease. This study was a first attempt to evaluate the distribution of these HFE gene mutations in the Transylvania region. Two-hundred and twenty-five healthy, unrelated volunteers originating from the Transylvania region, Romania, were screened for the HFE gene C282Y, H63D and S65C mutations, using molecular genetics assays (Polymerase Chain Reaction-Restriction Fragments Length Polymorphism). For the C282Y mutation, 7 heterozygotes (3.1%) were found, but no homozygous individual. In the case of the H63D mutation, 40 heterozygotes (17.8%) and 4 homozygotes (1.75%) for the mutant allele were evidenced. We found a compound heterozygous genotype (C282Y/H63D) in one individual (0.45%). Thus, the allele frequencies of the C282Y and H63D were 1.75% and 10.9%, respectively. Three individuals (1.3%) were found to harbour the S65C mutation in a heterozygous state, but none in a homozygous state: the allele frequency of the mutant allele was 0.75%. The distribution of the HFE gene C282Y, H63D and S65C mutations found in our group matches the tendencies observed in other European countries: a decreasing gradient from Northern to Southern Europe for the C282Y mutation; high frequency for the H63D mutation, and low frequency for the S65C mutation in most of the countries.

  19. A Facile Synthesis of Pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidine and Pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazine Bearing a Thiophene Moiety

    Directory of Open Access Journals (Sweden)

    Tilal Elsaman

    2013-01-01

    Full Text Available Pyridinone derivative 8 was synthesized and transformed into the respective chloropyridine 9, which was allowed to react with hydrazine hydrate to afford pyrazolo[3,4-b]pyridin-3-amine derivative 11. Compound 11 was used as a key intermediate for a facile synthesis of the title compounds 14, 15, 17, 21a,b, and 24a–c where the reaction of 11 with some 1,3-dielecrophiles resulted in the formation of pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidines 14, 15, and 17, whereas diazotization of compound 11 gave the respective diazonium salt 18 which was coupled with some active methylene-containing compounds to give the corresponding hydrazones 19a,b and 22a–c. Cyclization of the latter hydrazones yielded the pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazines 21a,b and 24a–c, respectively.

  20. 10-[1,1-Dichloro-4-(trimethylsilylbut-1-en-3-yn-2-yl]-10H-phenothiazine

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    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.

  1. Multiple C-H Bond Activations and Ring-Opening C-S Bond Cleavage of Thiophene by Dirhenium Carbonyl Complexes.

    Science.gov (United States)

    Adams, Richard D; Dhull, Poonam; Tedder, Jonathan D

    2018-06-14

    The reaction of Re 2 (CO) 8 (μ-C 6 H 5 )(μ-H) (1) with thiophene in CH 2 Cl 2 at 40 °C yielded the new compound Re 2 (CO) 8 (μ-η 2 -SC 4 H 3 )(μ-H) (2), which contains a bridging σ-π-coordinated thienyl ligand formed by the activation of the C-H bond at the 2 position of the thiophene. Compound 2 exhibits dynamical activity on the NMR time scale involving rearrangements of the bridging thienyl ligand. The reaction of compound 2 with a second 1 equiv of 1 at 45 °C yielded the doubly metalated product [Re 2 (CO) 8 (μ-H)] 2 (μ-η 2 -2,3-μ-η 2 -4,5-C 4 H 2 S) (3), formed by the activation of the C-H bond at the 5 position of the thienyl ligand in 2. Heating 3 in a hexane solvent to reflux transformed it into the ring-opened compound Re(CO) 4 [μ-η 5 -η 2 -SCC(H)C(H)C(H)][Re(CO) 3 ][Re 2 (CO) 8 (μ-H)] (4) by the loss of one CO ligand. Compound 4 contains a doubly metalated 1-thiapentadienyl ligand formed by the cleavage of one of the C-S bonds. When heated to reflux (125 °C) in an octane solvent in the presence of H 2 O, the new compound Re(CO) 4 [η 5 -μ-η 2 -SC(H)C(H)C(H)C(H)]Re(CO) 3 (5) was obtained by cleavage of the Re 2 (CO) 8 (μ-H) group from 4 with formation of the known coproduct [Re(CO) 33 -OH)] 4 . All new products were characterized by single-crystal X-ray diffraction analyses.

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

    Directory of Open Access Journals (Sweden)

    Frankie White

    2014-09-01

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

  3. Androstane-3β,5α,6β,17β-tetrol trihydrate

    Directory of Open Access Journals (Sweden)

    L. C. R. Andrade

    2011-07-01

    Full Text Available The title hydrated tetrol, C19H32O4·3H2O, was synthesized by stereoselective reduction of the compound 3β,5α,6β-trihydroxyandrostan-17-one. All rings are fused trans. The organic molecules are connected head-to-tail along the c axis via O—H...O hydrogen bonds. Layers of water molecules in the ab plane interconnect these chains. A quantum chemical ab initio Roothan Hartree–Fock calculation of the isolated molecule gives values for the molecular geometry close to experimentally determined ones, apart from the C—O bond lengths, whose calculated values are significantly smaller than the measured ones, probably a consequence of the involvement of the C—OH groups in the hydrogen-bonding network.

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

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    DAOUDA NDOYE

    2014-01-01

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

  5. 17 CFR 270.22e-2 - Pricing of redemption requests in accordance with Rule 22c-1.

    Science.gov (United States)

    2010-04-01

    ... 17 Commodity and Securities Exchanges 3 2010-04-01 2010-04-01 false Pricing of redemption requests in accordance with Rule 22c-1. 270.22e-2 Section 270.22e-2 Commodity and Securities Exchanges....22e-2 Pricing of redemption requests in accordance with Rule 22c-1. An investment company shall not be...

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

    Science.gov (United States)

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

    2009-04-01

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

  7. 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.

  8. Crystal and molecular structure of the coordination compounds of Er3+ with 1-(methoxydiphenylphosphoryl)-2-diphenylphosphorylbenzene [ErL21(NO3)2]2[Er(NO3)2(H2O)5]0.333(NO3)2.333 · 2.833H2O and its ethyl substituted derivative [ErL22(NO3)2][Er(NO3)5]0.5 · 0.5H2O

    International Nuclear Information System (INIS)

    Polyakova, I. N.; Baulin, V. E.; Ivanova, I. S.; Pyatova, E. N.; Sergienko, V. S.; Tsivadze, A. Yu.

    2015-01-01

    The coordination compounds of Er 3+ with 1-(methoxydiphenylphosphoryl)-2-diphenylphosphorylbenzene [ErL 2 1 (NO 3 ) 2 ] 2 [Er(NO 3 ) 2 (H 2 O) 5 ] 0.333 (NO 3 ) 2.333 · 2.833H 2 O (I) and its ethyl substituted derivative [ErL 2 2 (NO 3 ) 2 ][Er(NO 3 ) 5 ] 0.5 · 0.5H 2 O (II) are synthesized and their crystal structures are studied. I and II contain [ErL 2 (NO 3 ) 2 ] + complex cations of identical composition and close structure. The eight-vertex polyhedron of the Er atom in the shape of a distorted octahedron with two split trans vertices is formed by the O atoms of the phosphoryl groups of L ligands and nitrate anions. L ligands close nine-membered metallocycles. The structures contain spacious channels which are populated differently, namely, by disordered [Er(NO 3 ) 2 (H 2 O) 5 ] + complex cations, NO 3 − anions, and crystallization water molecules in I and disordered [Er(NO 3 ) 5 ] 2− complex anions and crystallization water molecules in II. The IR spectra of I and II are studied

  9. 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.

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

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    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°.

  11. Crystal structure of (1S,2R,6R,7R,8S,12S-4,10,17-triphenyl-15-thia-4,10-diazapentacyclo[5.5.5.01,16.02,6.08,12]heptadeca-13,16-diene-3,5,9,11-tetrone p-xylene hemisolvate

    Directory of Open Access Journals (Sweden)

    Wayland E. Noland

    2014-12-01

    Full Text Available The title tetrone compound, C32H22N2O4S· 0.5C8H10, is the major product (50% yield of an attempted Diels–Alder reaction of 2-(α-styrylthiophene with N-phenylmaleimide (2 equivalents in toluene. Recrystallization of the resulting powder from p-xylene gave the title hemisolvate; the p-xylene molecule is located about an inversion center. In the crystal, the primary tetrone contacts are between a carbonyl O atom and the four flagpole H atoms of the bicyclo[2.2.2]octene core, forming chains along [001].

  12. 2-(2-Hydroxy-3-methoxyphenyl-1H-benzimidazol-3-ium perchlorate

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    Chuan Chen

    2012-06-01

    Full Text Available In the title molecular salt, C14H13N2O2+·ClO4−, the ring systems in the cation are almost coplanar [dihedral angle = 5.53 (13°]. Intramolecular N—H...O and O—H...O hydrogen bonds generate S(6 and S(5 rings, respectively. In the crystal, the two H atoms involved in the intramolecular hydrogen bonds also participate in intermolecular links to acceptor O atoms of the perchlorate anions. A simple intermolecular N—H...O bond also occurs. Together, these form a double-chain structure along [101].

  13. 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.

  14. Browse Title Index

    African Journals Online (AJOL)

    Items 501 - 550 of 753 ... K Kamel, M Mohamed, B Abderrazek, C Mohamed, D Amine, B.S. Riadh, C Mohamed. Vol 17, No 2 (2011) ... S Ketata, H Fakhfakh, H Ketata, A Sahnoun, A Bahloul, T Boudawara, M N Mhiri. Vol 17, No 4 (2011) ... S U Alhasan, A Abdullahi, A A Sheshe, A Z Mohammed, S T Edino, S A Aji. Vol 17, No 3 ...

  15. 2,2′-(Ethane-1,2-diylbis(1H-benzimidazole

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    Guo-Liang Zhao

    2012-05-01

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

  16. 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].

  17. Bis(N,N-diethyldithiocarbamato-κ2S,S′(3-hydroxypyridine-κNzinc and bis[N-(2-hydroxyethyl-N-methyldithiocarbamato-κ2S,S′](3-hydroxypyridine-κNzinc: crystal structures and Hirshfeld surface analysis

    Directory of Open Access Journals (Sweden)

    Mukesh M. Jotani

    2016-12-01

    Full Text Available The common feature of the molecular structures of the title compounds, [Zn(C5H10NS22(C5H5NO], (I, and [Zn(C4H8NOS22(C5H5NO], (II, are NS4 donor sets derived from N-bound hydroxypyridyl ligands and asymmetrically chelating dithiocarbamate ligands. The resulting coordination geometries are highly distorted, being intermediate between square pyramidal and trigonal bipyramidal for both independent molecules comprising the asymmetric unit of (I, and significantly closer towards square pyramidal in (II. The key feature of the molecular packing in (I is the formation of centrosymmetric, dimeric aggregates sustained by pairs of hydroxy-O—H...S(dithiocarbamate hydrogen bonds. The aggregates are connected into a three-dimensional architecture by methylene-C—H...O(hydroxy and methyl-C—H...π(chelate interactions. With greater hydrogen-bonding potential, supramolecular chains along the c axis are formed in the crystal of (II, sustained by hydroxy-O—H...O(hydroxy hydrogen bonds, with ethylhydroxy and pyridylhydroxy groups as the donors, along with ethylhydroxy-O—H...S(dithiocarbamate hydrogen bonds. Chains are connected into layers in the ac plane by methylene-C—H...π(chelate interactions and these stack along the b axis, with no directional interactions between them. An analysis of the Hirshfeld surfaces clearly distinguished the independent molecules of (I and reveals the importance of the C—H...π(chelate interactions in the packing of both (I and (II.

  18. 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

  19. Synthesis and properties of 4-alkoxy-2-[2-hydroxy-3-(4-o,m,p-halogenoaryl-1 -piperazinyl)propyl]-6-methyl-1H-pyrrolo-[3,4-c]pyridine-1,3(2H)-diones with analgesic and sedative activities.

    Science.gov (United States)

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

    2006-01-01

    Synthesis of N-substituted derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (17-26) is described. The chlorides, containing OH group, used in the above synthesis can exist in two isomeric forms: chain (12, 14-16) and cyclic (12a, 14a-16a). All final imides studied exhibited analgesic activity in the "writhing syndrome" test which was superior than that of acetylsalicylic acid. In the "hot plate" test only two compounds (19, 20) were active as antinociceptive agents. Furthermore, all compounds tested significantly suppressed the spontaneous locomotor activity of mice.

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

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    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.

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

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    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.

  3. 1-[(E-(3-Hydroxy-4-methoxybenzylideneamino]-3-methylthiourea

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    Md. Azharul Arafath

    2016-10-01

    Full Text Available In the title thiosemicarbazone Schiff base compound, C10H13N3O2S, the dihedral angle between the benzene ring and methyl carbothioamide side arm was found to be 17.4 (4°. The presence of two intramolecular hydrogen bonds is noted, namely hydroxy-O—H...O(methoxy and amine-N—H...N(imine. In the crystal, pairwise amine-N—H...S hydrogen bonds give rise to centrosymmetric {...HNCS}2 synthons, which lead to dimeric aggregates.

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

    Energy Technology Data Exchange (ETDEWEB)

    Vega-Baez, José Luis; Sandoval-Ramírez, Jesús; Meza-Reyes, Socorro; Montiel-Smith, Sara; Gómez-Calvario, Victor [Facultad de Ciencias Químicas, Benemérita Universidad Autónoma de Puebla, Ciudad Universitaria, San Manuel, 72000 Puebla, Pue. (Mexico); Bernès, Sylvain, E-mail: sylvain-bernes@hotmail.com [DEP Facultad de Ciencias Químicas, UANL, Guerrero y Progreso S/N, Col. Treviño, 64570 Monterrey, NL (Mexico); Facultad de Ciencias Químicas, Benemérita Universidad Autónoma de Puebla, Ciudad Universitaria, San Manuel, 72000 Puebla, Pue. (Mexico)

    2008-04-01

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

  5. (E-2-(2-Nitroethenylfuran

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    Pedro Valerga

    2009-08-01

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

  6. 5-Ethyl-3-(2-fluorophenylsulfonyl-2-methyl-1-benzofuran

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    Hong Dae Choi

    2012-10-01

    Full Text Available In the title compound, C17H15FO3S, the 2-fluorophenyl ring makes a dihedral angle of 89.12 (8° with the mean plane of the benzofuran fragment. In the crystal, molecules are linked by weak C—H...O and C—H...π interactions.

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

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    Abdellah N'ait Ousidi

    2016-03-01

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

  8. (Z-3-(4-Chlorophenyl-1-(2,4-difluorophenyl-2-(1H-1,2,4-triazol-1-ylprop-2-en-1-one

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    Xin-Mei Peng

    2012-06-01

    Full Text Available The asymmetric unit of the title compound, C17H10ClF2N3O, contains three independent molecules. In each molecule, the C=C bond has a cis conformation with respect to the triazole and chlorophenyl groups. The dihedral angles formed by the triazole ring with the diflurophenyl and chlorophenyl benzene rings, respectively, are 20.10 (14 and 73.22 (15, 25.31 (15 and 84.44 (15, and 16.44 (13 and 61.72 (14° in the three molecules while the dihedral angles between the benzene rings are 66.54 (13, 85.82 (12 and 58.37 (12°.

  9. The effects of fabric for sleepwear and bedding on sleep at ambient temperatures of 17°C and 22°C

    Directory of Open Access Journals (Sweden)

    Shin M

    2016-04-01

    Full Text Available Mirim Shin,1 Mark Halaki,1 Paul Swan,2 Angus Ireland,2 Chin Moi Chow1 1Exercise, Health and Performance Research Group, Faculty of Health Sciences, The University of Sydney, Lidcombe, 2Australian Wool Innovation Limited, The Woolmark Company, Sydney, NSW, Australia Abstract: The fibers used in clothing and bedding have different thermal properties. This study aimed to investigate the influences of textile fabrics on sleep under different ambient temperature (Ta conditions. Seventeen healthy young participants (ten males underwent nine nights of polysomnography testing including an adaptation night. Participants were randomized to each of the three binary factors: sleepwear (cotton vs wool, bedding (polyester vs wool, and Ta (17°C vs 22°C with relative humidity set at 60%. Skin temperature (Tsk and core temperature (Tc were monitored throughout the sleep period. Sleep onset latency (SOL was significantly shortened when sleeping in wool with trends of increased total sleep time and sleep efficiency compared to cotton sleepwear. At 17°C, the proportion of sleep stages 1 (%N1 and 3 (%N3 and rapid eye movement sleep was higher, but %N2 was lower than at 22°C. Interaction effects (sleepwear × Ta showed a significantly shorter SOL for wool than cotton at 17°C but lower %N3 for wool than cotton at 22°C. A significantly lower %N2 but higher %N3 was observed for wool at 17°C than at 22°C. There was no bedding effect on sleep. Several temperature variables predicted the sleep findings in a stepwise multiple regression analysis and explained 67.8% of the variance in SOL and to a lesser degree the %N2 and %N3. These findings suggest that sleepwear played a contributory role to sleep outcomes and participants slept better at 17°C than at 22°C.Keywords: cotton, polyester, wool, polysomnography, skin temperature, core body temperature

  10. 3′,6′-Bis(diethylamino-3H-spiro[2-benzothiophene-1,9′-xanthene]-3-thione

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    Bing-Yuan Su

    2008-11-01

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

  11. 1,3-Dimethyl-1H-indole-2-carbonitrile

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    Jiang-Sheng Li

    2009-08-01

    Full Text Available The title compound, C11H10N2, crystallizes with two molecules in the asymmetric unit, both of which are essentially planar (r.m.s. deviations = 0.014 and 0.016 Å. In the crystal, aromatic π–π stacking interactions occur [shortest centroid–centroid separation = 3.5569 (11 Å].

  12. Crystal structure of 2,2′-({[2-(tritylsulfanylbenzyl]azanediyl}bis(ethane-2,1-diylbis(isoindoline-1,3-dione

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    Ulrich Flörke

    2014-09-01

    Full Text Available In the structure of the title compound, C46H37N3O4S, the planes of the two isoindoline units make a dihedral angle of 77.86 (3°. The dihedral angles between the benzyl plane and the isoindoline units are 79.56 (4 and 3.74 (9°. The geometry at the S atom shows a short [1.7748 (17 Å] S—Cbenzyl and a long [1.8820 (15 Å] S—Ctrityl bond and the C—S—C angle is 108.40 (7°. N—C bond lengths around the azane N atom are in the range 1.454 (2–1.463 (2 Å. he crystal packing exhibts two rather `non-classical' C—H...O hydrogen bonds that result in stacking of the molecules along the a as well as the b axis and give rise to columnar sub-structures.

  13. (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.

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

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    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.

  15. 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.

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

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    Samra Rahmouni

    2016-05-01

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

  17. 3-D silver(I)-lanthanide(III) heterometallic-organic frameworks constructed from 2,2'-bipyridine-3,3'-dicarboxylic acid: synthesis, structure, photoluminescence, and their remarkable thermostability.

    Science.gov (United States)

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

    2014-04-07

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

  18. (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.

  19. 1-(2-Ethoxy-2-methyl-2H-chromen-3-ylethanone

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    Afsaneh Zonouzi

    2009-04-01

    Full Text Available The Csp3 atom of the chromenyl fused-ring system in the title compound, C14H16O3, deviates by 0.407 (2 Å from the plane of the other atoms (r.m.s. deviation = 0.041 Å. The ethoxy substituent occupies a pseudo-axial position.

  20. 5-(4-Ethoxyphenyl-3-(pyridin-2-yl-4,5-dihydro-1H-pyrazole-1-carbothioamide

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    Hoong-Kun Fun

    2012-03-01

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

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

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    Alexander Briceño

    2010-03-01

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

  2. 8-Chloro-4-oxo-4H-chromene-3-carbaldehyde

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    Yoshinobu Ishikawa

    2014-07-01

    Full Text Available In the title compound, C10H5ClO3, a chlorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. deviation = 0.032 Å for the non-H atoms, with the largest deviation from the least-squares plane [0.0598 (14 Å] being for a pyran-ring C atom. In the crystal, molecules are linked through stacking interactions along the b axis [shortest centroid–centroid distance between the pyran and benzene rings = 3.566 (2 Å].

  3. 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.

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

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    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].

  5. 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

  6. 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.

  7. 4-(2,4-Dichlorophenyl-2-(1H-indol-3-yl-6-methoxypyridine-3,5-dicarbonitrile

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    M. N. Ponnuswamy

    2008-10-01

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

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

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    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.

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

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    Qiu-qi Ye

    2012-09-01

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

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

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    Chao Huang

    2017-09-01

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

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

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    Mehmet Akkurt

    2011-02-01

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

  12. 5-Isobutyl-4-phenylsulfonyl-1H-pyrazol-3(2H-one

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    M. Venkatesh

    2010-12-01

    Full Text Available The title compound, C13H16N2O3S, consists of two crystallographically independent molecules with similar geometries and exists in a keto form, the C=O bond lengths being 1.267 (2 and 1.254 (2 Å. In both molecules, the pyrazole rings are approximately planar, with maximum deviations of 0.017 (2 and 0.010 (2 Å, and the dihedral angles between the pyrazole and phenyl rings are 83.63 (11 and 70.07 (12°. In one molecule, an intramolecular C—H...O hydrogen bond with an S(6 ring motif is observed. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into two-dimensional networks parallel to the ab plane.

  13. 9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4H-thieno[2′,3′:4,5]pyrimidino[1,2-a]pyridin-4-one

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    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.

  14. {4,4′,6,6′-Tetraiodo-2,2′-[(2,2-dimethylpropane-1,3-diylbis(nitrilomethanylylidene]diphenolato}nickel(II

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    Hadi Kargar

    2012-07-01

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

  15. Ethyl 2-amino-4-(4-bromophenyl-6-methoxy-4H-benzo[h]chromene-3-carboxylate

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    Seik Weng Ng

    2013-03-01

    Full Text Available In the title compound, C23H20BrNO4, the pyran ring has a flattened boat conformation with the O and methine C atoms lying to one side of the plane [0.160 (5 and 0.256 (6 Å, respectively] defined by the remaining atoms. Nevertheless, the 4H-benzo[h]chromene ring system approximates a plane (r.m.s. deviation = 0.116 Å with the bromobenzene ring almost perpendicular [dihedral angle = 83.27 (16°] and the ester group coplanar [C—C—C—O = 3.4 (5°]; the methoxy substituent is also coplanar [C—O—C—C = 174.5 (3°]. In addition to an intramolecular N—H...O(ester carbonyl hydrogen bond, the ester carbonyl O atom also forms an intermolecular N—H...O hydrogen bond with the second amine H atom, generating a zigzag supramolecular chain along the c axis in the crystal packing. The chains are linked into layers in the bc plane by N—H...Br hydrogen bonds, and these layers are consolidated into a three-dimensional architecture by C—H...π interactions.

  16. 10,21-Dimethyl-2,7,13,18-tetraphenyl-3,6,14,17-tetraazatricyclo[17.3.1.18,12]tetracosa-1(23,2,6,8(24,9,11,13,17,19,21-decaene-23,24-diol cyclohexane 0.33-solvate

    Directory of Open Access Journals (Sweden)

    Sushil K. Gupta

    2011-10-01

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

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

    Science.gov (United States)

    Saheb, Vahid; Sheikhshoaie, Iran

    2011-10-15

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

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

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    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.

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

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    Naoto Kuwamura

    2016-01-01

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

  20. 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.

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

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    Yuan-Yuan Zhou

    2011-10-01

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

  2. Methyl (9aR*,10S*,11R*,13aS*,13bS*-9-oxo-6,7,9,9a,10,11-hexahydro-5H,13bH-11,13a-epoxypyrrolo[2′,1′:3,4][1,4]diazepino[2,1-a]isoindole-10-carboxylate

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    Flavien A. A. Toze

    2011-11-01

    Full Text Available The title compound, C17H18N2O4, is the methyl ester of the adduct of intramolecular Diels–Alder reaction between maleic anhydride and 1-(2-furyl-2,3,4,5-tetrahydro-1H-pyrrolo[1,2-a][1,4]diazepine. The molecule comprises a fused pentacyclic system containing four five-membered rings (viz. pyrrole, 2-pyrrolidinone, tetrahydrofuran and dihydrofuran and one seven-membered ring (1,4-diazepane. The pyrrole ring is approximately planar (r.m.s. deviation = 0.003 Å while the 2-pyrrolidinone, tetrahydrofuran and dihydrofuran five-membered rings have the usual envelope conformations. The central seven-membered diazepane ring adopts a boat conformation. In the crystal, molecules are bound by weak intermolecular C—H...O hydrogen-bonding interactions into zigzag chains propagating in [010]. In the crystal packing, the chains are stacked along the a axis.

  3. 39 CFR 211.1 - Disposition of former title 39, U.S.C.

    Science.gov (United States)

    2010-07-01

    ... 39 Postal Service 1 2010-07-01 2010-07-01 false Disposition of former title 39, U.S.C. 211.1... REGULATIONS § 211.1 Disposition of former title 39, U.S.C. Except as otherwise continued in effect as postal regulations, all provisions of former title 39, U.S.C., which were continued in effect as regulations of the...

  4. Bis[1,3-bis(2,4,6-trimethylphenyl-2,3-dihydro-1H-imidazol-2-ylidene]dinitrosyl(tetrahydroborato-κ2H,H′tungsten(0

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    Heinz Berke

    2011-01-01

    Full Text Available In the title paramagnetic 19-electron neutral complex, [W(BH4(C21H24N22(NO2], the W(0 atom is coordinated by two 1,3-bis(2,4,6-trimethylphenylimidazol-2-ylidene (IMes carbene ligands, two NO groups and two H atoms of an η2-tetrahydroborate ligand. Depending on the number of coordination sites (n assigned to the BH4− ligand, the coordination geometry of the W atom may either be described as approximately trigonal–bipyramidal (n = 1 or as very distorted octahedral with the bridging H atoms filling two coordination positions (n = 2. In the latter case, the coplanar NO groups and bridging H atoms (r.m.s. deviation = 0.032 Å form one octahedral plane, with mutually trans-oriented carbene ligands. In the crystal, molecules are connected via C—H...O interactions.

  5. 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.

  6. Crystal structure of diethyl 2-amino-6-[(thiophen-3-ylethynyl]azulene-1,3-dicarboxylate

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    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.

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

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    Jasim Alshawi

    2016-01-01

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

  8. Crystal structure of N′-[(E-(1S,3R-(3-isopropyl-1-methyl-2-oxocyclopentylmethylidene]-4-methylbenzenesulfonohydrazide

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    David Tymann

    2015-12-01

    Full Text Available The title compound, C17H24N2O3S, was synthesized in order to determine the relative configuration of the corresponding β-keto aldehyde. In the U-shaped molecule, the five-membered ring approximates an envelope, with the methylene C atom adjacent to the quaternary C atom being the flap, and the methyl and isopropyl substituents lying to the same side of the ring. The dihedral angles between the four nearly coplanar atoms of the five-membered ring and the flap and the aromatic ring are 35.74 (15 and 55.72 (9°, respectively. The bond angles around the S atom are in the range from 103.26 (12 to 120.65 (14°. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming a chain along the a axis.

  9. 3-[4-(10H-Indolo[3,2-b]quinolin-11-ylpiperazin-1-yl]propan-1-ol

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    Gary S. Nichol

    2011-12-01

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

  10. N-tert-Butyl-3-hydroxy-5-androstene-17-carboxamide monohydrate

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    Jiang-Sheng Li

    2009-07-01

    Full Text Available In the title compound, C24H39NOH2O, the A and C rings of the pregnolene derivative sterol adopt chair conformations, with the B ring in a flattened chair conformation and the five-membered ring in an envelope conformation twisted about the C/D ring junction. The N-tert-butylcarboxamide substituent is equatorial. The 3β-hydroxy H atom and one H atom of the water molecule are disordered over two positions with equal occupancies. In the crystal structure, O—H...O hydrogen bonds between the 3β-hydroxy groups of neighbouring molecules form dimers in the bc plane and these dimers are stacked along the a axis by additional O—H...O hydrogen bonds involving the water molecules. The steric effect of the bulky tert-butyl substituent in the carboxamide chain precludes hydrogen-bond formation by the N—H group.

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

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    Zukhra Ch. Kadirova

    2009-07-01

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

  12. Structure and magnetic properties of Gd2Co17-xCr x (1.17 ≤ x ≤ 3.0) compounds

    International Nuclear Information System (INIS)

    Fuquan, B.; Tegus, O.; Dagula, W.; Brueck, E.; Klaasse, J.C.P.; Buschow, K.H.J.

    2007-01-01

    The structure and magnetic properties of Gd 2 Co 17-x Cr x (1.17 ≤ x ≤ 3.0) compounds have been investigated by means of X-ray diffraction (XRD) and magnetization measurements. The powder X-ray diffraction patterns show that all samples crystallize as a single phase with the rhombohedral Th 2 Zn 17 -type structure. The lattice parameters a and the unit cell volume V increases slightly with increasing Cr content, but the c parameter varies in a less simple way with increasing Cr content. The X-ray diffraction patterns of the magnetically aligned samples show that all compounds investigated have uniaxial anisotropy. Spin reorientation phenomena occur in all of the compounds. The Curie temperature T C , the spin reorientation temperature T sr , the spontaneous magnetization M 0 and the saturation magnetization M s decrease with the increasing Cr content. The anisotropy constant K 1 and the anisotropy field B a of the compounds at room temperature reach a maximum for x = 1.76. The M 0 and M s increase with increasing temperature from 5 K to 300 K. The easy-axis anisotropy of all compounds changes to easy-plane anisotropy at low temperatures and the spin reorientation phenomena are more pronounced for low Cr concentration

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

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    Moayad Hossaini Sadr

    2011-12-01

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

  14. 2-{[(2-Methoxynaphthalen-1-ylmethyl]amino}phenol

    Directory of Open Access Journals (Sweden)

    Sara Mahdjoub

    2016-07-01

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

  15. Crystal structure of N-[(E-(1,3-benzodioxol-5-ylmethylidene]-4-chloroaniline

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    J. Pablo García-Merinos

    2014-11-01

    Full Text Available In the title compound, C14H10ClNO2, obtained by the condensation of 4-chloroaniline and piperonal, the five-membered ring is almost planar (r.m.s. deviation = 0.023 Å and the dihedral angle between the aromatic rings is 43.22 (14°. In the crystal, a short O...Cl contact of 3.173 (2 Å is observed. The molecules are arranged into corrugated (010 layers.

  16. 4-(2,4-Dichlorophenyl-6-(1H-indol-3-yl-2,2′-bipyridine-5-carbonitrile

    Directory of Open Access Journals (Sweden)

    M. N. Ponnuswamy

    2009-05-01

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

  17. (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.

  18. 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.

  19. 6-Bromo-1,3-di-2-propynyl-1H-imidazo[4,5-b]pyridin-2(3H-one

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    S. Dahmani

    2010-04-01

    Full Text Available The room-temperature reaction of propargyl bromide and 6-bromo-1,3-dihydroimidazo[4,5-b]pyridin-2-one in dimethylformamide yields the title compound, C12H8BrN3O, which features nitrogen-bound propynyl substituents. The imidazopyridine fused ring is almost planar (r.m.s. deviation = 0.011 Å; the propynyl chains point in opposite directions relative to the fused ring. One acetylenic H atom is hydrogen bonded to the carbonyl O atom of an inversion-related molecule, forming a dimer; adjacent dimers are linked by a second acetylene–pyridine C—H...N interaction, forming a layer motif.

  20. Textural and mechanical characterization of C-S-H gels from hydration of synthetic T1-C3S, β-C2S and their blends

    Directory of Open Access Journals (Sweden)

    Dolado, J. S.

    2011-06-01

    Full Text Available The textural and mechanical characterization of C-S-H gels formed from the hydration of pure T1-C3S, β-C2S and their blends are studied by Nitrogen sorption and nanoindentation experiments. The surface area and nanoporosity of C-S-H gels formed from the hydration of β-C2S and the 30-70 (T1-C3S and β-C2S mixture are higher than those from hydration of T1-C3S, and 70-30, with the difference decreasing with hydration age. Such changes are well supported by findings of nanoindentation study, which shows the greater relative volume of C-S-H phases with lower densities in the β-C2S and the 30-70 pastes. With the increase in hydration age, the relative volume of C-S-H phases with higher densities increased at the expenses of those with lower density. Important quantitative correlations were found among these textural characteristics and the mean chain length, determined from 29Si magic-angle-spinning (MAS NMR, of the C-S-H gels.La caracterización textural y mecánica de geles C-S-H formados a partir de la hidratación de muestras puras de T1-C3S, ß-C2S y sus mezclas ha sido estudiada por medio de adsorción de nitrógeno y nanoindentación. El área superficial y la nano-porosidad de los geles formados durante la hidratación del ß-C2S y la mezcla 30-70 (T1-C3S- ß-C2S son mayores que los correspondientes a los geles del T1-C3S, y la mezcla 70-30; esta diferencia disminuye con el tiempo de hidratación. Estos cambios coinciden con los resultados de nanoindentación que indican un aumento de volumen relativo de las fases C-S-H con una densidad menor en el caso del ß-C2S y la mezcla 30-70. Al aumentar el tiempo de hidratación, el volumen relativo de fases C-S-H de mayor densidad aumenta a expensas de aquellas de menor densidad. Importantes correlaciones cuantitativas se establecen entre las características texturales y la longitud de cadena media del gel C-S-H, determinada mediante RMN-MAS de 29Si.

  1. 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.

  2. (3S,4S)-3-Ethyl-4-hydroxy-3-(3-methoxyphenyl)-1-methylazepan-1-ium d-tartrate dihydrate

    OpenAIRE

    Zhui-Bai Qiu; Bo Chao; Xing-Hai Wang

    2008-01-01

    In the title compound, C16H26NO2+·C4H5O6−·2H2O, a meptazinol derivative, three C atoms of the azepane ring are disordered over two positions, with site-occupancy factors of 0.80 and 0.20; the major disorder component adopts a twist-chair conformation, while the minor component has a chair conformation. The benzene ring is axially substituted on the heterocyclic ring, resulting in a folded conformation of the cation. The absolute configuration was determined with reference to d...

  3. 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.

  4. 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.

  5. System of Sr(NO2)2-Sr(OH)2-H2O at 25 deg C

    International Nuclear Information System (INIS)

    Popova, T.B.; Berdyukova, V.A.; Khutsistova, F.M.

    1990-01-01

    Sr(NO 2 ) 2 -Sr(OH) 2 -H 2 O system was investigated by the methods of solubility, density, viscosity, electric conductivity and refractometry. It was established that its compoments form the compound 4Sr(NO 2 ) 2 xSr(OH) 2 x8H 2 O. The compound was separated from solution; its density, decomposition temperature were determined; IR spectra and X-ray patterns of prepared and initial compounds were obtained

  6. Coordination compounds of cobalt (3), chromium (3) and vanadium (3) with s-methylthiosemicarbazone of salicylic aldehyde

    Energy Technology Data Exchange (ETDEWEB)

    Leovats, V.M.; Gehrbehlehu, N.V.; Tsanich, V.D. (AN Moldavskoj SSR, Kishinev. Inst. Khimii)

    1982-04-01

    Coordination compounds of trivalent cobalt, chromium and vanadium with S-methylthiosemicarbazone of salicylic aldehyde H/sub 2/L of (Co(HL)/sub 2/)XxnH/sub 2/O (X=Cl, Br, I, NO/sub 3/, ClO/sub 4/), (CoL(NH/sub 3/)/sub 3/)NO/sub 3/, (Co(HL)/sub 2/)/sub 2/(Co(NCS)/sub 4/)x2H/sub 2/O, (CoCl(DH)/sub 2/(H/sub 2/L))xH/sub 2/O, (Cr(HL)/sub 2/)XxnH/sub 2/O (X=Cl, NO/sub 3/), (V(HL)/sub 2/)Clx1/2H/sub 2/O, (M(HL)L)xnH/sub 2/O (M=Co, Cr, V) compositions are synthesized and investigated. It is shown, that H/sub 2/L behaves as a tridentate ligand at the expense of (O, N, N) set of donor atoms. The effective magnetic moment of the compounds is calculated.

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

    Directory of Open Access Journals (Sweden)

    A. Dhandapani

    2015-02-01

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

  8. 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.

  9. 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.

  10. Synthesis of 1-amino-2-[3-(3-[2,6-14C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3,4-dione hydrochloride

    International Nuclear Information System (INIS)

    Swigor, J.E.; Algieri, A.A.; Standridge, R.T.; Pittman, K.A.

    1985-01-01

    The synthesis of the title compound is described. The condensation of 3-aminopropanol with phthalic anhydride and subsequent treatment with phosphorous tribromide produced N-[3-bromopropyl] phthalimide. Acylation with 3-hydroxybenzaldehyde, reduction with hydrogen over Raney nickel and subsequent treatment with thionyl chloride gave N-[3-(3-chloromethylphenoxy) propyl] phthalimide. Treatment with [2,6 - 14 C] piperidine introduced the radiolabel. Deprotection of the amino group with hydrazine and treatment with 3-methoxy-4-amino-3-cyclobutene-1,2-dione produced 1-amino-2-[3-(3-[2,6- 14 C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3, 4-dione. Treatment with hydrochloric acid yielded the title compound in an overall chemical yield of 22%. (author)

  11. 3-[(E-(2,4-Dichloropbenzylideneamino]benzoic acid

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    Adnan Ashraf

    2011-01-01

    Full Text Available In the crystal of the title compound, C14H9Cl2NO2, inversion-related dimers with R22(8 ring motifs are formed by intermolecular O—H...O hydrogen bonding. The 3-aminobenzoic acid group and the 2,4-dichlobenzaldehyde moiety subtend a dihedral angle of 55.10 (2°. The H atom of the carboxyl group is disordered over two sites with equal occupancies.

  12. 2-(4-Fluoroanilino-3-(2-hydroxyethylquinazolin-4(3H-one

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The molecular and crystal structures of the title compound, C16H14FN3O2, are stabilized by intramolecular N—H...O and intermolecular O—H...O hydrogen bonds. The existence of non-classical intramolecular C—H...N hydrogen bonds provides a dihedral angle between the fluoro-substituted benzene and pyrimidinone rings of 7.9 (1°.

  13. Textural and mechanical characterization of C-S-H gels from hydration of synthetic T1-C3S, β-C2S and their blends

    International Nuclear Information System (INIS)

    Goni, S.; Guerrero, A.; Puertas, F.; Hernandez, M. S.; Palacios, M.; Dolado, J. S.; Zhu, W.; Howind, T.

    2011-01-01

    The textural and mechanical characterization of C-S-H gels formed from the hydration of pure T1-C 3 S, β-C 2 S and their blends are studied by Nitrogen sorption and nano indentation experiments. The surface area and nano porosity of C-S-H gels formed from the hydration of β-C 2 S and the 30-70 (T1-C 3 S and β-C 2 S mixture) are higher than those from hydration of T1-C 3 S, and 70-30, with the difference decreasing with hydration age. Such changes are well supported by findings of nano indentation study, which shows the greater relative volume of C-S-H phases with lower densities in the β-C 2 S and the 30-70 pastes. With the increase in hydration age, the relative volume of C-S-H phases with higher densities increased at the expenses of those with lower density. Important quantitative correlations were found among these textural characteristics and the mean chain length, determined from 2 9Si magic-angle-spinning (MAS) NMR, of the C-S-H gels. (Author) 36 refs.

  14. (E)-3-Hydr?oxy-13-methyl-16-[4-(methyl?sulfan?yl)benzyl?idene]-7,8,9,11,12,13,15,16-octa?hydro-6H-cyclo?penta?[a]phen?an????thren-17(14H)-one

    OpenAIRE

    Gunasekaran, B.; Murugan, R.; Narayanan, S. Sriman; Manivannan, V.

    2008-01-01

    In the title compound, C26H28O2S, the dihedral angles between the mean plane of the five membered ring and the 4-(methylsulfanyl)benzylidine 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.

  15. 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].

  16. 3-(Pyridin-2-ylcoumarin

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    Yu-Xia Da

    2010-11-01

    Full Text Available In the title compound, C14H9NO2, the dihedral angle between the pyridine ring and the lactone ring is 10.40 (3°. The coumarin ring system is nearly planar, with a dihedral angle of 1.40 (2° between the lactone and benzene rings. An intramolecular C—H...O hydrogen bond occurs. In the crystal, inversion dimers linked by pairs of C—H...O interactions occur, generating R22(14 loops.

  17. 2-(2-Methyl-1,3-dioxolan-2-yl-1,1-diphenylethanol

    Directory of Open Access Journals (Sweden)

    Dennis P. Arnold

    2010-01-01

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

  18. (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.

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

    Directory of Open Access Journals (Sweden)

    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. Crystal structures of (RS-N-[(1R,2S-2-benzyloxy-1-(2,6-dimethylphenylpropyl]-2-methylpropane-2-sulfinamide and (RS-N-[(1S,2R-2-benzyloxy-1-(2,4,6-trimethylphenylpropyl]-2-methylpropane-2-sulfinamide: two related protected 1,2-amino alcohols

    Directory of Open Access Journals (Sweden)

    Matthew R. Carbone

    2014-11-01

    Full Text Available The title compounds, C22H31NO2S, (1, and C23H33NO2S, (2, are related protected 1,2-amino alcohols. They differ in the substituents on the benzene ring, viz. 2,6-dimethylphenyl in (1 and 2,4,6-trimethylphenyl in (2. The plane of the phenyl ring is inclined to that of the benzene ring by 28.52 (7° in (1 and by 44.65 (19° in (2. In the crystal of (1, N—H...O=S and C—H...O=S hydrogen bonds link molecules, forming chains along [100], while in (2, similar hydrogen bonds link molecules into chains along [010]. The absolute structures of both compounds were determined by resonance scattering.

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Yong Wang

    2009-04-01

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

  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. 2-Oxo-2H-chromen-3-yl benzoate

    Directory of Open Access Journals (Sweden)

    Konan René Kambo

    2017-05-01

    Full Text Available In the title compound, C16H10O4, the dihedral angle between the coumarin ring system (r.m.s. deviation = 0.015 Å and the benzoate group is 83.58 (9°, which compares to a value of 81.8° obtained from a DFT calculation at the B3LYP/6–311 G(d,p level. In the crystal, C—O...π and C—H...π interactions and aromatic π–π [Cg...Cg = 3.7214 (14 and 3.7059 (14 Å] stacking generate a three-dimensional network.

  5. Aminosilanes derived from 1H-benzimidazole-2(3H)-thione

    International Nuclear Information System (INIS)

    Palomo-Molina, Juliana; García-Báez, Efrén V.; Contreras, Rosalinda; Pineda-Urbina, Kayim; Ramos-Organillo, Angel

    2015-01-01

    In two trimethylsilyl-substituted 1H-benzimidazole-2(3H)-thiones, noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe 3 groups form helicoidal arrangements in one, and dimerization results in the formation of R s 2 (8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings, in the second compound. Two new molecular structures, namely 1,3-bis(trimethylsilyl)-1H-benzimidazole-2(3H)-thione, C 13 H 22 N 2 SSi 2 , (2), and 1-trimethylsilyl-1H-benzimidazole-2(3H)-thione, C 10 H 14 N 2 SSi, (3), are reported. Both systems were derived from 1H-benzimidazole-2(3H)-thione. Noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe 3 groups form helicoidal arrangements in (2). Dimerization of (3) results in the formation of R 2 2 (8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings

  6. (R,S-3-Carboxy-2-(isoquinolinium-2-ylpropanoate monohydrate

    Directory of Open Access Journals (Sweden)

    Vladimir Stilinović

    2010-06-01

    Full Text Available The title compound, C13H11NOH2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquinoline group and a deprotonated carboxyl group. In the crystal, molecules are connected via short O—H...O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enantiomers along [001]. These chains are additionally connected by hydrogen bonding between water molecules and the deprotonated carboxy groups of neighbouring molecules.

  7. Crystal structure of (2R*,3aR*-2-phenylsulfonyl-2,3,3a,4,5,6-hexahydropyrrolo[1,2-b]isoxazole

    Directory of Open Access Journals (Sweden)

    Yaiza Hernández

    2017-01-01

    Full Text Available The title compound, C12H15NO3S, was prepared by 1,3-dipolar cycloaddition of 3,4-dihydro-2H-pyrrole 1-oxide and phenyl vinyl sulfone. In the molecule, both fused five-membered rings display a twisted conformation. In the crystal, C—H...O hydrogen bonds link neighbouring molecules, forming chains running parallel to the b axis.

  8. Textural and mechanical characterization of C-S-H gels from hydration of synthetic T1-C{sub 3}S, {beta}-C{sub 2}S and their blends; Caracterizacion textural y mecanica de geles C-S-H formados en la hidratacion de muestras sinteticas T1-C{sub 3}S, {beta}-C{sub 2}S y sus mezclas

    Energy Technology Data Exchange (ETDEWEB)

    Goni, S.; Guerrero, A.; Puertas, F.; Hernandez, M. S.; Palacios, M.; Dolado, J. S.; Zhu, W.; Howind, T.

    2011-07-01

    The textural and mechanical characterization of C-S-H gels formed from the hydration of pure T1-C{sub 3}S, {beta}-C{sub 2}S and their blends are studied by Nitrogen sorption and nano indentation experiments. The surface area and nano porosity of C-S-H gels formed from the hydration of {beta}-C{sub 2}S and the 30-70 (T1-C{sub 3}S and {beta}-C{sub 2}S mixture) are higher than those from hydration of T1-C{sub 3}S, and 70-30, with the difference decreasing with hydration age. Such changes are well supported by findings of nano indentation study, which shows the greater relative volume of C-S-H phases with lower densities in the {beta}-C{sub 2}S and the 30-70 pastes. With the increase in hydration age, the relative volume of C-S-H phases with higher densities increased at the expenses of those with lower density. Important quantitative correlations were found among these textural characteristics and the mean chain length, determined from {sup 2}9Si magic-angle-spinning (MAS) NMR, of the C-S-H gels. (Author) 36 refs.

  9. 1-[5-(2-Chlorophenyl-3-(4-methylphenyl-4,5-dihydro-1H-pyrazol-1-yl]ethan-1-one

    Directory of Open Access Journals (Sweden)

    Farook Adam

    2016-01-01

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

  10. 8-Bromo-3,4-dihydro-2H-1,3-thiazino[2,3:2′,1′]imidazo[5′,4′-b]pyridine

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    Hend Bel Ghacham

    2010-05-01

    Full Text Available The imidazopyridine ring system in the title compound, C9H8BrN3S, is almost planar [r.m.s. deviation of the C and N atoms = 0.007 (1 Å]. The S and methylene C atoms connected to the five-membered ring lie within this plane. The remaining two methylene groups of the thiazine ring are disordered over two sets of sites in a 0.817 (5:0.183 (5 ratio.

  11. Crystal structure of (1S,2S,2′R,3a′S,5R-2′-[(5-bromo-1H-indol-3-ylmethyl]-2-isopropyl-5,5′-dimethyldihydro-2′H-spiro[cyclohexane-1,6′-imidazo[1,5-b]isoxazol]-4′(5′H-one

    Directory of Open Access Journals (Sweden)

    Siwar Ghannay

    2016-08-01

    Full Text Available In the title compound, C24H32BrN3O2, the six-membered cyclohexane ring adopts a chair conformation and the isoxasolidine ring adopts a twisted conformation. The molecule has five chiral centres and the absolute configuration has been determined in this analysis. The molecular structure is stabilized by weak intramolecular C—H...O and C—H...N contacts. In the crystal, molecules are linked by N—H...N and C—H...O hydrogen bonds, forming undulating sheets parallel to the bc plane.

  12. Crystal and molecular structure of 2,2’-(quinoxaline-2,3-diyl)dipyridinium dinitrate (H_2L)(NO_3)_2

    International Nuclear Information System (INIS)

    Egorova, O. A.; Polyakova, I. N.; Sergienko, V. S.; Davydov, V. V.

    2016-01-01

    The crystal structure of 2,2’-(quinoxaline-2,3-diyl)dipyridinium dinitrate (H_2L)(NO_3)_2 is studied by X-ray diffraction (T = 150 K, R1 = 0.0467). The H_2L"2"+ cation is located on the twofold rotation axis and connected with two NO_3"− anions by strong N–H···O hydrogen bonds. Planar quinoxaline fragments of cations form stacks with the interplanar spacing of 3.308 Å. The structure of the diprotonated H_2L"2"+ cation is compared with those of the monoprotonated H_2L"2"+ cation and neutral L molecule.

  13. Synthesis of [2,4-3H] 17β-dihydroequilin sulfate

    International Nuclear Information System (INIS)

    Bhavnani, B.R.

    1994-01-01

    [2,4- 3 H] 17β-dihydroequilin-3-sulfate ammonium salt suitable for in vivo pharmacokinetic studies was synthesized from [2,4- 3 H] equilin. Sulfation of [2,4- 3 H] equilin with pyridine-chlorosulfonic acid mixture gave in high yields [2,4- 3 H] equilin sulfate, which was then reduced with sodium borohydride to yield [2,4- 3 H] 17β-dihydroequilin sulfate. The reduction was sterospecific and no 17α-reduced products were formed. (author)

  14. N-(4-Nitrobenzoyl)-N'-(1,5-dimethyl-3-oxo-2-phenyl-1H-3(2H)-pyrazolyl)-thiourea hydrate: Synthesis, spectroscopic characterization, X-ray structure and DFT studies

    Science.gov (United States)

    Arslan, N. Burcu; Kazak, Canan; Aydın, Fatma

    2012-04-01

    The title molecule (C19H17N5O4S·H2O) was synthesized and characterized by IR-NMR spectroscopy, MS and single-crystal X-ray diffraction. The molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the compound in the ground state have been calculated by using the density functional theory (DFT) method with 6-31G(d) basis set, and compared with the experimental data. All the assignments of the theoretical frequencies were performed by potential energy distributions using VEDA 4 program. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and 1H and 13C NMR chemical shift values show good agreement with experimental data. To determine conformational flexibility, the molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which was varied from -180° to +180° in steps of 10°. Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and thermodynamic properties of the compound were investigated by theoretical calculations.

  15. (5S-4-(2,2-Dimethylpropyl-5-isopropyl-1,3,4-oxadiazinan-2-one

    Directory of Open Access Journals (Sweden)

    Kate L. Edler

    2010-12-01

    Full Text Available The title compound, C11H22N2O2, has one chiral center and packs in the monoclinic space group P21. The asymmetric unit has five crystallographically independent molecules, four of which engage in intermolecular N—H...O hydrogen bonding.

  16. 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.

  17. (S,S,S,S-Nebivolol hydrochloride hemihydrate

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    Yoann Rousselin

    2012-12-01

    Full Text Available The asymmetric unit of the title hydrated salt, C22H26F2NO4+·Cl−·0.5H2O, consists of an (S,S,S,S-nebivolol {nebivol = bis[2-(6-fluoro-3,4-dihydro-2H-1-benzopyran-2-yl-2-hydroxyethyl]ammonium} cation, a chloride anion and a half-occupancy water molecule. The dihedral angle between the mean planes of the benzene rings is 50.34 (12°. The pyran rings adopt half-chair conformations. The crystal packing features O—H...O hydrogen bonds and weak N—H...Cl, O—H...Cl, and O—H...Cl interactions, producing layers along (010.

  18. 2-[(E-(2S,5R-2-Isopropyl-5-methylcyclohexylidene]-N-methylhydrazine-1-carbothioamide

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    Adriano Bof de Oliveira

    2016-03-01

    Full Text Available There are two molecules in the asymmetric unit of the title compound, C12H23N3S, which are linked by two strong N—H...S hydrogen bonds, building a non-centrosymmetric dimer with graph-set motif R22(8. The molecules are further connected by N—H...S interactions into a two-dimensional hydrogen-bonded polymeric structure along the [001] direction. The absolute structure is based on the refinement of the Flack parameter.

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

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    Rachid Bouhfid

    2014-03-01

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

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

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    Kil Sik Min

    2008-02-01

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

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

    Science.gov (United States)

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

    2013-01-01

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

  2. 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.

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

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    Chen-Yen Tsai

    2009-06-01

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

  4. {2-[(3,5-Dichloro-2-oxidobenzylideneamino-κ2N,O]-3-methylpentanoato-κO}(N,N′-dimethylformamide-κOcopper(II

    Directory of Open Access Journals (Sweden)

    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.

  5. 3β,5α,6β-Trihydroxyandrostan-17-one

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    L.C.R. Andrade

    2011-05-01

    Full Text Available The title compound, C19H30O4, is an androstan-17-one derivative synthesized from the dehydroepiandrosterone through a sequential addition of an oxidant, followed by a trans-diaxial opening of the epoxide generated, with Bi(OTf3 (OTf is trifluoromethanesulfonate. The six-membered rings have a slightly flattened chair conformation, while the five-membered ring adopts a 14-α envelope conformation. All rings are trans fused. In the crystal, the molecules are connected by O—H...O hydrogen bonds involving the hydroxyl and carbonyl groups, forming a three-dimensional network. A quantum mechanical ab initio Roothan Hartree–Fock calculation of the free molecule gives bond lengths, valency angles and ring torsion angles of the free molecule at equilibrium geometry (energy minimum close to the experimental values.

  6. Insulators containing CuCl4X22- (X=H2O, NH3) units: Origin of the orthorhombic distortion observed only for CuCl4(H2O)22-

    DEFF Research Database (Denmark)

    García-Fernández, P.; García Lastra, Juan Maria; Trueba, A.

    2012-01-01

    The origin of the difference in structure between compounds containing CuCl4X22- (X=H2O, NH3) units is analyzed by means of first-principles calculations. While NH3-containing compounds display tetragonal symmetry, H2O-containing ones display an orthorhombic distortion at low temperature where...... the equatorial Cl- ions are no longer equivalent. Our simulations of optical and vibrational transitions show good agreement with all available experimental optical absorption and Raman data. As a salient feature, the value of the force constant for the B1g mode, K(B1g), driving the orthorhombic distortion......CuCl4(H2O)2 has a local origin....

  7. (E-6-Amino-1,3-dimethyl-5-[(pyridin-2-ylmethylideneamino]pyrimidine-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Irvin Booysen

    2011-09-01

    Full Text Available In the title compound, C12H13N5O2, a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å. The N=C bond is E-configured. Intracyclic angles in the pyridine moiety cover the range 117.6 (2–124.1 (2°. Intra- and intermolecular N—H...N and N—H...O hydrogen bonds are observed in the crystal structure, as are intra- and intermolecular C—H...O contacts which, in total, connect the molecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14 Å is between the two different types of six-membered rings.

  8. Propyl 3-oxo-2,3-dihydro-1,2-benzothia-zole-2-carboxyl-ate.

    Science.gov (United States)

    Wang, Xiang-Hui; Yang, Jian-Xin; You, Cheng-Hang; Lin, Qiang

    2011-09-01

    The title compound, C(11)H(11)NO(3)S, was synthesized by the reaction of benzo[d]isothia-zol-3(2H)-one with propyl carbono-chloridate in toluene. The benzoisothiazolone ring system is approximately planar with a maximum deviation from the mean plane of 0.0226 (14) Å for the N atom. Weak inter-molecular C-H⋯O hydrogen bonding occurs in the crystal structure.

  9. 3-[2-(5H-Indolo[2,3-b]quinoxalin-5-ylethyl]-1,3-oxazolidin-2-one

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    Abdussalam Alsubari

    2010-09-01

    Full Text Available The title compound, C19H16N4O2, has an almost planar fused N-heterocyclic system (r.m.s. deviation = 0.031 Å and an almost planar five-membered 1,3-oxazolidine ring (r.m.s. deviation = 0.015 Å at the ends of an ethylene chain [N—C—C—N torsion angle = −65.6 (2°]. The ring systems are inclined at 38.1 (1° to one another.

  10. Spin reorientation and magnetic anisotropy in Y2Co17-xCr x (x 1.17-3.0) compounds

    International Nuclear Information System (INIS)

    Fuquan, B.; Tegus, O.; Dagula, W.; Brueck, E.; Boer, F.R. de; Buschow, K.H.J.

    2005-01-01

    Spin reorientation transitions and magnetic anisotropy in Y 2 Co 17-x Cr x (x = 1.17-3.0) compounds have been investigated by means of X-ray diffraction and magnetization measurements. The powder X-ray diffraction patterns show that most samples crystallize as a single phase with the rhombohedral Th 2 Zn 17 -type structure. However, in the compound Y 2 Co 14 Cr 3 the Th 2 Zn 17 phase coexist with the hexagonal Th 2 Ni 17 -type phase. The lattice parameters a and c hardly change and the unit cell volume V increases slightly with increasing Cr content. The X-ray diffraction patterns of the aligned powder of the samples have confirmed that at room temperature the compound with x = 1.17 has planar anisotropy, but the compounds with x = 1.76, 2.34 and 3.00 have uniaxial anisotropy. Spin reorientation phenomena occur in all of the compounds. With increasing Cr content, the Curie temperature, the spin reorientation temperature, the spontaneous magnetization, and the anisotropy constant K 2 of the Y 2 Co 17-x Cr x (x = 1.17-3.0) compounds decrease strongly while the anisotropy constant K 1 increases in the range of x from 1.17 to 2.34 and then decreases in the range of x from 2.34 to 3.00

  11. Crystal structure and thermochemical properties of 1-decylammonium hydrobromide (C10H21NH3Br)(s)

    International Nuclear Information System (INIS)

    Zhang Lijun; Di Youying; Lu Dongfei

    2011-01-01

    Highlights: → Crystal structure of 1-decylammonium hydrobromide was reported. → Lattice potential energy of the compound was obtained. → Molar volumes of the compound and its cation were obtained. → Ionic radius of its cation of the compound was calculated. → Molar enthalpy of dissolution at infinite dilution was determined. → Hydration enthalpies of the compound and its cation were calculated. - Abstract: The crystal structure of 1-decylammonium hydrobromide was determined by X-ray crystallography. Lattice potential energy and molar volumes of the solid compound and its cation were obtained respectively. The ionic radius of the cation can be calculated from the corresponding effective volume of the cation. The molar enthalpies of dissolution of the compound at different concentrations m/(mol . kg -1 ) at T = 298.15 K were measured by an isoperibol solution-reaction calorimeter at T = 298.15 K. According to the Pitzer's electrolyte solution theory, the molar enthalpy of dissolution of the compound at infinite dilution (Δ s H m ∞ ) and Pitzer parameters (β MX (0)L and β MX (1)L ) were obtained. The values of apparent relative molar enthalpies ( Φ L) of the title compound and relative partial molar enthalpies (L 2 -bar and L 1 -bar) of the solute and the solvent at different concentrations were derived from the experimental values of the enthalpy of dissolution of the compound. Finally, hydration enthalpies of the compound and its cation were calculated by designing a thermochemical cycle in accordance with lattice potential energy and the molar enthalpy of dissolution of the title compound at infinite dilution.

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

    Directory of Open Access Journals (Sweden)

    Nadeem Abad

    2018-04-01

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

  13. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    Directory of Open Access Journals (Sweden)

    YuanQi Yu

    2011-10-01

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

  14. (4Z-4-[1-(2-Aminoanilinoethylidene]-3-methyl-1-phenyl-4,5-dihydro-1H-pyrazol-5-one

    Directory of Open Access Journals (Sweden)

    Mohamed Samba

    2017-02-01

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

  15. (E-1-(1,3-Benzodioxol-5-yl-3-[4-(dimethylaminophenyl]prop-2-en-1-one

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    Karthik Kumara

    2017-01-01

    Full Text Available In the title compound, C18H17NO3, the olefinic double bond adopts an E conformation. The molecule is nearly planar as indicated by the dihedral angle of 3.11 (6° between the benzodioxole and benzene rings. The carbonyl group lies in the plane of the olefinic double bond and the benzodioxole ring. The trans conformation of the C=C double bond in the central enone group is confirmed by the C=C—C—C torsion angle of −177.82 (14°.

  16. 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%.

  17. (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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    Lin Chen

    2011-01-01

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

  19. Bis[2-(2-pyridylmethyleneaminobenzenesulfonato-κ3N,N′,O]cadmium(II dihydrate

    Directory of Open Access Journals (Sweden)

    Miao Ou-Yang

    2008-11-01

    Full Text Available The title complex, [Cd(Paba2]·2H2O or [Cd(C12H9N2O3S2]·2H2O, was synthesized by the reaction of the potassium salt of 2-(2-pyridylmethyleneaminobenzenesulfonic acid (PabaK with CdCl2·2.5H2O in methanol. The CdII atom lies on a crystallographic twofold axis and is coordinated by four N atoms and two O atoms from two deprotonated tridentate 2-(2-pyridylmethyleneaminobenzenesulfonate ligands in a slightly distorted octahedral environment. There are extensive hydrogen bonds of the type O—H...O between the uncoordinated water molecules and the sulfonate O atoms, through which the complex forms a layered structure parallel to (001.

  20. 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.

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

    Directory of Open Access Journals (Sweden)

    Sibi Narayanan

    2012-12-01

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

  2. Synthesis of 15N-enriched urea (CO(15NH22 from 15NH3, CO, and S in a discontinuous process

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    C. R. Sant Ana Filho

    2012-12-01

    Full Text Available CO(15NH22 enriched with the stable isotope 15N was synthesized based on a reaction involving CO, 15NH3, and S in the presence of CH3OH. The method differs from the industrial method; a stainless steel reactor internally lined with polytetrafluoroethylene (PTFE was used in a discontinuous process under low pressure and temperature. The yield of the synthesis was evaluated as a function of the parameters: the amount of reagents, reaction time, addition of H2S, liquid solution and reaction temperature. The results showed that under optimum conditions (1.36, 4.01, and 4.48 g of 15NH3, CO, and S, respectively, 40 ml CH3OH, 40 mg H2S, 100 ºC and 120 min of reaction 1.82 g (yield 76.5% of the compound was obtained per batch. The synthesized CO(15NH22 contained 46.2% N, 0.55% biuret, melting point of 132.55 ºC and did not exhibit isotopic fractionation. The production cost of CO(15NH22 with 90.0 at. % 15N was US$ 238.60 per gram.

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

    Science.gov (United States)

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

    2011-01-01

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

  4. (R,S)-3-Carb?oxy-2-(isoquinolinium-2-yl)propanoate monohydrate

    OpenAIRE

    Stilinovi?, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-01-01

    The title compound, C13H11NOH2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquinoline group and a deprotonated carboxyl group. In the crystal, molecules are connected via short O—H...O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enantiomers along [001]. These chains are additionally connected by hydrogen bonding between water molecules and the deprotonated carboxy groups of neighbourin...

  5. Crystal structure of (E-1-(4′-methoxy-[1,1′-biphenyl]-4-yl-3-(3-nitrophenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    T. Vidhyasagar

    2015-01-01

    Full Text Available The title compound, C22H17NO4, crystallizes with two independent molecules (A and B in the asymmetric unit. Each molecule exists as an E isomer with C—C=C—C torsion angles of −175.69 (17 and −178.41 (17° in A and B, respectively. In molecule A, the planes of the terminal benzene rings are twisted by an angle of 26.67 (10°, while the biphenyl unit is non-planar, the dihedral angle between the rings being 30.81 (10°. The dihedral angle between the nitrophenyl ring and the inner phenyl ring is 6.50 (9°. The corresponding values in molecule B are 60.61 (9, 31.07 (8 and 31.05 (9°. In the crystal, molecules are arranged in a head-to-head manner, with the 3-nitrophenyl groups nearly parallel to one another. The A and B molecules are linked to one another via C—H...O hydrogen bonds, forming chains lying parallel to (-320 and enclosing R22(10 and R22(12 ring motifs. The methoxy group in both molecules is positionally disordered with a refined occupancy ratio of 0.979 (4:0.021 (4 for molecule A and 0.55 (4:0.45 (4 for molecule B.

  6. 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.

  7. 2-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]indane-1,3-dione

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    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. 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)

  9. (E-2,2′-[3-(2-Nitrophenylprop-2-ene-1,1-diyl]bis(3-hydroxycyclohex-2-en-1-one

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    Joo Hwan Cha

    2012-01-01

    Full Text Available In the title compound, C21H21NO6, each of the cyclohexenone rings adopts a half-chair conformation. Each of the pairs of hydroxy and carbonyl O atoms are oriented to allow for the formation of intramolecular O—H...O hydrogen bonds, which are typical of xanthene derivatives.

  10. 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.

  11. 5-[3-(2,5-Dimethoxyphenylprop-2-enylidene]-1,3-diethyl-2-thioxohexahydropyrimidine-4,6-dione

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    Abdullah Mohamed Asiri

    2009-08-01

    Full Text Available 1,3-Diethyl-2-thiobarbituric acid reacts with 2,5-dimethoxybenzaldehyde to form the title Knoevenagel product, C19H22N2O4S. In the compound, the two six-membered rings at either end of the three-membered –CHCHCH– chain are nearly coplanar with this fragment (r.m.s. deviation of the two six-membered rings and the three chain atoms = 0.08 Å.

  12. [2,6-Difluoro-3-(pyridin-2-yl-κNpyridin-4-yl-κC4](pentane-2,4-dionato-κ2O,O′iridium(III

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    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.

  13. Crystal structure of bis{S-hexyl 3-[4-(dimethylaminobenzylidene]dithiocarbazato-κ2N3,S}copper(II

    Directory of Open Access Journals (Sweden)

    E. Zangrando

    2015-06-01

    Full Text Available In the title complex, [Cu(C16H24N3S22], the CuII atom is coordinated by two azomethine N and two thiolate S atoms of the chelating Schiff base ligands, resulting in a distorted square-planar coordination environment. The S—Cu—N chelating angle is of 84.41 (5°. The CuII atom is located on a crystallographic inversion centre, leading to a trans configuration of the N,S-chelating ligands.

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

    Science.gov (United States)

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

    2018-03-26

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

  15. 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.

  16. 9-Butyl-9H-carbazole

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The title compound, C16H17N, is a carbazole derivative that has been designed and synthesized as a potential organic electronic device, such as an OLED. The tricyclic aromatic ring system is essentially planar, the two outer rings making a dihedral angle of 4.8 (1°. No classical hydrogen bonds are observed in the crystal structure.

  17. 9-Ethyl-2,3-dihydro-9H-carbazol-4(1H-one

    Directory of Open Access Journals (Sweden)

    S. Sriman Narayanan

    2008-09-01

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

  18. 1-(3-Bromopropylindoline-2,3-dione

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    Fatima Zahrae Qachchachi

    2016-04-01

    Full Text Available In the title compound, C11H10BrNO2, the indoline ring system has an r.m.s. deviation of 0.026 Å. The side chain (including the Br atom has a trans–gauche conformation, as indicated by the N—C—C—C and C—C—C—Br torsion angles of −177.5 (3 and 68.1 (3°, respectively. In the crystal, molecules are linked by weak C—H...O hydrogen bonds, forming a three-dimensional network.

  19. 4-{[(1-Phenyl-1H-pyrazol-3-yloxy]methyl}-1,3-dioxolan-2-one

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2012-11-01

    Full Text Available The title compound was obtained by the reaction of tosylated glycerol carbonate with 1-phenyl-1H-pyrazol-3-ol in a good 71% yield. Detailed spectroscopic data (1H-NMR, 13C-NMR, 15N-NMR, IR, MS are presented.

  20. (2E-3-(3-Methoxy-1-phenyl-1H-pyrazol-4-yl-2-propenal

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    Algirdas Šačkus

    2009-12-01

    Full Text Available The palladium-catalyzed reaction of 4-bromo-3-methoxy-1-phenyl-1H-pyrazole with acrolein diethyl acetal gives the title compound in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

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

    Directory of Open Access Journals (Sweden)

    Yun Wei

    2012-04-01

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

  2. Crystal structure of mer-tris{2,6-difluoro-3-[5-(2-fluorophenylpyridin-2-yl-κN]pyridin-4-yl-κC4}iridium(III dichloromethane hemisolvate n-hexane hemisolvate

    Directory of Open Access Journals (Sweden)

    Youngjin Kang

    2017-12-01

    Full Text Available The asymmetric unit of the title compound, [Ir(C17H11F2N23]·0.5CH3(CH24CH3·0.5CH2Cl2, comprises one IrIII atom, three 2,6-difluoro-3-[5-(2-fluorophenylpyridin-2-yl]pyridin-4-yl ligands and half each of an n-hexane and a dichloromethane solvent molecule located about crystallographic inversion centres. The IrIII atom displays a distorted octahedral coordination geometry, having three C,N-chelating 2,6-difluoro-3-[5-(2-fluorophenylpyridin-2-yl]pyridin-4-yl ligands arranged in a meridional manner. The IrIII ion lies almost in the equatorial plane [deviation = 0.0069 (15 Å]. The average distance [2.041 (3 Å] of Ir—C bonds is slightly shorter than that [2.076 (3 Å] of Ir—N bonds. A variety of intra- and intermolecular C—H...F and C—H...π hydrogen bonds, as well as intermolecular C—F...π interactions, contribute to the stabilization of the molecular and crystal structures, and result in the formation of a two-dimensional network parallel to the ab plane. No interactions between n-hexane solvent molecules and the other components in the title compound are observed.

  3. Synthesis, vibrational and optical properties of a new three-layered organic-inorganic perovskite (C4H9NH3)4Pb3I4Br6

    International Nuclear Information System (INIS)

    Dammak, T.; Elleuch, S.; Bougzhala, H.; Mlayah, A.; Chtourou, R.; Abid, Y.

    2009-01-01

    An organic-inorganic hybrid perovskite (C 4 H 9 NH 3 ) 4 Pb 3 I 4 Br 6 was synthesized and studied by X-ray diffraction, Raman and infrared spectroscopies, optical transmission and photoluminescence. The title compound, abbreviated (C 4 ) 4 Pb 3 I 4 Br 6 , crystallises in a periodic two-dimensional multilayer structure with P2 1 /a space group. The structure is built up from alternating inorganic and organic layers. Each inorganic layer consists of three sheets of PbX 6 (X=I, Br) octahedra. Raman and infrared spectra of the title compound were recorded in the 100-3500 and 400-4000 cm -1 frequency ranges, respectively. An assignment of the observed vibration modes is reported. Optical transmission measurements, performed on thin films of (C 4 ) 4 Pb 3 I 4 Br 6 , revealed two absorption bands at 474 and 508 nm. Photoluminescence measurements have shown a green emission peak at 519 nm.

  4. Aminosilanes derived from 1H-benzimidazole-2(3H)-thione

    Energy Technology Data Exchange (ETDEWEB)

    Palomo-Molina, Juliana [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico); García-Báez, Efrén V. [Unidad Profesional Interdisciplinaria de Biotecnología, Instituto Politécnico Nacional, Avenida Acueducto s/n, Barrio La Laguna Ticomán, México DF 07340 (Mexico); Contreras, Rosalinda [Departamento de Química, Centro de Investigación y de Estudios Avanzados del IPN, Apartado Postal 14-740, México DF 07000 (Mexico); Barrio La Laguna Ticomán, México DF 07340 (Mexico); Pineda-Urbina, Kayim; Ramos-Organillo, Angel, E-mail: aaramos@ucol.mx [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico)

    2015-08-12

    In two trimethylsilyl-substituted 1H-benzimidazole-2(3H)-thiones, noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in one, and dimerization results in the formation of R{sub s} {sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings, in the second compound. Two new molecular structures, namely 1,3-bis(trimethylsilyl)-1H-benzimidazole-2(3H)-thione, C{sub 13}H{sub 22}N{sub 2}SSi{sub 2}, (2), and 1-trimethylsilyl-1H-benzimidazole-2(3H)-thione, C{sub 10}H{sub 14}N{sub 2}SSi, (3), are reported. Both systems were derived from 1H-benzimidazole-2(3H)-thione. Noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in (2). Dimerization of (3) results in the formation of R{sub 2}{sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings.

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

    OpenAIRE

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

    2011-01-01

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

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

    International Nuclear Information System (INIS)

    Ke, W.; Sun, N.B.

    2013-01-01

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

  7. 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.

  8. 9-Ethyl-3,6-diformyl-9H-carbazole

    Directory of Open Access Journals (Sweden)

    Jun Jie Wang

    2008-07-01

    Full Text Available The structure of the title compound, C16H13NO2, was determined as a part of a project on the synthesis of new compounds which can make two-photon absorptions. In the crystal structure, both aldehyde groups are located within the carbazole plane. One of these groups is disordered and was refined using a split model with site-occupation factors for each position of 0.5.

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

    NARCIS (Netherlands)

    Duchateau, R; Meetsma, A; Teuben, JH

    1996-01-01

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

  10. 3-Cyanoanilinium nitrate

    Directory of Open Access Journals (Sweden)

    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.

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

    Science.gov (United States)

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

    2012-01-01

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

  12. 4-({[6-(4-Chlorobenzyl-4-methyl-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl]sulfanyl}acetyl-3-phenylsydnone

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    Hoong-Kun Fun

    2011-04-01

    Full Text Available In the title syndone (1,2,3-oxadiazol-3-ylium-5-olate compound, C21H16ClN5O4S, the dihedral angle between the benzene and oxadiazole rings is 55.62 (11° and that between the triazine and the chloro-substituted phenyl rings is 82.45 (9°. There is an intramolecular C—H...S hydrogen bond, which generates an S(5 ring motif. In the crystal, inversion dimers linked by pairs of C—H...O hydrogen bonds generate R22(20 loops. The dimers are connected by C—H...N and C—H...O hydrogen bonds.

  13. 4-(2,3-Dihydroxybenzylideneamino-3-methyl-1H-1,2,4-triazol-5(4H-one

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    Şamil Işık

    2009-12-01

    Full Text Available All the non-H atoms of the title compound, C10H10N4O3, are almost coplanar, the maximum deviation from planarity being 0.065 (3 Å. The dihedral angle between the aromatic rings is 1.66 (6°. The molecule adopts the enol–imine tautomeric form with an intramolecular hydrogen-bonding interaction between the Schiff base N atom and the hydroxy group. In the crystal, intermolecular N—H...O and O—H...O hydrogen bonds link the molecules into a three-dimensional network.

  14. (4R-4-Benzyl-3-{(4S-4-chloro-4-[(S-2,2-dimethyl-1,3-dioxolan-4-yl]butanoyl}-1,3-oxazolidin-2-one

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    Sandra Börding

    2012-01-01

    Full Text Available The title compound, C19H24ClNO5, was synthesized and subsequently employed in an Evans alkylation. The purpose was to prove the absolute configuration in the projected synthesis of the side chain of (–-Lytophilippine A. The oxazolidinone and the isopropylidene acetal rings have twisted conformations. The oxazolidinone and side-chain carbonyl groups are orientated in an antiperiplanar arrangement to minimize van der Waals repulsions. Furthermore, the Cl atom and the acetonide-protected secondary alcohol are also in an antiperiplanar arrangement with a torsion angle of 173.64 (14°. The absolute configuration was determined and agrees with the configuration of the used chiral auxiliary.

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

    Science.gov (United States)

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

    2016-09-19

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

  16. 2,2′-(Diselane-1,2-diyldinicotinamide N,N′-dimethylformamide disolvate

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    Aixia Feng

    2010-05-01

    Full Text Available The asymmetric unit of the title compound, C12H10N4O2Se2·2C3H7NO, contains two solvent molecules and two half molecules of the dinicotinamide, each of which sits on a center of symmetry passing through the middle of the Se—Se bond. In each molecule, the two pyridyl groups and diseleno group are approximately coplanar (r.m.s. deviations from planarity for all non-H atoms = 0.011 and 0.008 Å in the two molecules. Intermolecular N—H...O hydrogen bonds stablilize the crystal packing.

  17. Ethyl 2-amino-4-(3-chlorophenyl-5,10-dioxo-5,10-dihydro-4H-benzo[g]chromene-3-carboxylate

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    Xiao Hu

    2009-06-01

    Full Text Available The title molecule, C22H16ClNO5, was obtained by the reaction of (E-ethyl 3-(3-chlorophenyl-2-cyanoacrylate and 2-hydroxynaphthalene-1,4-dione catalysed by triethylamine in ethanol. In the crystal structure, the chlorobenzene ring makes a dihedral angle of 88.63 (4° with the fused ring system. The six-membered ring formed by an intramolecular N—H...O hydrogen bond is almost planar. The crystal packing is stabilized by N—H...O hydrogen bonds.

  18. 2,5-Bis[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctylsulfanyl]-1,3,4-thiadiazole

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    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.

  19. (6S-2-tert-Butyl-6-[(4S,5R-3,4-dimethyl-5-phenyloxazolidin-2-yl]phenol

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    Alexander E. Anderson

    2010-04-01

    Full Text Available The title compound, C21H27NO2, exhibits hydrogen bonding between the phenolic H atom and the heterocyclic N atom. The absolute configuration of the molecule is known from the synthetic procedure.

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

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    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].

  1. Pentacarbonyl-1κ2C,2κ3C-[(diphenylphosphoryldiphenylphosphane-1κP]-μ-ethane-1,2-dithiolato-1:2κ4S,S′:S,S′-diiron(I(Fe—Fe

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    Xu-Feng Liu

    2011-11-01

    Full Text Available The dinuclear title compound, [Fe2(C2H4S2(C24H20OP2(CO5] or (μ-SCH2CH2S-μFe2(CO5[Ph2PP(OPh2], contains a butterfly-shaped Fe2S2 core in which the Fe...Fe separation is 2.5275 (6 Å. One of the Fe atoms is also coordinated to three carbonyl ligands and the other to two carbonyl ligands and one phosphane ligand [Ph2PP(OPh2]. Both Fe-atom geometries could be described as grossly distorted octahedral and the Ph2PP(OPh2 ligand lies trans to the Fe...Fe link.

  2. 2,2′-[1,1′-(Heptane-1,7-diyldioxydinitrilodiethylidyne]di-1-naphthol

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    Wen-Kui Dong

    2009-07-01

    Full Text Available The molecule of the title compound, C31H34N2O4, adopts an L-shaped configuration, in which the naphthalene units are approximately perpendicular, making a dihedral angle of 87.89 (3°. Intramolecular H-bonds are formed between the OH substituents and the N atoms at each end of the molecule. In the crystal structure, each molecule links six other molecules into an infinite three-dimensional network supramolecular structure, which is built from one-dimensional zigzag chains via weak C—H...π stacking and intermolecular C—H...O hydrogen bonds.

  3. 4-[(3-Hydroxyanilino(phenylmethylidene]-3-methyl-1-phenyl-1H-pyrazol-5(4H-one

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    Keraghel Saida

    2012-06-01

    Full Text Available In the title compound, C23H19N3O2, the dihedral angles formed by the pyrazolone ring with the three benzene rings are 30.91 (6, 60.96 (4 and 57.01 (4°. The ligand is in the enamine–keto form and its structure is stabilized by an intramolecular N—H...O hydrogen bond. In the crystal, O—H...N hydrogen bonds link molecules into chains parallel to [01-1].

  4. Mechanism of improved maintenance of 2,3-diphosphoglycerate in stored blood by the xanthone compound 2-(2-hydroxyethoxy)-6-(1-H-tetrazole-5-yl)xanthen-9-one (BW A440C).

    Science.gov (United States)

    Beutler, E; Forman, L; West, C; Gelbart, T

    1988-03-15

    The effect of the xanthone derivative 2-(2-hydroxyethoxy)-6-(1-H-tetrazole-5-yl)xanthen-9-one (BW A440C) on red cells was studied. When added to stored red cells at a concentration of 6 mM, greatly improved preservation of 2,3-diphosphoglycerate (2,3-DPG) was observed. There was no effect on internal pH of the erythrocyte. At a concentration 0.500 mM, many red cell enzyme activities were inhibited completely. At a 0.500 mM concentration, however, inhibition of pyruvate kinase and diphosphoglycerate phosphatase was most striking. Inhibition of either of these enzymes could result in elevation of 2,3-DPG levels. BW A440C in concentrations which elevated 2,3-DPG levels in humans caused a decrease in 2,3-DPG levels in rabbits and markedly impaired the viability of 21-day stored rabbit erythrocytes.

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

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    M. S. Begum

    2015-12-01

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

  6. 4,4-Dimethyl-3,4-dihydropyrido[2′,3′:3,4]pyrazolo[1,5-a][1,3,5]triazin-2-amine ethanol monosolvateFused heterocyclic systems with s-triazine ring. Part 16. for part 15, see Sachdeva et al. (2010.

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    Lip Lin Koh

    2011-01-01

    Full Text Available In the title compound, C10H12N6·C2H5OH, the planarity of the heterocyclic system is slightly distorted at the triazine ring (r.m.s. deviation = 0.1191 Å, which adopts a conformation best described as intermediate between a flattened twisted boat and a half-boat with the tertiary Csp3 atom at the bow. In the crystal, molecules form centrosymmetric dimers connected by N...H—O and O...H—N hydrogen bonds between the amino group H atom, the ethanol solvent molecule and the triazine N atom, making an R44(12 graph-set motif. The other H atom of the amino group and the H atom on the endocyclic N atom form N...H—N hydrogen bonds with the N atoms of the pyrazole and pyridine rings, respectively, linking the molecules into C(7C(7 chains with the R22(8 binary graph-set motif running along [010].

  7. (2,2′-Bipyridine-κ2N,N′iodido(piperidine-1-carbodithioato-κ2S,S′copper(II

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    Le-Qing Fan

    2009-01-01

    Full Text Available In the title compound, [Cu(C6H10NS2I(C10H8N2], the CuII ion is coordinated by one iodide ion, two N atoms of the bipyridine ligand and two S atoms from the piperidinecarbodithioate ligand in a distorted square-pyramidal environment. π–π stacking interactions, with centroid–centroid distances of 3.643 (4 Å, between pyridyl rings of the bipyridyl ligands of neighbouring molecules lead to chains propagating parallel to the a axis.

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

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    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.

  9. 2,2′-Dihydroxybiphenyl-3,3′-dicarbaldehyde dioxime

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    Ekaterina Golovnia

    2009-08-01

    Full Text Available The molecule of the title compound, C14H12N2O4, lies across a crystallographic inversion centre situated at the mid-point of the C—C intra-annular bond. The molecule is not planar, the dihedral angle between the aromatic rings being 50.1 (1°. The oxime group is in an E position with respect to the –OH group and forms an intramolecular O—H...N hydrogen bond. In the crystal structure, intermolecular O—H...O hydrogen bonds link molecules into chains propagating along [001]. The crystal structure is further stabilized by intermolecular stacking interactions between the rings [centroid-to-centroid distance = 3.93 (1 Å], resulting in layers parallel to the bc plane.

  10. Crystal structure of the salt bis(triethanolamine-κ4N,O,O′,O′′cadmium bis[2-(2-oxo-2,3-dihydro-1,3-benzothiazol-3-ylacetate

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    Jamshid Mengnorovich Ashurov

    2016-04-01

    Full Text Available The reaction of 2-(2-oxo-2,3-dihydro-1,3-benzothiazol-3-ylacetic acid (NBTA and triethanolamine (TEA with Cd(CH3OO2 resulted in the formation of the title salt, [Cd(C6H15NO32](C9H6NO3S2. In its crystal structure, the complex cation [Cd(TEA2]2+ and two independent NBTA− units with essentially similar geometries and conformations are present. In the complex cation, each TEA molecule behaves as an N,O,O′,O′′-tetradentate ligand, giving rise to an eight-coordinate CdII ion with a bicapped trigonal–prismatic configuration. All ethanol groups of each TEA molecule form three five-membered chelate rings around the CdII ion. The Cd—O and Cd—N distances are in the ranges 2.392 (2–2.478 (2 and 2.465 (2–2.475 (3 Å, respectively. O—H...O hydrogen bonds between the TEA hydroxy groups and carboxylate O atoms connect cationic and anionic moieties into chains parallel to [110]. Each NBTA− anion is additionally linked to a symmetry-related anion through π–π stacking interactions between the benzene and thiazoline rings [minimum centroid-to-centroid separation = 3.604 (2 Å]. Together with additional C—H...O interactions, these establish a double-layer polymeric network parallel to (001.

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

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    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.

  12. 6-Bromo-2-(4-chlorophenyl-3-methyl-3H-imidazo[4,5-b]pyridine

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    Selma Bourichi

    2016-05-01

    Full Text Available In the title compound, C13H9BrClN3, the imidazopyridine fused-ring system is almost planar, with r.m.s. deviation of 0.006 (19 Å, and makes a dihedral angle of 29.32 (8° with the mean plane of the 4-chlorophenyl group. In the crystal, C—H...N hydrogen bonds link the molecules into chains propagating in the [100] direction. Weak intermolecular π–π interactions between the five- and six-membered rings of the 3H-imidazo[4,5-b]pyridine moieties of neighbouring molecules [centroid–centroid distance = 3.8648 (12 Å] further consolidate the packing into layers parallel to the ab plane.

  13. 4-(Prop-2-yn-1-ylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine

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    Mohamed El Hafi

    2017-10-01

    Full Text Available The asymmetric unit of the title compound, C8H6N4S, consists of two independent molecules differing in the orientation of the side chain. In the crystal, molecules form dimers through N—H...N hydrogen bonds. The dimers stack along the a-axis direction with weak π–π stacking interactions [centroid–centroid distances of 3.898 (2 and 3.908 (2 Å]. The crystal studied was refined as a two-component twin.

  14. 1,1′-[Imidazolidine-1,3-diylbis(methylene]bis(1H-benzotriazole

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    Augusto Rivera

    2012-02-01

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

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

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    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.

  16. 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.

  17. 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

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    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.

  18. 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.

  19. Crystal structure of ethyl (E-2-cyano-3-(thiophen-2-ylacrylate: two conformers forming a discrete disorder

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    Brian Castro Agudelo

    2017-09-01

    Full Text Available In the title compound, C10H9NO2S, all the non-H atoms, except for the ethyl fragment, lie nearly in the same plane. Despite the molecular planarity, the ethyl fragment presents more than one conformation, giving rise to a discrete disorder, which was modelled with two different crystallographic sites for the ethoxy O and ethoxy α-C atoms, with occupancy values of 0.5. In the crystal, the three-dimensional array is mainly directed by C—H...(O,N interactions, giving rise to inversion dimers with R22(10 and R22(14 motifs and infinite chains running along the [100] direction.

  20. 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)

  1. Solvothermal synthesis and characterisation of new one-dimensional indium and gallium sulphides: [C1N4H26]0.5[InS2] and [C1N4H26]0.5[GaS2

    International Nuclear Information System (INIS)

    Vaqueiro, Paz

    2006-01-01

    Two new main group metal sulphides, [C 1 N 4 H 26 ] 0.5 [InS 2 ] (1) and [C 1 N 4 H 26 ] 0.5 [GaS 2 ] (2) have been prepared solvothermally in the presence of 1,4-bis(3-aminopropyl)piperazine and their crystal structures determined by single-crystal X-ray diffraction. Both compounds are isostructural and crystallise in the monoclinic space group P2 1 /n (Z=4), with a=6.5628(5), b=11.2008(9), c=12.6611(9) A and β=94.410(4) o (wR=0.035) for compound (1) and a=6.1094(5), b=11.2469(9), c=12.7064(10) A and β=94.313(4) o (wR=0.021) for compound (2). The structure of [C 1 N 4 H 26 ] 0.5 [MS 2 ] (M=In,Ga) consists of one-dimensional [MS 2 ] - chains which run parallel to the crystallographic a axis and are separated by diprotonated amine molecules. These materials represent the first example of solvothermally prepared one-dimensional gallium and indium sulphides. -- Graphical abstract: [C 1 N 4 H 26 ] 0.5 [InS 2 ] and [C 1 N 4 H 26 ] 0.5 [GaS 2 ], prepared under solvothermal conditions, consist of one-dimensional [MS 2 ] - chains separated by diprotonated 1,4-bis(3-aminopropyl)piperazine molecules

  2. Crystal structure of bis-[(acetato-κO)(imidazolidine-2-thione-κS)bis-(tri-phenyl-phosphane-κP)silver(I)] di-μ-imidazol-idine-2-thione-κ(4) S:S-bis-[(imidazol-id-ine-2-thione-κS)bis-(tri-phenyl-phosphane-κP)silver(I)] di-acetate aceto-nitrile disolvate tetra-hydrate.

    Science.gov (United States)

    Nimthong-Roldán, Arunpatcha; Ratthiwan, Janejira; Lakmas, Sawanya; Wattanakanjana, Yupa

    2016-04-01

    In the title compound, [Ag2(C3H6N2S)4(C18H15P)2](C2H3O2)2·[Ag(C2H3O2)(C3H6N2S)(C18H15P)2]2·2C2H3N·4H2O, the Ag(I) ion in the mononuclear neutral complex exhibits a distorted tetra-hedral environment with coordination by two P atoms from tri-phenyl-phosphane (PPh3) ligands, one S atom of an imidazolidine-2-thione (etu) ligand and one O atom of an acetate anion. The binuclear cationic complex comprises two inversion-related [Ag(C3H6N2S)2(C18H15P)] units with Ag(I) ions bridged by two S atoms from etu ligands forming a four-membered Ag-S-Ag-S ring. Each Ag(I) ion is coordinated by a P atom of a PPh3 ligand, two S atoms of bridging etu ligands and the terminal S atom of an etu ligand in a distorted tetra-hedral environment. In the crystal, the mononuclear complex is linked to lattice water mol-ecules through O-H⋯O and N-H⋯O hydrogen bonds, forming a chain along [100]. In addition, the binuclear complex mol-ecules are connected to acetate anions and lattice water mol-ecules via O-H⋯O, N-H⋯O and O-H⋯S hydrogen bonds, also along [100].

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

    Directory of Open Access Journals (Sweden)

    Yan-Lin Zhang

    2011-10-01

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

  4. N-[5-Methyl-2-(2-nitro-phen-yl)-4-oxo-1,3-thia-zolidin-3-yl]pyridine-3-carboxamide monohydrate.

    Science.gov (United States)

    Akkurt, Mehmet; Celik, Ismail; Demir, Hale; Ozkırımlı, Sumru; Büyükgüngör, Orhan

    2011-01-08

    In the title compound, C(16)H(14)N(4)O(4)S·H(2)O, the benzene and pyridine rings make a dihedral angle of 85.8 (1)°. Both enanti-omers of the chiral title compound are statistically disordered over the same position in the unit cell. The methyl and carbonyl group attached to the stereogenic center (C(5) of the thia-zolidine ring) were therefore refined with common site-occupation factors of 0.531 (9) and 0.469 (9), respectively, for each stereoisomer. In the crystal, inter-molecular N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds link the mol-ecules, forming a three-dimensional supra-molecular network. The crystal structure further shows π-π stacking inter-actions [centroid-centroid distance = 3.5063 (13) Å] between the pyridine rings.

  5. 3-Ethylsulfinyl-2-(4-iodophenyl-5-methyl-1-benzofuran

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    Hong Dae Choi

    2010-08-01

    Full Text Available In the title compound, C17H15IO2S, the 4-iodophenyl ring makes a dihedral angle of 35.39 (8° with the plane of the benzofuran fragment. In the crystal, molecules are linked by intermolecular C—H...O and C—H...π interactions, and an I...O contact [3.378 (2 Å]. The crystal structure also exhibits aromatic π–π interactions between the benzene rings of neighbouring molecules [centroid–centroid distance = 3.495 (3 Å].

  6. Characterization, electrical transport and magnetic properties of the rare earth misfit layer compounds (TbS)(1.21)NbS2, (TbS)(1.20)TaS2, (DyS)(1.22)NbS2 and (DyS)(1.21)TaS2

    NARCIS (Netherlands)

    Zhou, W.Y.; Meetsma, A.; deBoer, J.L.; Wiegers, G.A

    1996-01-01

    X-ray powder and single-crystal X-ray diffraction of the title compounds showed that they are planar intergrowth compounds, built of alternating sandwiches TS2 (T=Nb, Ta) and double layers LnS (Ln=Tb, Dy), present in three orientational variants related by rotations of 120 degrees around the c axis

  7. 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.

  8. 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.

  9. 2,6-Diaminopyridinium bis(4-hydroxypyridine-2,6-dicarboxylato-κ3O2,N,O6ferrate(III dihydrate

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    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.

  10. 2-[3-(Naphthalen-2-ylphenyl]naphthaleneCAS 103068–173.

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    Mark L. Wolfenden

    2013-02-01

    Full Text Available The title compound, C26H18, consists of a benzene ring with meta-substituted 2-naphthalene substituents, which are essentially planar [r.m.s. deviations = 0.022 (1 and 0.003 (1 Å]. The conformation is syn, with equivalent torsion angles about the benzene–naphthalene bonds of −36.04 (13 and +34.14 (13°. The molecule has quasi-Cs molecular symmetry.

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

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    Lucimara Julio Martins

    2014-12-01

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

  12. 1-[3-(4-Chlorophenyl-5-(4-methoxyphenyl-4,5-dihydro-1H-pyrazol-1-yl]ethanone

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    Hoong-Kun Fun

    2012-04-01

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

  13. Synthesis and vibrational spectra of cooper(II) and erbium(III) complexes with 2-diazo[2'-(oxymethyldiphenylphosphinyl)phenyl]-4-tert-butylphenol (HL) - [CuL2]·2H2O and Er(NO3)3·2HL·2H2O. Crystal structure of [CuL2]·2H2O

    International Nuclear Information System (INIS)

    Tsivadze, A.Yu.; Minacheva, L.Kh.; Ivanova, I.S.; Pyatova, E.N.; Sergienko, V.S.; Baulin, V.E.

    2008-01-01

    Paper describes synthesis of CuL 2 ·2H 2 O (I) complex cupric salt and of Er(NO 3 ) 3 ·2HL·2H 2 O (II) erbium nitrate complex (HL=2-diazo-[2'(oxymethyl-diphenyl-phosphinyl)phenyl]-4-tert-butylphenol). One interprets the fundamental frequencies within the IR-spectra of (I) and (II) compounds. One has performed X-ray diffraction analysis of I compound. The crystals are monoclinic ones, a=15.157(3), b=17.080(2), c=22.451(9) A, β=106.09(3) Deg, V=5584(3) A 3 , Z=4, C2/c sp.gr., R=0.0546 as to 1152 reflections with I>2σ(I). The copper atom coordination polyhedron (C 2 symmetry) may be described as a symmetrically-prolonged square bipyramid (4+2). Cu polyhedron central square is formed by substituted phenol oxygen atom and by one of diazo-group nitrogen atoms of either of two deprotonated ligands, namely: L - (Cu-N 1.969(6), Cu-O 1.899(5) A). The angles between lying opposite O and N atoms constitute 157.6 Deg, while the rest equatorial angles range within 90.6 Deg-95.9 Deg. The axial positions are occupied by O(2) and O(2A) anisole atoms (Cu-O 2.737(6) A, O(2)Cu(1)O(2A) angle constitutes 132.3 Deg). Within crystal I the complex molecules and the crystallization molecules of water are combined by by the hydrogen bond system. According to the IR-spectra data, within complex II in contrast to compound I erbium atom coordination by HL ligand involves oxygen phosphoryl atom [ru

  14. 4-Methyl-5-phenyl-1H-pyrazol-3-ol

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    Tara Shahani

    2010-07-01

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

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

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    Muhammet Işıklan

    2010-11-01

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

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

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    Shao-Ming Ying

    2008-01-01

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

  17. (2-Methyl-4-oxo-4H-pyran-3-olato-κ2O3,O4bis(triphenylphosphane-κPcopper(I–triphenylphosphane–methanol (1/1/1

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    Fabian M. A. Muller

    2011-05-01

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

  18. N,N',N"-Tris[(5-methoxy-1H-indol-3-ylethyl]benzene-1,3,5-tricarboxamide

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    Ute Schmidt

    2015-03-01

    Full Text Available The title indole-based compound that enforces tripodal topology and is potential applicable for the use as artificial receptor, was prepared by a simple reaction of 1,3,5-benzenetricarbonyl trichloride with 5-methoxytryptamine. The compound was characterized by elemental analysis, 1H-NMR, 13C-NMR and mass spectrometry.

  19. 4-(3-Bromopropyloxy-1-hydroxy-9,10-anthraquinone

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    Natsumi Ohira

    2016-05-01

    Full Text Available In the molecule of the title compound, C17H13BrO4, the anthraquinone ring system is slightly bent, with a dihedral angle of 169.99 (7° between the planes of the two benzene rings. The side chain (O—C—C—C—Br has a gauche–gauche conformation, as indicated by the O—C—C—C and C—C—C—Br torsion angles of −66.9 (2 and −65.8 (2°, respectively. In addition, there is an intramolecular O—H...O hydrogen bond enclosing an S(6 ring motif. The hydrogen-bond donor is bifurcated; in the crystal, a pair of O—H...O hydrogen bonds connects two molecules, forming an inversion dimer with an R22(12 ring motif.

  20. 4-((E-{2-[N-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylcarboximidoyl]benzylidene}amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

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    Richard Betz

    2011-10-01

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

  1. 5-Bromo-4-(3,4-dimethoxyphenylthiazol-2-amine

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    Hazem A. Ghabbour

    2012-06-01

    Full Text Available In the title compound, C11H11BrN2O2S, the thiazole ring makes a dihedral angle of 53.16 (11° with the adjacent benzene ring. The two methoxy groups are slightly twisted from the attached benzene ring with C—O—C—C torsion angles of −9.2 (3 and −5.5 (3°. In the crystal, molecules are linked by a pair of N—H...N hydrogen bonds into an inversion dimer with an R22(8 ring motif. The dimers are further connected by N—H...O hydrogen bonds into a tape along [-110].

  2. 1,3-Bis[(4-nitrobenzylideneaminooxy]propane

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    Wen-Kui Dong

    2009-09-01

    Full Text Available The complete molecule of title compound, C17H16N4O6, is generated by a crystallographic twofold axis. Within the molecule, the two benzene units are approximately perpendicular, making a dihedral angle of 85.91 (4°. In the crystal, molecules are linked into a three-dimensional network by C—H...O hydrogen bonds and short O...O and N...O interactions, with distances of 2.998 (2 and 2.968 (3 Å, respectively.

  3. 3-[(R-3,3-Dichloro-2-hydroxypropyl]-8-hydroxy-6-methoxy-1H-isochromen-1-one

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    Yong-Cheng Lin

    2008-09-01

    Full Text Available The title compound, C13H12Cl2O5, is an isocoumarin compound which has been isolated from the ethyl acetate extract of the fermentation broth of actinomycete Streptomyces sp. (V4 from the South China Sea. There are intra- and intermolecular hydrogen bonds and halogen bonds [Cl...Cl = 3.434 (2 Å; C—Cl...Cl = 121.6°]. The intermolecular O—H...O hydrogen bonds link molecules into chains along the b 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. Intrinsic magnetic properties of Sm{sub 2}Fe{sub 17-x}M{sub x}N{sub y}/C{sub y} (M=Al, Ga or Si)

    Energy Technology Data Exchange (ETDEWEB)

    Kubis, M.; Eckert, D.; Gebel, B.; Mueller, K.-H. E-mail: khm@ifw-dresden.de; Schultz, L

    2000-07-01

    Curie temperature T{sub c}, saturation polarization J{sub s} and anisotropy field H{sub a} of Sm{sub 2}Fe{sub 17-x}M{sub x}N{sub y}/C{sub y} with M=Al, Ga or Si (x{<=}3, y{approx}3) were determined by thermomagnetic measurements and a numerical fitting procedure of demagnetization curves. An increasing amount of the substitutional element M leads to an increase of T{sub c} of the Sm{sub 2}Fe{sub 17-x}M{sub x} parent compounds and generally to a decrease of T{sub c}, J{sub s} and H{sub a} for the interstitial nitrides and carbides. However, for small M contents, x{<=}1, an increased H{sub a} was observed compared to the substitution-free interstitial compounds. Gas-carburized and melt-carburized Sm{sub 2}Fe{sub 15}Ga{sub 2}C{sub y} samples showed large differences in J{sub s} and H{sub a} but identical T{sub c} values.

  6. 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

  7. (R,S)-3-Carb-oxy-2-(isoquinolinium-2-yl)propanoate monohydrate.

    Science.gov (United States)

    Stilinović, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-05-22

    The title compound, C(13)H(11)NO(4)·H(2)O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquino-line group and a deprotonated carboxyl group. In the crystal, mol-ecules are connected via short O-H⋯O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enanti-omers along [001]. These chains are additionally connected by hydrogen bonding between water mol-ecules and the deprotonated carb-oxy groups of neighbouring mol-ecules.

  8. 1-Chloro-3-(6-nitro-1H-indazol-1-ylpropan-2-ol

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    Mohamed Mokhtar Mohamed Abdelahi

    2017-05-01

    Full Text Available In the title compound, C10H10ClN3O3, the side chain is oriented nearly perpendicular to the mean plane of the indazole ring system. In the crystal, complementary sets of O—H...N and C—H...O hydrogen bonds form chains of molecules stacked along the a-axis direction

  9. 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.

  10. Ethyl 2-[(5Z-5-(4-methoxybenzylidene-2,4-dioxo-1,3-thiazolidin-3-yl]acetate

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    Hamza Tachallait

    2016-07-01

    Full Text Available In the title compound, C15H15NO5S, the benzene and heterocyclic rings are close to being coplanar [dihedral angle = 1.49 (6°]. In the crystal, pairwise C—H...O hydrogen bonds form dimers, which are arranged into `stair-step' rows by way of C=O–π interactions between a carbonyl group and the benzene ring [O...π = 3.3837 (12 Å].

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

    OpenAIRE

    Liu, Yaru; Sun, Junshan; Wang, Xinli

    2009-01-01

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

  12. 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.

  13. (E)-6-Amino-1,3-dimethyl-5-[(pyridin-2-yl-methyl-idene)amino]-pyrimidine-2,4(1H,3H)-dione.

    Science.gov (United States)

    Booysen, Irvin; Hlela, Thulani; Ismail, Muhammed; Gerber, Thomas; Hosten, Eric; Betz, Richard

    2011-09-01

    In the title compound, C(12)H(13)N(5)O(2), a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å). The N=C bond is E-configured. Intra-cyclic angles in the pyridine moiety cover the range 117.6 (2)-124.1 (2)°. Intra- and inter-molecular N-H⋯N and N-H⋯O hydrogen bonds are observed in the crystal structure, as are intra- and inter-molecular C-H⋯O contacts which, in total, connect the mol-ecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14) Å is between the two different types of six-membered rings.

  14. Vinclozolin: 3-(3,5-dichlorophenyl-5-ethenyl-5-methyl-1,3-oxazolidine-2,4-dione

    Directory of Open Access Journals (Sweden)

    Seonghwa Cho

    2014-07-01

    Full Text Available In the title compound, C12H9Cl2NO3, which is the fungicide vinclozolin, the dihedral angle between the oxazolidine ring mean plane [r.m.s. deviation = 0.029 Å] and the benzene ring is 77.55 (8°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming chains along [010]. The chains are linked by short Cl...Cl contacts [3.4439 (3 and 3.5798 (3 Å], resulting in a three-dimensional architecture.

  15. 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...

  16. (4aS,10aS-7-Hydroxy-8-isopropyl-1,1,4a-trimethyl-1,2,3,4,4a,9,10,10a-octahydrophenanthrene: a new diterpenoid compound

    Directory of Open Access Journals (Sweden)

    Ahmed Benharref

    2008-03-01

    Full Text Available The new title diterpenoid compound, C20H30O, is a natural product isolated from Tetraclinis articulata wood via chloroform extraction. The asymmetric unit contains four molecules with the same S,S configuration, deduced from the chemical synthesis. Indeed, an overlay analysis, calculated using structure-matching software, shows that the four molecules can be superimposed. The central ring has a half-chair conformation, whereas the saturated ring displays a chair conformation.

  17. 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.

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

    OpenAIRE

    Xu, Sheng-Zhen

    2007-01-01

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

  19. Coordination compounds of the nitrate salts of oxycation uranyl (UO22+) and praseodymium(III), neodymium(III) and erbium(III) with 2,2'-bipyridine-1,1'-dioxide

    International Nuclear Information System (INIS)

    Madan, S.; Chan, K.S.

    1977-01-01

    Coordination compounds with 2,2'-bipyridine-1,1'-dioxide (bipyO 2 ) having the composition [UO 2 (bipyO 2 ) 2 (NO 3 ) 2 ].4H 2 O, [Pr(bipyO 2 ) 4 (NO 3 ) 2 ]NO 3 .2H 2 O, [Dy(bipyO 2 ) 4 (NO 3 ) 2 ]NO 3 .4H 2 O and [Er(bipyO 2 ) 4 (NO 3 ) 2 ]NO 3 .4H 2 O have been synthesized. These new complexes have been characterized by electrical conductance, X-ray powder patterns and IR spectral measurements. (author)

  20. Multiple anion...π interactions in tris(1,10-phenanthroline-κ(2)N,N')iron(II) bis[1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide] monohydrate.

    Science.gov (United States)

    Setifi, Zouaoui; Domasevitch, Konstantin V; Setifi, Fatima; Mach, Pavel; Ng, Seik Weng; Petříček, Vaclav; Dušek, Michal

    2013-11-01

    In the ionic structure of the title compound, [Fe(C12H8N2)3](C9H5N4O2)2·H2O, the octahedral tris-chelate [Fe(phen)3](2+) dications [Fe-N = 1.9647 (14)-1.9769 (14) Å; phen is 1,10-phenathroline] afford one-dimensional chains by a series of slipped π-π stacking interactions [centroid-to-centroid distances = 3.792 (3) and 3.939 (3) Å]. The 1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide anions, denoted tcnoetOH(-), reveal an appreciable delocalization of π-electron density, involving the central propenide [C-C = 1.383 (3)-1.401 (2) Å] fragment and four nitrile groups, and this is also supported by density functional theory (DFT) calculations at the B97D/6-311+G(2d,2p) level. Primary noncovalent inter-moiety interactions comprise conventional O-H...O(N) and weak C-H...O(N) hydrogen bonding [O...O(N) = 2.833 (2)-3.289 (5) Å and C...O(N) = 3.132 (2)-3.439 (2) Å]. The double anion...π interaction involving a nitrile group of tcnoetOH(-) and two cis-positioned pyridine rings (`π-pocket') of [Fe(phen)3](2+) [N...centroid = 3.212 (2) and 3.418 (2) Å] suggest the relevance of anion...π stackings for charge-diffuse polycyanoanions and common M-chelate species.

  1. Crystal structure of chlorido(η2-phenyl isothiocyanate-κ2C,S-mer-tris(trimethylphosphane-κPiridium(I

    Directory of Open Access Journals (Sweden)

    Joseph S. Merola

    2014-11-01

    Full Text Available The molecule of the title compound, [IrCl(C7H5NS(C3H9P3], is a distorted octahedral iridium complex with three PMe3 ligands arranged in a meridional geometry, a chloride ion cis to all three PMe3 groups and the phenyl isothiocyanate ligand bonded in an η2-fashion through the C and S atoms. The C atom is trans to the chloride ion and the S atom is responsible for a significant deviation from an ideal octahedral geometry. The geometric parameters for the metal-complexing phenyl isothiocyanate group are compared with other metal-complexed phenyl isothiocyanates, as well as with examples of uncomplexed aryl isothiocyanates.

  2. 3-Methyl-1-(prop-2-en-1-ylquinoxalin-2(1H-one

    Directory of Open Access Journals (Sweden)

    Youssef Ramli

    2010-07-01

    Full Text Available In the molecule of the title compound, C12H12N2O, the quinoxaline ring is planar with an r.m.s. deviation of 0.007 (15 Å. The dihedral angle between the quinoxaline and propenyl planes is 82.1 (2°. The crystal packing is stabilized by offset π–π stacking between the quinoxaline rings [centroid–centroid distance = 3.8832 (9 Å].

  3. 1,5-Bis(2-hydroxy-3-methoxybenzylidenecarbonohydrazide methanol 0.47-solvate

    Directory of Open Access Journals (Sweden)

    Mouhamadou Moustapha Sow

    2014-04-01

    Full Text Available In the title compound, C17H18N4O5·0.47CH3OH, the virtually planar (r.m.s. deviation = 0.128 Å carbonohydrazide molecule is located on a twofold axis and conformation of its C=N bonds is E. There are short intramolecular O—H...N hydrogen bonds between the hydroxy groups and hydrazide N atoms. In the crystal, bifurcated N—H...(O,O hydrogen bonds assemble the carbonohydrazide molecules into a three-dimensional network. There are C2 symmetric voids in this network, 47% of which are occupied by disordered methanol molecules.

  4. {1-[(3,5-Dimethyl-4H-1,2,4-triazol-4-ylimino]ethyl}ferrocene

    Directory of Open Access Journals (Sweden)

    Mao-Ping Song

    2008-10-01

    Full Text Available In the title compound, [Fe(C5H5(C11H13N4], the triazolyl and Cp ring form a dihedral angle of 76.6 (3°. In the crystal structure, there are both intra- and intermolecular C—H...π interactions, forming a one-dimensional chain structure along [010].

  5. 3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H-thione

    Directory of Open Access Journals (Sweden)

    Zbigniew Karczmarzyk

    2013-02-01

    Full Text Available The title compound, C11H13N3S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2:0.23 (2 for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3 Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18 and 86.56 (49° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15° and this conformation is stabilized by an intramolecular C—H...S contact. In the crystal, pairs of N—H...S hydrogen bonds link molecules into inversion dimers. π–π interactions are observed between the triazole and benzene rings, with centroid–centroid separations of 3.547 (4 and 3.544 (12 Å for components A and B, and slippages of 0.49 (6 and 0.58 (15 Å, respectively.

  6. Methyl (2Z-2-{[N-(2-formylphenyl-4-methylbenzenesulfonamido]methyl}-3-(naphthalen-1-ylprop-2-enoate

    Directory of Open Access Journals (Sweden)

    R. Madhanraj

    2012-02-01

    Full Text Available In the title compound, C29H25NO5S, the sulfonyl-bound benzene ring forms dihedral angles of 42.1 (1 and 48.5 (1°, respectively, with the formyl-substituted benzene ring and the naphthalene residue. In the crystal, pairs of C—H...O interactions lead to the formation of R22(10 inversion dimers, which are linked by further C—H...O interactions into supramolecular tapes running along [100]. The crystal packing is further stabilized by C—H...π interactions.

  7. 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.

  8. Production of 15N-enriched nitric acid (H15NO3

    Directory of Open Access Journals (Sweden)

    C. R. Sant Ana Filho

    2008-12-01

    Full Text Available Techniques that employ 15N have proved to be an important tool in many areas of the agronomic and biomedical sciences. Nevertheless, their use is limited by methodological difficulties and by the price of compounds in the international market. Nitric compounds (15NO3- have attracted the interest of researchers. However, these compounds are not currently produced in Brazil. Thus, in the present work H15NO3 was obtained from the oxidation of anhydrous 15NH3. The method we used differs from the industrial process in that the absorption tower is replaced with a polytetrafluoroethylene-lined, stainless-steel hydration reactor. The process output was evaluated based on the following parameters: reaction temperature; ratio of reagents; pressure and flow of 15NH3(g through the catalyst (Pt/Rh. The results showed that, at the best conditions (500 ºC; 50 % excess O2; 0.4 MPa; and 3.39 g.min-1 of 15NH3, a conversion percentage (N-15NH3 to N-15NO3- of 62.2 %, an overall nitrogen balance (N-15NH3 + N-15NO3- of 86.8 %, and purity higher than 99 % could be obtained.

  9. Vibrational spectrum of solid picene (C22H14)

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  10. Vinclozolin: 3-(3,5-di-chloro-phen-yl)-5-ethenyl-5-methyl-1,3-oxazolidine-2,4-dione.

    Science.gov (United States)

    Cho, Seonghwa; Kim, Jineun; Lee, Sangjin; Kim, Tae Ho

    2014-07-01

    In the title compound, C12H9Cl2NO3, which is the fungicide vinclozolin, the dihedral angle between the oxazolidine ring mean plane [r.m.s. deviation = 0.029 Å] and the benzene ring is 77.55 (8)°. In the crystal, mol-ecules are linked via C-H⋯O hydrogen bonds, forming chains along [010]. The chains are linked by short Cl⋯Cl contacts [3.4439 (3) and 3.5798 (3) Å], resulting in a three-dimensional architecture.

  11. 4-[(5-Hydroxy-3-methyl-1-phenyl-1H-pyrazol-4-ylphenylmethyl]-5-methyl-2-phenyl-1H-pyrazol-3(2H-one ethanol hemisolvate

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2009-01-01

    Full Text Available The asymmetric unit of the title compound, C27H24N4O2·0.5C2H6O, comprises two crystallographically independent molecules (A and B with slightly different conformations, and one ethanol molecule of crystallization. Intramolecular C—H...O and O—H...O hydrogen bonds generate six- and eight-membered rings, producing S(6 and S(8 ring motifs, respectively. In molecule A, one of the benzene rings is disordered over two positions, with site-occupancy factors of 0.542 (11 and 0.458 (11. The dihedral angles between the central benzene ring and the two outer benzene rings are 73.88 (9 and 82.6 (2/88.9 (2° in molecule A, and 80.81 (8 and 79.38 (8° in molecule B. In the crystal structure, molecules form infinite one-dimensional chains in the (101 plane. The crystal structure is stabilized by intermolecular O—H...N, N—H...N, N—H...O and C—H...O hydrogen bonds, weak C—H...π and π–π [centroid–centroid = 3.5496 (1 Å] interactions.

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

    OpenAIRE

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2010-03-03

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

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

    OpenAIRE

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2010-03-03

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

  16. 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)

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    NARCIS (Netherlands)

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

    1989-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Felix Katzsch

    2016-04-01

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

  20. Ethyl 2-cyano-5-oxo-5-(thiophen-2-yl-3-(3,4,5-trimethoxyphenylpentanoate

    Directory of Open Access Journals (Sweden)

    M. Prabhuswamy

    2012-12-01

    Full Text Available In the title compound, C21H23NO6S, the dihedral angle between the thiopene and benzene rings is 88.66 (6°. In the crystal, molecules are connected by C—H...N and C—H...O hydrogen bonds, forming a tape along [10-1]. In addition, C—H...π and π–π stacking [centroid–centroid distance = 3.879 (2 Å between the thiophene rings] interactions are observed.

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Giuseppe Daidone

    2013-10-01

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

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

    Science.gov (United States)

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

    2009-01-01

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

  4. Thermodynamic properties of hydrated cement phases: C-S-H, C-A-S-H and M-S-H

    International Nuclear Information System (INIS)

    Roosz, Cedric

    2016-01-01

    representative phases of the studied chemical system, and (ii) a precise knowledge of the structure and chemical formulas of these phases. Three types of hydrates were therefore synthesized and characterized: C-S-H, C-A-S-H and M-S-H. Analytical methods such as XRD, TGA and solid state NMR ( 29 Si, 27 Al) are used to ascertain similarities between the structure of C-(A-)S-H and that of tobermorite, and between the structure of M-S-H and that of Mg-Si phyllosilicates 2:1. Hydrates, however, have a lower crystallinity, with defects in the polymerization of silica chains, and random stacking faults (turbostratism). A multi-technique approach is also used, combining adsorption isotherm(water and nitrogen) and 1 HNMR with XRD and TGA, and allows characterization of different types of water more or less bound to the structure of C-(A-)S-H. This study allowed to highlight and quantify the different types of water in the C-(A-)S-H structure. The impact of the drying process was also highlighted on the quantification of different types of water, including interlayer water. The acquisition of thermodynamic parameters of the synthesized phases is carried out from the analysis of equilibrium solutions for the calculation of log K and Δ f G 0 , while calorimetric acquisitions permit obtaining heat capacities and the calculation of S 0 . Finally, enthalpy of formation of these phases is calculated from the Gibbs free energy of formation and entropies. The predictive model is developed from the acquired thermodynamic properties. The Gibbs free energy of formation Δ f G 0 is predicted from an electronegativity model, while Cp and S 0 are predicted through polyhedral decomposition model. Finally, a comparison of data obtained with those published in the literature, and the realization of predominance diagrams generalized to the whole CaO-MgO-Al 2 O 3 -SiO 2 -H 2 O system assess the reliability of the proposed model. (author) [fr

  5. (3R,4S,5S,8S,10R,13R-3-Hydroxykaura-9(11,16-dien-18-oic acid

    Directory of Open Access Journals (Sweden)

    Karren D. Beattie

    2012-02-01

    Full Text Available The title compound, C20H28O3, was isolated during our investigation into the chemical composition and pharmacological activity of Centipeda cunninghamii (DC. A. Braun & Asch. (Asteraceae. The enantiopure compound, a diterpene with a carbon skeleton, is composed of three six- and one five-membered rings in chair, twist-boat, half-chair and envelope conformations, respectively. Each molecule makes one intra- and one intermolecular O—H...O hydrogen bond in the crystal lattice, forming hydrogen-bonded chains along [010]. The absolute configuration of the compound was assigned on the basis of optical rotation measurements.

  6. 4,4′,4′′-Tris(2-pyridyl-2,2′,2′′-[(2,4,6-trimethylbenzene-1,3,5-triyltris(methylenetris(sulfanediyl]tripyrimidine

    Directory of Open Access Journals (Sweden)

    Ya-Wen Zhang

    2009-08-01

    Full Text Available The title compound, C39H33N9S3, features a mesitylene unit substituted with three thioether arms. The distances from the center of mesitylene unit to the N atoms of the three pyridine rings in the arms are 10.05 (1, 9.94 (3 and 8.79 (3 Å. The crystal structure shows weak intramolecular C—H...N hydrogen bonds.

  7. (3S,4S)-3-Ethyl-4-hydr-oxy-3-(3-methoxy-phen-yl)-1-methyl-azepan-1-ium d-tartrate dihydrate.

    Science.gov (United States)

    Wang, Xing-Hai; Chao, Bo; Qiu, Zhui-Bai

    2008-04-02

    In the title compound, C(16)H(26)NO(2) (+)·C(4)H(5)O(6) (-)·2H(2)O, a meptaz-inol derivative, three C atoms of the azepane ring are disordered over two positions, with site-occupancy factors of 0.80 and 0.20; the major disorder component adopts a twist-chair conformation, while the minor component has a chair conformation. The benzene ring is axially substituted on the heterocyclic ring, resulting in a folded conformation of the cation. The absolute configuration was determined with reference to d-tartaric acid. The crystal structure is stabilized by an extensive network of intra- and inter-molecular O-H⋯O hydrogen bonds.

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

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    Adel S. El-Azab

    2012-07-01

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

  9. Spectroscopic and molecular modeling studies of N-(4-(3-methyl-3-phenylcyclobutyl-3-phenylthiazole-2(3H-ylideneaniline by using experimental and density functional methods

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    Fatih Şen

    2017-05-01

    Full Text Available In the present study, a combined experimental and computational study on molecular structure and spectroscopic characterization on the title compound has been reported. The crystal was synthesized and its molecular structure brought to light by X-ray single crystal structure determination. The spectroscopic properties of the compound were examined by FT-IR and NMR (1H and 13C techniques. FT-IR spectra of the target compound in solid state were observed in the region 4000–400 cm−1. The 1H and 13C NMR spectra were recorded in CDCl3 solution. The molecular geometries were those obtained from the X-ray structure determination optimized using the density functional theory (DFT/B3LYP method with the 6-31G(d, p and 6-31G+(d, p basis set in ground state. From the optimized geometry of the molecule, geometric parameters (bond lengths, bond angles and torsion angles, vibrational assignments and chemical shifts of the title compound have been calculated theoretically and compared with those of experimental data. Besides, molecular electrostatic potential (MEP, frontier molecular orbitals (FMOs, Mulliken population analysis, Thermodynamic properties and non-linear optical (NLO properties of the title molecule were investigated by theoretical calculations.

  10. 3-{2-[2-(2-Fluorobenzylidenehydrazinyl]-1,3-thiazol-4-yl}-2H-chromen-2-one

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    Afsheen Arshad

    2010-06-01

    Full Text Available In the title compound, C19H12FN3O2S, the chromene ring system and the thiazole ring are approximately planar [maximum deviations of 0.023 (3 Å and 0.004 (2 Å, respectively]. The chromene ring system is inclined at angles of 4.78 (10 and 26.51 (10° with respect to the thiazole and benzene rings, respectively, while the thiazole ring makes a dihedral angle of 23.07 (12° with the benzene ring. The molecular structure is stabilized by an intramolecular C—H...O hydrogen bond, which generates an S(6 ring motif. The crystal packing is consolidated by intermolecular N—H...O hydrogen bonds, which link the molecules into chains parallel to [100], and by C—H...π and π–π [centroid–centroid distance = 3.4954 (15 Å] stacking interactions.

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

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    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.

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

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    Vahid Amani

    2010-10-01

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

  13. 2-(4-Fluorophenyl-2H-chromen-4(3H-one

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    Michał Wera

    2012-02-01

    Full Text Available In the crystal structure of the title compound, C15H11FO2, molecules form inversion dimers through pairs of weak C—H...O hydrogen bonds. Dimers oriented in parallel, linked by C—H...π contacts, are arranged in columns along the b axis. The fluorophenyl ring and the benzene ring of the 2H-chromen-4(3H-one unit are inclined to one another by 70.41 (16°. They are respectively parallel in a given column or almost perpendicular [oriented at an angle of 87.8 (1°] in neighbouring (inversely oriented columns, forming a herringbone pattern.

  14. 5-(2,4-Dichlorophenoxy-3-methyl-1-phenyl-1H-pyrazole-4-carbaldehyde

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    S. Madan Kumar

    2016-07-01

    Full Text Available In the crystal structure of the title compound, C17H12Cl2N2O2, the pyrazole ring makes dihedral angles of 65.0 (2 and 43.9 (2° with the dichlorophenyl and phenyl rings, respectively. The dihedral angle between the chlorophenyl and phenyl rings is 59.1 (2°. In the crystal, the molecules are linked by C—H...O hydrogen bonds and weak C—Cl...π and C—H...π interactions, generating a three-dimensional network.

  15. Crystal and molecular structure of 2,2’-(quinoxaline-2,3-diyl)dipyridinium dinitrate (H{sub 2}L)(NO{sub 3}){sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Egorova, O. A. [People’s Friendship University of Russia (Russian Federation); Polyakova, I. N., E-mail: polyakova@igic.ras.ru; Sergienko, V. S. [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation); Davydov, V. V. [People’s Friendship University of Russia (Russian Federation)

    2016-07-15

    The crystal structure of 2,2’-(quinoxaline-2,3-diyl)dipyridinium dinitrate (H{sub 2}L)(NO{sub 3}){sub 2} is studied by X-ray diffraction (T = 150 K, R1 = 0.0467). The H{sub 2}L{sup 2+} cation is located on the twofold rotation axis and connected with two NO{sub 3}{sup −} anions by strong N–H···O hydrogen bonds. Planar quinoxaline fragments of cations form stacks with the interplanar spacing of 3.308 Å. The structure of the diprotonated H{sub 2}L{sup 2+} cation is compared with those of the monoprotonated H{sub 2}L{sup 2+} cation and neutral L molecule.

  16. Hydrates of the alkali trioxidomonosulfidomolybdates and -tungstates. K{sub 2}[(Mo/W)O{sub 3}S] . 1.5 H{sub 2}O and (Rb/Cs){sub 2}[(Mo/W)O{sub 3}S] . H{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Lehner, Anna J.; Braitsch, Milan; Roehr, Caroline [Freiburg Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie

    2012-11-01

    The trioxidomonosulfidomolybdate and -tungstate anions [(Mo/W)O{sub 3}S]{sup 2-} are the first products formed when passing H{sub 2}S gas through a solution of the oxidometalates. Their potassium, rubidium and cesium salt hydrates form as crystalline precipitates from these solutions depending on pH, the polarity of the solvent, educt concentrations and temperature. The structures of the sesqui- (K) and mono- (Rb, Cs) hydrates have been determined by means of X-ray single crystal diffraction data. The potassium sesquihydrates K{sub 2}[(Mo/W)O{sub 3}S] . 1.5 H{sub 2}O are isotypic and crystallize with a new structure type (monoclinic, space group C2/c, M = Mo/W: a = 987.0(2)/993.13(11), b = 831.75(14)/831.10(11), c = 1868.9(4)/1865.2(2) pm, {beta} = 99.34(2)/99.153(8) , R1 = 0.0352/0.0390). In the crystal structure the [(Mo/W)O{sub 3}S]{sup 2-} anions are connected via hydrogen bonds to form columns along the c direction. Channels containing only water molecules run along the [101] direction. The dehydration process proceeds in a topotactic reaction between 60 to 95 C and yields crystals of the anhydrous salts K{sub 2}[(Mo/W)O{sub 3}S]. The two different K+ cations exhibit a 5 + 3 and 5 + 2 O/S coordination. The heavier alkali metal cations form the four monohydrates (Rb/Cs){sub 2}[(Mo/W)O{sub 3}S] . H{sub 2}O (trigonal rhombohedral, space group R anti 3m) with lattice parameters for the Rb/Cs molybdates of a = 621.17(6)/624.62(10), c = 3377.9(4)/3388.6(8) pm (R1 = 0.0505/0.0734) and the tungstates of a = 642.80(3)/643.3(4), c = 3532.8(3)/3566(4) pm (R1 = 0.0348/0.0660). In the structures the 3m symmetrical tetrahedra are arranged to form double layers in such a way, that the O{sub 3} bases of the tetrahedra are pointing towards each other in a staggered conformation. These double layers are stacked in the c direction in a rhombohedral sequence. In these hydrates, there are no distinct hydrogen bonds. Instead, partially disordered pairs of H{sub 2}O molecules are

  17. (E-3-[4-(Pentyloxyphenyl]-1-phenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Asghar Abbas

    2009-06-01

    Full Text Available The title compound, C20H22O2, crystallizes with two independent molecules in the asymmetric unit. In each molecule, all the non-H atoms lie in a common plane (r.m.s. deviations of 0.098 and 0.079 Å. There is a π–π stacking interaction in the crystal structure. The central aromatic rings of the two molecules, which are stacked head-to-tail one above the other, are separated by centroid-to-centroid distances of 3.872 (13 and 3.999 (10 Å.

  18. 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.

  19. Effects of rehydration nutrients on H2S metabolism and formation of volatile sulfur compounds by the wine yeast VL3.

    Science.gov (United States)

    Winter, Gal; Henschke, Paul A; Higgins, Vincent J; Ugliano, Maurizio; Curtin, Chris D

    2011-11-02

    In winemaking, nutrient supplementation is a common practice for optimising fermentation and producing quality wine. Nutritionally suboptimal grape juices are often enriched with nutrients in order to manipulate the production of yeast aroma compounds. Nutrients are also added to active dry yeast (ADY) rehydration media to enhance subsequent fermentation performance. In this study we demonstrate that nutrient supplementation at rehydration also has a significant effect on the formation of volatile sulfur compounds during wine fermentations. The concentration of the 'fruity' aroma compounds, the polyfunctional thiols 3-mercaptohexan-1-ol (3MH) and 3-mercaptohexyl acetate (3MHA), was increased while the concentration of the 'rotten egg' aroma compound, hydrogen sulfide (H2S), was decreased. Nutrient supplementation of the rehydration media also changed the kinetics of H2S production during fermentation by advancing onset of H2S production. Microarray analysis revealed that this was not due to expression changes within the sulfate assimilation pathway, which is known to be a major contributor to H2S production. To gain insight into possible mechanisms responsible for this effect, a component of the rehydration nutrient mix, the tri-peptide glutathione (GSH) was added at rehydration and studied for its subsequent effects on H2S formation. GSH was found to be taken up during rehydration and to act as a source for H2S during the following fermentation. These findings represent a potential approach for managing sulfur aroma production through the use of rehydration nutrients.

  20. 5-(4-Fluorophenyl-2,2,6-trimethyl-4H-1,3-dioxin-4-one

    Directory of Open Access Journals (Sweden)

    Julio Zukerman-Schpector

    2009-07-01

    Full Text Available The 1,3-dioxine ring in the title compound, C13H13FO3, is in a half-boat conformation with the methyl-bonded C atom 0.612 (2 Å out of the plane defined by the remaining five atoms.

  1. (2S,4R-2-[(1R-1-(4-Bromophenyl-2-nitroethyl]-4-ethylcyclohexanone

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    Chi-Xiao Zhang

    2013-02-01

    Full Text Available The crystal structure of the title compound, C16H20BrNO3, contains three chiral centers in the configuration 1R,2S,6R. The cyclohexane ring is in a chair conformation. In the crystal, molecules are linked by weak C—H...O interactions, forming chains along the a-axis direction.

  2. Crystal structure, Hirshfeld analysis and molecular docking with the vascular endothelial growth factor receptor-2 of (3Z-5-fluoro-3-(hydroxyiminoindolin-2-one

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    Bianca Barreto Martins

    2017-07-01

    Full Text Available The reaction between 5-fluoroisatin and hydroxylamine hydrochloride in acidic ethanol yields the title compound, C8H5FN2O2, whose molecular structure matches the asymmetric unit and is nearly planar with an r.m.s. deviation for the mean plane through all non-H atoms of 0.0363 Å. In the crystal, the molecules are linked by N—H...N, N—H...O and O—H...O hydrogen-bonding interactions into a two-dimensional network along the (100 plane, forming rings with R22(8 and R12(5 graph-set motifs. The crystal packing also features weak π–π interactions along the [100] direction [centroid-to-centroid distance 3.9860 (5 Å]. Additionally, the Hirshfeld surface analysis indicates that the major contributions for the crystal structure are the O...H (28.50% and H...F (16.40% interactions. An in silico evaluation of the title compound with the vascular endothelial growth factor receptor-2 (VEGFR-2 was carried out. The title compound and the selected biological target VEGFR-2 show the N—H...O(GLU94, (CYS96N—H...O(isatine and (PHE95N—H...O(isatine intermolecular interactions, which suggests a solid theoretical structure–activity relationship.

  3. 4-{3-[Hydroxy(phenylmethyl]-5-thioxo-4,5-dihydro-1H-1,2,4-triazol-4-yl}benzenesulfonamide

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2010-04-01

    Full Text Available In the title compound, C15H14N4O3S2, the hydroxy group is disordered over two positions with occupancies of 0.619 (5 and 0.381 (5. The benzene ring attached to the heterocycle makes a dihedral angle of 86.92 (9° with respect to the best plane through the five-membered ring. The crystal packing is stabilized by intermolecular O—H...O, N—H...S, N—H...N, C—H...O and C—H...N hydrogen bonds, and N—H...π and C—H...π interactions.

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

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    Gang-Hong Pan

    2012-10-01

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

  5. Hydration reactions in pastes C3S+C3A+CaSO4.2aq+H20 at 25°C.I

    NARCIS (Netherlands)

    Corstanje, W.A.; Stein, H.N.; Stevels, J.M.

    1973-01-01

    A characteristic retardation of the hydration of C3A is found in pastes C3S+C3A+CaSO4.2aq+H2O of weight ratios 1:3:z:4 at certain values of z, when sulphate concentration becomes insufficient for monosulphate formation. This retardation is ascribed to precipitation of amorphous Al(OH)3, when C3A

  6. 5′-Methylsulfanyl-4′-oxo-7′-phenyl-3′,4′-dihydro-1′H-spiro[cyclohexane-1,2′-quinazoline]-8′-carbonitrile dimethylformamide monosolvate

    Directory of Open Access Journals (Sweden)

    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.

  7. 2-Isobutyl-6-(4-methoxyphenylimidazo[2,1-b][1,3,4]thiadiazole

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    Hoong-Kun Fun

    2011-02-01

    Full Text Available In the title compound, C15H17N3OS, the dihedral angle between the statistically planar imidazo[2,1-b][1,3,4]thiadiazole fused-ring system (r.m.s. deviation = 0.002 Å and the methyoxbenzene ring is 4.52 (6°. In the crystal, molecules are arranged into columns and stacked down the a axis. The crystal structure is stabilized by weak C—H...π and π–π interactions [centroid–centroid separations = 3.6053 (8 and 3.7088 (7 Å].

  8. Crystal structure of 1-(2,4-dimethylphenyl-2-(4-trimethylsilyl-1H-1,2,3-triazol-1-ylethanone

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    G. B. Venkatesh

    2014-12-01

    Full Text Available The asymmetric unit of the title compound, C15H21N3OSi, contains two molecules with similar conformations (r.m.s. overlay fit for the 20 non-H atoms = 0.163 Å. The dihedral angles between the planes of the 1,2,3-triazole and 2,4-dimethylbenzene rings are 27.0 (3 and 19.5 (3°. In the crystal, molecules are linked by very weak C—H...O and C—H...N hydrogen bonds to generate [100] chains. The chains are cross-linked by C—H...π interactions.

  9. {μ-2-[4-(1,3-Benzothiazol-2-ylphenyl]-2-azapropane-1,3-dithiolato-κ4S,S′:S,S′}bis[tricarbonyliron(I

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    Da-yong Jiang

    2012-03-01

    Full Text Available The title compound, [Fe2(C15H12N2S3(CO6], was prepared as an azadithiolatodiiron model for the active site of [FeFe]-hydrogenase. The Fe2S2 core adopts a butterfly shape, with each metal having a pseudo square-pyramidal geometry. The N-substituted azadithiolate is μ2-κ4S,S′:S,S′-coordinated to the Fe(CO3 moieties to form two fused six-membered rings with different conformations. The sum of the C—N—C angles around the N atom [356.85 (15°] indicates a flattening of the trigonal–pyramidal geometry about the N atom and an increase in the degree of sp2-hybridization.

  10. 5-(4-Bromophenyl-2-(3,4-methylenedioxyphenyl-3-methylsulfanyl-1-benzofuran

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    Hong Dae Choi

    2009-10-01

    Full Text Available The title compound, C22H15BrO3S, crystallizes with four molecules in the asymmetric unit. The 4-bromophenyl rings are rotated out of the benzofuran planes, with dihedral angles for the four molecules of 20.8 (2, 17.8 (2, 23.5 (4 and 23.9 (4°. The dihedral angles between the 3,4-methylenedioxyphenyl ring and the benzofuran plane are 13.5 (2, 7.1 (2, 18.6 (3 and 14.2 (3° in the four molecules. The crystal structure is stabilized by weak nonclassical intermolecular C—H...O hydrogen bonds. The crystal structure also exhibits intermolecular aromatic π–π interactions between the benzene and furan rings and between the 4-bromophenyl and 3,4-methylenedioxyphenyl rings from molecules of the same type; the centroid–centroid distances are 3.92 (1 and 3.79 (1, 3.91 (1, 3.77 (1 and 3.77 (1, and 3.79 (1 and 3.75 (1Å in the four molecules.

  11. N-(2,6-Dimethyl-3-oxo-1-thia-4-azaspiro[4.5]dec-4-yl-2-hydroxy-2,2-diphenylacetamide

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    Eser Ihan

    2008-10-01

    Full Text Available In the title compound, C24H28N2O3S, the pendant methyl C atom bonded to the cyclohexane ring is disordered over two sites in a 0.580 (11:0.420 (11 ratio. The cyclohexane ring adopts a distorted chair conformation while the thiazolidine ring has an envelope conformation. The two phenyl rings make a dihedral angle of 71.8 (2° with each other. The conformation is stabilized by an intramolecular N—H...O hydrogen bond. In the crystal structure, an intermolecular hydrogen bond O—H...O occurs.

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

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    2009-03-01

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

  13. Poly[(μ3-benzene-1,3,5-tricarboxylato-κ3O1:O3:O5(μ2-2-methylimidazolato-κ2N:N′tris(2-methylimidazole-κNdizinc(II

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    Palanikumar Maniam

    2011-06-01

    Full Text Available Hydrothermal reaction involving zinc nitrate hexahydrate, trisodium benzene-1,3,5-tricarboxylate (Na3BTC and 2-methylimidazole (2-MeImH yielded the title compound, [Zn2(C9H3O6(C4H5N2(C4H6N23]. In this mixed-ligand metal-organic compound, Zn2+ ions are coordinated by N atoms from 2-MeImH molecules and (2-MeIm− ions, as well as by O atoms from (BTC3− ions. This results in two different distorted tetrahedra, viz. ZnN3O and ZnN2O2. These tetrahedra are interconnected via (BTC3− ions and N:N′-bridging (2-MeIm− ions, thus forming a layered structure in the bc plane. Hydrogen bonds between the O atoms of carboxylate ions and NH groups of 2-MeImH ligands link the layers into a three-dimensional structure.

  14. A neodymium(III)-ammonium complex involving oxalate and carbonate ligands: (NH4)2[Nd2(C2O4)3(CO3)(H2O)].H2O.

    Science.gov (United States)

    Trombe, Jean-Christian; Galy, Jean; Enjalbert, Renée

    2002-10-01

    The title compound, diammonium aqua-mu-carbonato-tri-mu-oxalato-dineodymium(III) hydrate, (NH(4))(2)[Nd(2)(CO(3))(C(2)O(4))(3)(H(2)O)].H(2)O, involving the two ligands oxalate and carbonate, has been prepared hydrothermally as single crystals. The Nd atoms form a tetranuclear unit across the inversion centre at (1/2, 1/2, 1/2). Starting from this tetranuclear unit, the oxalate ligands serve to develop a three-dimensional network. The carbonate group acts as a bis-chelating ligand to two Nd atoms, and is monodentate to a third Nd atom. The oxalate groups are all bis-chelating. The two independent Nd atoms are ninefold coordinated and the coordination polyhedron of these atoms is a distorted monocapped antiprism.

  15. Bis[O,O′-bis(4-tert-butylphenyl dithiophosphato-κ2S,S′]bis(pyridine-κNlead(II

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    Xiulan Zhang

    2013-09-01

    Full Text Available In the title compound, [Pb(C20H26O2PS22(C5H5N2], the PbII ion is coordinated by two S,S′-bidentate anions and two pyridine molecules. The PbN2S4 coordination geometry approximates to a pentagonal bipyramid with one equatorial site vacant. The N atoms occupy the axial sites. One of the pyridine molecules is disordered over two sets of sites in a 0.907 (7:0.093 (7 ratio and one of the tert-butyl groups is disordered over two sets of sites in a 0.534 (6:0.466 (6 ratio. An intramolecular C—H...O interaction occurs in one of the ligands. In the crystal, pairs of short Pb...S contacts [3.4018 (11 Å] generate a centrosymmetric dimeric assembly with the distant S atom lying in the region of the vacant coordination site of the metal atom. No directional packing interactions occur.

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

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    Chin Hoe Teh

    2009-04-01

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

  17. (R,S)-3-Carb­oxy-2-(isoquinolinium-2-yl)propanoate monohydrate

    Science.gov (United States)

    Stilinović, Vladimir; Frkanec, Leo; Kaitner, Branko

    2010-01-01

    The title compound, C13H11NOH2O, is a monohydrate of a betaine exhibiting a positively charged N-substituted isoquino­line group and a deprotonated carboxyl group. In the crystal, mol­ecules are connected via short O—H⋯O hydrogen bonds between protonated and deprotonated carboxyl groups into chains of either R or S enanti­omers along [001]. These chains are additionally connected by hydrogen bonding between water mol­ecules and the deprotonated carb­oxy groups of neighbouring mol­ecules. PMID:21579503

  18. 2-Chloroquinazolin-4(3H-one

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    Dong-Lei Cao

    2012-06-01

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

  19. [(2S-2-(3,5-Dichloro-2-oxidobenzylideneamino-3-(4-hydroxyphenylpropionato-κ3O,N,O′](dimethylformamide-κOcopper(II

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    Hong Liang

    2008-04-01

    Full Text Available In the title complex, [Cu(C16H11Cl2NO4(C3H7NO] , the CuII atom is coordinated by two O atoms and one N atom from the tridentate ligand L2− {LH2 = (2S-[2-(3,5-dichloro-2-hydroxybenzylideneimino]-3-(4-hydroxyphenylpropionic acid} and one O atom from a dimethylformamide molecule, resulting in a slightly distorted square-planar geometry. The structure forms a one-dimensional chain through weak coordination bonds [Cu...O 3.080 (1, Cu...Cl 3.269 (1 Å] and a three-dimensional network through O—H...O and C—H...O hydrogen bonds.

  20. Assembly of bicyclic or monocyclic clusters from [(η5-C5Me5)2Mo2(μ3-S)4(CuMeCN)2]2+ with tetraphosphine or N,P mixed ligands: syntheses, structures and enhanced third-order NLO performances.

    Science.gov (United States)

    Ren, Zhi-Gang; Sun, Sha; Dai, Min; Wang, Hui-Fang; Lü, Chun-Ning; Lang, Jian-Ping; Sun, Zhen-Rong

    2011-09-07

    Reactions of the preformed cluster [(η(5)-C(5)Me(5))(2)Mo(2)(μ(3)-S)(4)Cu(2)(MeCN)(2)](ClO(4))(2) (1) with two tetraphosphine ligands, 1,4-N,N,N',N'-tetra(diphenylphosphanylmethyl)benzene diamine (dpppda) and N,N,N',N'-tetra(diphenylphosphanylmethyl)ethylene diamine (dppeda), produced two bicyclic clusters {[(η(5)-C(5)Me(5))(2)Mo(2)(μ(3)-S)(4)Cu(2)](2)(L)}(ClO(4))(4) (3: L = dpppda; 4: L = dppeda). Analogous reactions of 1 or [(η(5)-C(5)Me(5))(2)Mo(2)(μ(3)-S)(4)Cu(2)(MeCN)(2)](PF(6))(2) (2) with two N,P mixed ligands, N,N-bi(diphenylphosphanylmethyl)-2-aminopyridine (bdppmapy) and N-diphenylphosphanylmethyl-4-aminopyridine (dppmapy), afforded two monocyclic clusters {[(η(5)-C(5)Me(5))(2)Mo(2)(μ(3)-S)(4)Cu(2)](2)(L)(2)}X(4) (5: L = bdppmapy, X = ClO(4); 6: L = dppmapy, X = PF(6)). Compounds 3-6 were fully characterized by elemental analysis, IR spectra, UV-vis spectra, (1)H and (31)P{(1)H} NMR spectra, ESI-MS and single-crystal X-ray crystallography. In the tetracations of 3-6, two cubane-like [Mo(2)(μ(3)-S)(4)Cu(2)] cores are linked either by one dpppda or dppeda bridge to form a bicyclic structure or by a pair of bdppmapy or dppmapy bridges to afford a monocyclic structure. The third-order nonlinear optical (NLO) properties of 1 and 3-6 in MeCN were also investigated by femtosecond degenerate four-wave mixing (DFWM) technique with a 50 fs pulse width at 800 nm. Compounds 3-6 exhibited enhanced third-order NLO performances relative to that of 1. This journal is © The Royal Society of Chemistry 2011

  1. Crystal structure of 1,3-bis(2,3-dimethylquinoxalin-6-ylbenzene

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    Charles E. Diesendruck

    2015-12-01

    Full Text Available The title compound, C26H22N4 (I, was synthesized by C—H iridium-catalyzed borylation followed by Suzuki coupling. The molecular structure of (I consists of a central benzene ring with 3-dimethylquinoxalin-6-yl groups at the 1 and 3 positions. These 2,3-dimethylquinoxalin-6-yl groups twist significantly out of the plane of the benzene ring. There are intermolecular π–π interactions which result in a two-dimensional extended structure. The layers extend parallel to the ab plane and stack along the c axis.

  2. 2-Methyl-1,10b-dihydro-5H-pyrazolo[1,5-c][1,3]benzoxazin-5-one

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    Jan Světlík

    2009-05-01

    Full Text Available In the title compound, C11H10N2O2, a potential inhibitor of the cyclooxygenase-2 isoenzyme, the pyrazoline ring exists in a flat-envelope conformation while the puckering of the central oxazine ring is more severe. As a result, the molecule as a whole is non-planar. The formal sp3 pyrazoline N atom is sp2 hybridized, with the lone-pair electrons delocalized through conjugation with the carbonyl group rather than the double bond of the pyrazoline ring.

  3. 3-[(2,4-Dichlorophenyliminomethyl]-2-hydroxy-5-methylbenzaldehyde

    Directory of Open Access Journals (Sweden)

    Işın Kılıç

    2009-06-01

    Full Text Available The title compound, C15H11Cl2NO2, is a Schiff base which adopts the phenol–imine tautomeric form in the solid state, being stabilized by a strong intramolecular O—H...N hydrogen bond. The molecule is almost planar (r.m.s. deviation for all non-H atoms = 0.049 Å, displaying a dihedral angle of 3.1 (3° between the planes of the two aromatic rings.

  4. (E-1-(2-Aminophenyl-3-(4-chlorophenylprop-2-en-1-one

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    Rodrigo Abonia

    2016-10-01

    Full Text Available The title chalcone (E-1-(2-aminophenyl-3-(4-chlorophenylprop-2-en-1-one was prepared with an excellent yield from a Claisen–Schmidt condensation reaction between o-aminoacetophenone and p-chlorobenzaldehyde. This product will be used as a key precursor for the development of an alternative route for the total synthesis of dubamine and graveoline alkaloids. Single crystals of the title compound suitable for X-ray diffraction were grown via slow evaporation in ethanol at room temperature. A complete crystallographic study was performed in depth to unequivocally confirm its structure and determine some interesting supramolecular properties. The crystal structure of the title o-aminochalcone, C15H12ClNO, shows two molecules per asymmetric unit (Z′ = 2 and adopts an E configuration about the C=C double bond. In the title compound, the mean plane of the non-H atoms of the central chalcone fragment C—C(O—C—C—C is as follows: [r.m.s. deviation = 0.0130 Å for A-B and 0.0043 for C-D molecules]. In the crystal, molecules are linked by N—H...N and C—H...O, hydrogen bonds forming edge-fused R66(46 rings parallel to (100. Additionally, N—H...O hydrogen bonds generate a three-dimensional network.

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

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    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.

  6. 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].

  7. Indole-3-thiouronium nitrate

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    Martin Lutz

    2008-01-01

    Full Text Available In the title compound, C9H10N3S+·NO3−, the indole ring system and the thiouronium group are nearly perpendicular, with a dihedral angle of 88.62 (6°. Hydrogen bonding generates two-dimensional networks which are linked to each other via π stacking interactions of the indole groups [average inter-planar ring–ring distance of 3.449 (2 Å].

  8. (2S,4aR,6aR,7R,9S,10aS,10bR-7-Carboxy-2-(3-furyl-6a,10b-dimethyl-4,10-dioxoperhydrobenzo[f]isochromen-9-yl acetate

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The asymmetric unit of the title compound, C22H26O8, contains two crystallographically independent molecules with closely comparable conformations (r.m.s. overlay = 0.54 Å for 30 non-H atoms. All six-membered rings display chair conformations, with a slight distortion for the lactone ring. The molecules are connected by O—H...O hydrogen bonds into chains along [010], with the independent molecules segregated into separate chains. The two molecules in the asymmetric unit face each other in a head-to-tail fashion, with the furan ring of one molecule turned towards the carboxylic acid terminal of the other molecule.

  9. Crystal structure of 1-[(6-chloropyridin-3-ylsulfonyl]-1,2,3,4-tetrahydroquinoline

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    S. Jeyaseelan

    2015-06-01

    Full Text Available The tetrahydropyridine ring of the quinoline system in the title compound, C14H13ClN2O2S, adopts a half-chair conformation with the bond-angle sum at the N atom being 350.0°. The dihedral angle between the least-squares planes of the two aromatic rings is 50.13 (11°. In the crystal, inversion dimers linked by pairs of C—H...O hydrogen bonds generate R22(10 loops. Additional intermolecular C—H...O hydrogen bonds generate C(7 chains along [100].

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

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    Alain Igau

    2013-12-01

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

  11. Synthesis, crystal structure, thermal analysis and dielectric properties of [(C{sub 4}H{sub 9}){sub 4}N]{sub 3}Bi{sub 2}Cl{sub 9} compound

    Energy Technology Data Exchange (ETDEWEB)

    Trigui, W., E-mail: walatrigui@yahoo.fr; Oueslati, A.; Chaabane, I.; Hlel, F.

    2015-07-15

    A new organic–inorganic tri-tetrabutylammonium nonachlorobibismuthate(III) compound was prepared. It was found to crystallize in the monoclinic system (P2{sub 1}/n space group) with the following lattice parameters: a=11.32(2) Å, b=22.30(3) Å, c=28.53(2) Å and β=96.52(0)°. The [Bi{sub 2}Cl{sub 9}]{sup 3−} anions are surrounded by six [(C{sub 4}H{sub 9})N]{sup +} cations, forming an octahedral configuration. These octahedra are sharing corners in order to provide the tri-dimensional network cohesion. The differential scanning calorimetry reveals four order-disorder reversible phase transitions located at 214, 238, 434 and 477 K. The Raman and infrared spectra confirm the presence of both cationic [(C{sub 4}H{sub 9})N]{sup +} and anionic [Bi{sub 2}Cl{sub 9}]{sup 3−} parts. The dielectric parameters, real and imaginary dielectric permittivity (ε′ and ε″), and dielectric loss tangent (tg δ), were measured in the frequency range of 209 kHz–5 MHz at different temperatures. The variations of dielectric dispersion (ε') and dielectric absorption (ε″) with frequency show a distribution of relaxation times, which is probably related to the change in the dynamical state of the [(C{sub 4}H{sub 9}){sub 4}N]{sup +} cations and the [Bi{sub 2}Cl{sub 9}]{sup 3−} anions. - Graphical abstract: Projection of the atomic arrangement of the [(C{sub 4}H{sub 9}){sub 4}N]{sub 3}Bi{sub 2}Cl{sub 9} compound along the b axis. - Highlights: • The structure of the (TBA){sub 3}Bi{sub 2}Cl{sub 9} compound was solved and reported. • The cristal belongs to the monoclinic system with P2{sub 1}/n space group. • DSC discloses four order–disorder reversible phases transitions. • The temperature-dependent permittivity ε' and ε″ has been investigated.

  12. 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.

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  14. Identification of solution products of lanthanoid (3) diethyldithiocarbamatohexamethyl phosphotriamide compounds from IR, electron and sup 1 H, sup 13 C, sup 31 P NMR absorption spectra. Identifikatsiya produktov rastvoreniya diehtilditiokarbamatogeksametil fosfotriamidnykh soedinenij lantanoidov (3) po IK, ehlektronnym i YaMR sup 1 H, sup 13 C, sup 31 P spektram pogloshcheniya

    Energy Technology Data Exchange (ETDEWEB)

    Skopenko, V V; Savost' yanova, A F; Trachevskij, V V; Gorbalyuk, A D; Sukhan, T A [Kievskij Gosudarstvennyj Univ., Kiev (Ukrainian SSR)

    1991-01-01

    By the methods of conductometry, IR, electron and {sup 1}H, {sup 13}C, {sup 31}P NMR spectroscopy nonaqueous solutions of the compounds (La(S{sub 2}CNEt{sub 2})Hmpa{sub 5})(BPh{sub 4}){sub 2}, Hmpa=OP(NMe{sub 2}){sub 3}; (Ln(S{sub 2}CNEt{sub 2}){sub 2}Hmpa{sub 3})BPh{sub 4}, Ln=Y, La-Lu; (Ln(S{sub 2}CNEt{sub 2}){sub 3}Hmpa{sub 2}), Ln=La-Gd, have been investigated. It is ascertained that bis-dithiocarbamate compounds are dissolved in all the studied solvents with preservation of composition and structure of lanthanide (3) inner coordination sphere. Tris-dithiocarbamates in nonaqueous solutions are subjected to reactions of ligand redistribution according to schemes depending on the solvent nature. In the process of dissolving of lanthanum monodithiocarbamate bond isomerization of dithiocarbamate groups occurs, which is pronounced in splitting of {sup 1}H and {sup 13}C NMR signals.

  15. 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

  16. Synthesis and fundamental properties of stable Ph(3)SnSiH(3) and Ph(3)SnGeH(3) hydrides: model compounds for the design of Si-Ge-Sn photonic alloys.

    Science.gov (United States)

    Tice, Jesse B; Chizmeshya, Andrew V G; Groy, Thomas L; Kouvetakis, John

    2009-07-06

    The compounds Ph(3)SnSiH(3) and Ph(3)SnGeH(3) (Ph = C(6)H(5)) have been synthesized as colorless solids containing Sn-MH(3) (M = Si, Ge) moieties that are stable in air despite the presence of multiple and highly reactive Si-H and Ge-H bonds. These molecules are of interest since they represent potential model compounds for the design of new classes of IR semiconductors in the Si-Ge-Sn system. Their unexpected stability and high solubility also makes them a safe, convenient, and potentially useful delivery source of -SiH(3) and -GeH(3) ligands in molecular synthesis. The structure and composition of both compounds has been determined by chemical analysis and a range of spectroscopic methods including multinuclear NMR. Single crystal X-ray structures were determined and indicated that both compounds condense in a Z = 2 triclinic (P1) space group with lattice parameters (a = 9.7754(4) A, b = 9.8008(4) A, c = 10.4093(5) A, alpha = 73.35(10)(o), beta = 65.39(10)(o), gamma = 73.18(10)(o)) for Ph(3)SnSiH(3) and (a = 9.7927(2) A, b = 9.8005(2) A, c = 10.4224(2) A, alpha = 74.01(3)(o), beta = 65.48(3)(o), gamma = 73.43(3)(o)) for Ph(3)SnGeH(3). First principles density functional theory simulations are used to corroborate the molecular structures of Ph(3)SnSiH(3) and Ph(3)SnGeH(3), gain valuable insight into the relative stability of the two compounds, and provide correlations between the Si-Sn and Ge-Sn bonds in the molecules and those in tetrahedral Si-Ge-Sn solids.

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

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    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. Different Dimensional and Structural Variations in Coordination Compounds of Cadmium, Manganese and Nickel Constructed from the Ligand 2,2'-Bipyidine-3,3',6,6'-tetracarboxylic Acid (H{sub 4}bptc)

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, Jing; Yang, Tiantian; Fu, Lulu; Luo, Ya; Wu, Jiashou [Yangtze Univ., Jingzhou (China)

    2013-09-15

    The reactions of hydrated CdCl{sub 2}, MnCl{sub 2}, and NiCl{sub 2} with 2,2'-bipyidine-3,3',6,6'-tetracarboxylic acid (H{sub 4}bptc) afforded the mononuclear [Cd{sup II}(H{sub 2}bptc)(H{sub 2}O){sub 3}]·H{sub 2}O (1), linear [Cd(H{sub 2}bptc)(H{sub 2}O)]·3H{sub 2}O{sub n} (2), 3-D hetero-bimetallic [NaCd(Hbptc)(H{sub 2}O)] (3), layer [Mn(H{sub 2}bptc)(H{sub 2}O)]n (4) and a dinuclear compound [Ni{sub 2}(H{sub 2}bptc)-(H{sub 2}O){sub 2}]·6H{sub 2}O (5). These compounds have been characterized by elemental analysis, IR, and their structures have been determined by X-ray crystallography. The thermal stabilities of 1-3 were measured by thermogravimetric analysis (TGA) and their solid state luminescence properties together with the free ligand H{sub 4}bptc were investigated at room temperature.

  19. Synthesis and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).

    Science.gov (United States)

    Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B

    2016-08-01

    Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms.

  20. Study of interaction in the Pb(NO3)2-Cs3[Fe(CN)6]-H2O at 25 deg C

    International Nuclear Information System (INIS)

    Slivko, T.A.; Stepina, S.B.; Poletaev, I.F.; Golikova, N.B.

    1982-01-01

    The method of ''residual concentrations'' has been used to study the interaction in the lead nitrate-cesium hexacyanoferrate (3)-water system at 25 deg C. It is shown, that only one compound CsPb[Fe(CN) 6 ]x4H 2 O is formed in the studied range of the concentrations. Chemical and thermogravimetric analysis and infrared spectroscopy have been used at the determination of the compound composition. Thermolysis of the compound in the air is studied. Identification of the hydrated and waterless compound is accomplished with the help of the diffractometer DRON-1. The rate of the formation of mixed cesium hexacyanoferrates (3) with lead, zinc and nickel is compared

  1. 3-Chloro-2-ethyl-6-nitro-2H-indazole

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    Mohamed Mokhtar Mohamed Abdelahi

    2017-05-01

    Full Text Available In the title compound, C9H8ClN3O2, the orientation of the ethyl substituent is partly determined by an intramolecular C—H...Cl hydrogen bond. The indazole moiety is slightly folded with an angle of 0.70 (8° between the five- and six-membered rings. In the crystal, molecules pack in layers parallel to [100] through C—H...π(ring and N...;O...π(ring interactions.

  2. The structural, microhardness and thermal properties of a semiorganic NLO crystal: Lithium paranitrophenolate trihydrate (NO2-C6H4-OLi.3H2O)

    International Nuclear Information System (INIS)

    Boaz, B. Milton; Raman, P. Santhana; Raja, S. Xavier Jesu; Das, S. Jerome

    2005-01-01

    The crystallographic parameters, morphology, microhardness anisotropy and thermal properties including differential thermal analysis (DTA), thermo gravimetric analysis (TGA) of a new nonlinear optical material lithium paranitrophenolate trihydrate (NPLi.3H 2 O) are reported. The single crystals of NPLi.3H 2 O show effective phase matchable second harmonic generation properties for frequency conversion. Optically clear single crystals having dimensions up to 12 mm x 8 mm x 4 mm have been grown successfully within a period of 60 days by isothermal solvent evaporation technique. The title compound crystallizes in monoclinic system with space group Pa. Microhardness measurement on different planes verifies the hardness anisotropy and thermal studies reveal good thermal stability of the material. The NLO property of the crystal is verified by employing Kurtz powder test. The crystal has a wide range of optical transparency from 400 nm to 1500 nm

  3. Ethyl 3-[(3,5-dimethylphenylaminocarbonyl]propanoate

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    B. Thimme Gowda

    2009-08-01

    Full Text Available The non-H atoms in the title compound, C14H19NO3, lie on a mirror plane. The amide O and ester carbonyl O atoms are trans to each other. Furthermore, the C=O and O—CH2 bonds of the ester group are syn with respect to each other. In the crystal, molecules are packed into centrosymmetric dimers through intermolecular N—H...O hydrogen bonds.

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

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    Rainer Beckert

    2013-12-01

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

  5. 1-Decyl-6-nitro-1H-benzimidazol-2(3H-one

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    Younes Ouzidan

    2011-11-01

    Full Text Available The title molecule, C17H25N3O3, is built up from fused six- and five-membered rings linked to a –C10H21 chain. The fused-ring system is essentially planar, the largest deviation from the mean plane being 0.009 (2 Å. The chain is roughly perpendicular to this plane, making a dihedral angle of 79.5 (2°. In the crystal, N—H...O hydrogen bonds build infinite chains along [010]. There are channels in the structure containing disordered hexane. The contribution of this solvent to the scattering power was suppressed using the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  6. (E-3-Propoxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one monohydrate

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    Burkhon Zh Elmuradov

    2010-05-01

    Full Text Available The title compound, C15H16N2O2·H2O, was synthesized via the alkylation of 3-hydroxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one with n-propyl iodide in the presence of sodium hydroxide. The organic molecule and the water molecule both lie on a crystallographic mirror plane. In the crystal structure, intermolecular O—H...O and O—H...N hydrogen bonds link the components into extended chains along [100].

  7. 2-[(2,4,4,6,6-Pentachloro-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinin-2-ylazanidyl]pyridinium

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    Safaa A. Ahmed

    2012-02-01

    Full Text Available The title compound, C5H5Cl5N5P3, crystallizes as a zwitterion in which the pyridine N atom is protonated. An S(6 ring motif is formed via an intramolecular C—H...N hydrogen bond. The triazatriphosphinine ring adopts an envelope conformation, with one N atom displaced by 0.145 (1 Å from the other atoms. In the crystal, N—H...N and C—H...N hydrogen bonds link the molecules into centrosymmetric dimers containing one R22(7 ring motif and two R22(8 ring motifs.

  8. Pharmacophore-based screening of differentially-expressed PGF, DDIT4, COMP and CHI3L1 from hMSC cell lines reveals five novel therapeutic compounds for primary osteoporosis

    Directory of Open Access Journals (Sweden)

    Catherine Jessica Lai

    2016-06-01

    Full Text Available As many societies age, primary osteoporosis (PO is increasingly a major health problem. Current drug treatments such as alendronate and risedronate have known side effects. We took an agnostic empirical approach to find PO therapeutic compounds. We examined 13,548,960 probe data-points from mesenchymal stromal cell (hMSC lines and found that PGF, DDIT4, and COMP to be up-regulated, and CHI3L1, down-regulated. We then identified their druggable domains. For the up-regulated differentially-expressed genes, we used protein–protein interactions to find residue clusters as binding surfaces. We then employed pharmacophore models to screen 15,407,096 conformations of 22,723,923 compounds, which identified (6R,9R-6-(2-furyl-9-(1H-indol-3-yl-2-(trifluoromethyl-5,6,7, 9-tetrahydro-4H[1,2,4]triazolo[5,1],(2S-N1-[2-[2-(methylamino-2-oxo-ethyl]phenyl]-N2-phenylpyrrolidine-1,2-dicarboxamide, and 2-furyl-(1H-indol-3-yl-methyl-BLAHone as candidate compounds. For the down-regulated CH13L1, we relied on genome-wide disease signatures to identify (11alpha-9-fluoro-11,17,21-trihydroxypregn-4-ene-3,20-dione and Genistein as candidate compounds. Our approach differs from previous research as we did not confine our drug targets to hypothesized compounds in the existing literature. Instead, we allowed the full expression profile of PO cell lines to reveal the most desirable targets. Second, our differential gene analysis revealed both up- and down-regulated genes, in contrast to the literature, which has focused on inhibiting only up-regulated genes. Third, our virtual screening universe of 22,723,923 compounds was more than 100 times larger than those in the known literature.

  9. Poly[propane-1,3-diammonium [cuprate(II-bis(μ2-pyridine-2,3-dicarboxylato] trihydrate

    Directory of Open Access Journals (Sweden)

    Shabnam Hooshmand

    2008-02-01

    Full Text Available The title polymeric compound {(C3H12N2[Cu(C7H3NO42]·3H2O}n or {(pnH2[Cu(py-2,3-dc2]·3H2O}n (pn is propane-1,3-diamine and py-2,3-dcH2 is pyridine-2,3-dicarboxylic acid, was synthesized by reaction of copper(II chloride dihydrate with a proton-transfer compound, propane-1,3-diammonium pyridine-2,3-dicarboxylate or (pnH2(py-2,3-dc, in aqueous solution. The anion is a six-coordinate complex (site symmetry overline{1}, with a distorted octahedral geometry around CuII, consisting of two bidentate pyridine-2,3-dicarboxylate groups and two O atoms of bridging ligands from (py-2,3-dc2− fragments, which are located in trans positions. The (pnH22+ cation is disordered over two sites by the center of inversion. Intermolecular hydrogen bonds, π–π [centroid–centroid distances of 3.539 (3 Å] and C—O...π stacking interactions [O...Cg = 3.240 (5 Å; Cg is the center of the pyridine ring], connect the various components into a supramolecular structure.

  10. Crystal structure of diaphorin methanol monosolvate isolated from Diaphorina citri Kuwayama, the insect vector of citrus greening disease

    Directory of Open Access Journals (Sweden)

    D. Marian Szebenyi

    2018-04-01

    Full Text Available The title compound C22H39NO9·CH3OH [systematic name: (S-N-((S-{(2S,4R,6R-6-[(S-2,3-dihydroxypropyl]-4-hydroxy-5,5-dimethyltetrahydro-2H-pyran-2-yl}(hydroxymethyl-2-hydroxy-2-[(2R,5R,6R-2-methoxy-5,6-dimethyl-4-methylenetetrahydro-2H-pyran-2-yl]acetamide methanol monosolvate], was isolated from the Asian citrus psyllid, Diaphorina citri Kuwayama, and crystallizes in the space group P21. `Candidatus Profftella armatura' a bacterial endosymbiont of D. citri, biosynthesizes diaphorin, which is a hybrid polyketide–nonribosomal peptide comprising two highly substituted tetrahydropyran rings joined by an N-acyl aminal bridge [Nakabachi et al. (2013. Curr. Biol. 23, 1478–1484]. The crystal structure of the title compound establishes the complete relative configuration of diaphorin, which agrees at all nine chiral centers with the structure of the methanol monosolvate of the di-p-bromobenzoate derivative of pederin, a biogenically related compound whose crystal structure was reported previously [Furusaki et al. (1968. Tetrahedron Lett. 9, 6301–6304]. Thus, the absolute configuration of diaphorin is proposed by analogy to that of pederin.

  11. (4′-Phenyl-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′bis(thiocyanato-κNzinc(II unknown solvate

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    An-ran Wang

    2016-11-01

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

  12. (E)-3-[4-(Pent-yloxy)phen-yl]-1-phenyl-prop-2-en-1-one.

    Science.gov (United States)

    Abbas, Asghar; Khawar Rauf, M; Bolte, Michael; Hasan, Aurangzeb

    2009-05-14

    The title compound, C(20)H(22)O(2), crystallizes with two independent mol-ecules in the asymmetric unit. In each mol-ecule, all the non-H atoms lie in a common plane (r.m.s. deviations of 0.098 and 0.079 Å). There is a π-π stacking inter-action in the crystal structure. The central aromatic rings of the two mol-ecules, which are stacked head-to-tail one above the other, are separated by centroid-to-centroid distances of 3.872 (13) and 3.999 (10) Å.

  13. 2,4-Bis(4-fluorophenyl-1,5-dimethyl-3-azabicyclo[3.3.1]nonan-9-one

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    S. Rizwana Begum

    2013-10-01

    Full Text Available The asymmetric unit of the title compound, C22H23F2NO, contains two independent molecules, A and B. The bicyclic system adopts a twin-chair conformation in both molecules. The dihedral angles between the fluorophenyl rings are 55.27 (8 and 56.37 (7° in molecules A and B, respectively. The NH groups are not involved in hydrogen bonding due to the steric hindrance of fluorophenyl groups. The crystal structure features weak C—H...O interactions.

  14. Synthesis, X-ray Single Crystal Structure, Molecular Docking and DFT Computations on N-[(1E)-1-(2H-1,3-Benzodioxol-5-yl)-3-(1H-imidazol-1-yl)propylidene]-hydroxylamine: A New Potential Antifungal Agent Precursor.

    Science.gov (United States)

    Al-Wabli, Reem I; Al-Ghamdi, Alwah R; Ghabbour, Hazem A; Al-Agamy, Mohamed H; Monicka, James Clemy; Joe, Issac Hubert; Attia, Mohamed I

    2017-02-28

    Mycoses are serious health problem, especially in immunocompromised individuals. A new imidazole-bearing compound containing an oxime functionality was synthesized and characterized with different spectroscopic techniques to be used for the preparation of new antifungal agents. The stereochemistry of the oxime double bond was unequivocally determined via the single crystal X-ray technique. The title compound 4 , C 13 H 13 N₃O₃·C₃H₈O, crystallizes in the monoclinic space group P 2₁with a = 9.0963(3) Å, b = 14.7244(6) Å, c = 10.7035(4) Å, β = 94.298 (3)°, V = 1429.57(9) ų, Z = 2. The molecules were packed in the crystal structure by eight intermolecular hydrogen bond interactions. A comprehensive spectral analysis of the title molecule 4 has been performed based on the scaled quantum mechanical (SQM) force field obtained by density-functional theory (DFT) calculations. A molecular docking study illustrated the binding mode of the title compound 4 into its target protein. The preliminary antifungal activity of the title compound 4 was determined using a broth microdilution assay.

  15. Structural, Spectroscopic (FT-IR, Raman and NMR, Non-linear Optical (NLO, HOMO-LUMO and Theoretical (DFT/CAM-B3LYP Analyses of N-Benzyloxycarbonyloxy-5-Norbornene-2,3-Dicarboximide Molecule

    Directory of Open Access Journals (Sweden)

    Nuri ÖZTÜRK

    2018-02-01

    Full Text Available The experimental spectroscopic investigation of N-benzyloxycarbonyloxy-5-norbornene-2,3-dicarboximide (C17H15NO5 molecule has been done using 1H and 13C NMR chemical shifts, FT-IR and Raman spectroscopies. Conformational forms have been determined depending on orientation of N-benzyloxycarbonyloxy and 5-norbornene-2,3-dicarboximide (NDI groups of the title compound. The structural geometric optimizations, vibrational wavenumbers, NMR chemical shifts (in vacuum and chloroform and HOMO-LUMO analyses for all conformers of the title molecule have been done with DFT/CAM-B3LYP method at the 6-311++G(d,p basis set. Additionally, based on the calculated HOMO and LUMO energy values, some molecular properties such as ionization potential (I, electron affinity (A, electronegativity (χ, chemical hardness (h, chemical softness (z, chemical potential (μ and electrophilicity index (w parameters are determined for all conformers. The non-linear optical (NLO properties have been studied for the title molecule. We can say that the experimental spectral data are in accordance with calculated values.

  16. 2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate

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    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.

  17. 3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H)-thione.

    Science.gov (United States)

    Karczmarzyk, Zbigniew; Pitucha, Monika; Wysocki, Waldemar; Pachuta-Stec, Anna; Stańczuk, Andrzej

    2013-02-01

    The title compound, C(11)H(13)N(3)S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2):0.23 (2) for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3) Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18) and 86.56 (49)° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15)° and this conformation is stabilized by an intra-molecular C-H⋯S contact. In the crystal, pairs of N-H⋯S hydrogen bonds link mol-ecules into inversion dimers. π-π inter-actions are observed between the triazole and benzene rings, with centroid-centroid separations of 3.547 (4) and 3.544 (12) Å for components A and B, and slippages of 0.49 (6) and 0.58 (15) Å, respectively.

  18. Synthesis of 14C-labeled 3-{[1-ethoxycarbonyl-3-phenyl-(1S)-propyl]amino}-2,3,4,5-tetrahydro-2-oxo -1H-1-(3S)-benzazepine-1-acetic acid hydrochloride ([14C]CGS 14824A)

    International Nuclear Information System (INIS)

    Chaudhuri, N.K.; Patera, R.; Markus, B.; Mingsang Sung

    1987-01-01

    The title compound, CGS 14824A, was synthesized with a 14 C-label in the azepine ring in 14 steps starting with 1-bromo-3-phenylpropane (1) and K 14 CN in an overall yield of 1.31%. The reaction of 1 with K 14 CN yielded the nitrile 2 which upon hydrolysis followed by ring closure gave α-tetralone-1- 14 C (4). Bromination of 4 followed by oxime formation gave the bromo oxime 5, which upon Beckmann rearrangement by acid treatment yielded the ring expansion product 6. The bromine atom of 6 was then replaced by an azido group, and an acetic ester side chain was introduced at the nitrogen atom. Catalytic reduction of the azido compound 8 gave a mixture of epimeric amino esters which was resolved by salt formation with L-tartaric acid. The negatively rotating isomer was then reacted with 4-phenyl-2-oxo-butanoate in presence of sodium cyanoborohydride to give a mixture of diastereoisomers which were separated as their benzyl esters by chromatography. The major isomer was then converted to labeled CGS 14824A. (author)

  19. Vibrational spectroscopic (FT-IR, FT-Raman) and quantum mechanical study of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a][1,4] diazepine

    Science.gov (United States)

    Kuruvilla, Tintu K.; Prasana, Johanan Christian; Muthu, S.; George, Jacob

    2018-04-01

    The spectroscopic properties of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine were investigated in the present study using FT-IR and FT-Raman techniques. The results obtained were compared with quantum mechanical methods, as it serves as an important tool in interpreting and predicting vibrational spectra. The optimized molecular geometry, the vibrational wavenumbers, the infrared intensities and Raman scattering were calculated using density functional theory B3LYP method with 6-311++g (d,p) basis set. All the experimental results were in line with the theoretical data. The molecular electrostatic potential (MEP) and HOMO LUMO energies of the title compound were accounted. The results indicated that the title compound has a lower softness value (0.27) and high electrophilicity index (4.98) hence describing its biological activity. Further, natural bond orbital was also analyzed as part of the work. Fukui functions were calculated in order to explain the chemical selectivity or the reactivity site in 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine. The thermodynamic properties of the title compound were closely examined at different temperatures. It revealed the correlations between heat capacity (C), entropy (S) and enthalpy changes (H) with temperatures. The paper further explains that the title compound can act as good antidepressant through molecular docking studies.

  20. 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].