(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.

(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.

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.

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.

(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.

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

Science.gov (United States)

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

2017-09-01

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

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

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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].

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.

[2,3,7,8,13,14,17,18-Octakis(ethylsulfanyl-5,10,15,20-porphyrazinato]zinc(II

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Mehmet Akkurt

2010-08-01

Full Text Available In the title compound, [Zn(C32H40N8S8], the ZnII ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn...S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the ZnII ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10:0.159 (10, 0.802 (10:0.198 (10 and 0.457 (13:0.543 (13. Weak intramolecular C—H...N and C—H...S interactions contribute to the stability of the molecular conformation. Intermolecular C—H...S contacts, weak C—H...π interactions and π–π stacking interactions [centroid–centriod distances = 3.832 (4 and 3.850 (5 Å] contribute to the stabilization of the crystal structure.

Rietveld refinement of the structures of 1.0 C-S-H and 1.5 C-S-H

KAUST Repository

Battocchio, Francesco

2012-11-01

Low-Q region Rietveld analyses were performed on C-S-H synchrotron XRD patterns, using the software MAUD. Two different crystal structures of tobermorite 11 Å were used as a starting model: monoclinic ordered Merlino tobermorite, and orthorhombic disordered Hamid tobermorite. Structural modifications were required to adapt the structures to the chemical composition and the different interlayer spacing of the C-S-H samples. Refinement of atomic positions was done by using special constraints called fragments that maintain interatomic distances and orientations within atomic polyhedra. Anisotropic crystallite size refinement showed that C-S-H has a nanocrystalline disordered structure with a preferred direction of elongation of the nanocrystallites in the plane of the Ca interlayer. The quality of the fit showed that the monoclinic structure gives a more adequate representation of C-S-H, whereas the disordered orthorhombic structure can be considered a more realistic model if the lack of long-range order of the silica chain along the c-direction is assumed. © 2012 Elsevier Ltd. All rights reserved.

Resorcinol ninhydrin complex: 1,5,9-trihydroxy-8-oxatetracyclo[7.7.0.02,7.010,15]hexadeca-2,4,6,10(15,11,13-hexaen-16-one

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B. Sridhar

2012-05-01

Full Text Available In the title compound, C15H10O5, the cyclopentanone (r.m.s. deviation = 0.049 Å and oxolane (r.m.s. deviation = 0.048 Å rings make a dihedral angle of 67.91 (4°. An intramolecular O—H...O hydrogen bond is observed. In the crystal, molecules associate via O—H...O hydrogen bonds, forming a three-dimensional network.

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) ųof 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) ųof compound (2). Structural analyses reveal that the title compounds are isostructural.

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.

(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.

Bis(2-methyl-1H-imidazol-3-ium naphthalene-1,5-disulfonate dihydrate

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Yu-feng Wang

2012-06-01

Full Text Available The asymmetric unit of the title organic salt, 2C4H7N2+·C10H6O6S22−·2H2O, consists of a 2-methylimidazolium cation, a half of a naphthalene-1,5-disulfonate anion, which lies about a center of symmetry, and a water molecule. In the crystal, N—H...O and O—H...O hydrogen bonds link the cations, anions and water molecules into the layers parallel to (111.

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.

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

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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.

(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.

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.

Anastomose arterial com fio de polidioxanona e fio de polipropileno. Estudo comparativo em cães Arterial anastomose with polydioxanone and polypropilene suture. Comparative study in dogs

OpenAIRE

Eloísa de Brida Tormena; Carlos Edmundo Rodrigues Fontes; César Orlando Peralta Bandeira; Amaury José Teixeira Nigro; Marcos Victor Ferreira; Lia Yoneka Toda; Fabiana de Cássia Merenda

2002-01-01

Este estudo teve por objetivo comparar os efeitos do fio absorvível de polidioxanona com o fio inabsorvível de polipropileno, em anastomoses término-terminais, em artérias femorais de cães. Foram utilizados 20 cães, separados em dois grupos, para observação no 7º e no 30º dia de pós-operatório. Cada cão teve suas artérias femorais seccionadas e aproximadas em um lado com pontos separados de fio de polidioxanona 6-0, e no lado contralateral com o fio de polipropileno 6-0. A escolha do fio foi ...

(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

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-03-15

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

[2,3,7,8,13,14,17,18-Octa-kis(ethyl-sulfan-yl)-5,10,15,20-porphyrazinato]zinc(II).

Science.gov (United States)

Akkurt, Mehmet; Coşkun, Naciye Yılmaz; Kılıçaslan, Fatma Aytan; Yalçın, Sabiha Manav; Büyükgüngör, Orhan; Gül, Ahmet

2010-07-24

In the title compound, [Zn(C(32)H(40)N(8)S(8))], the Zn(II) ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn⋯S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the Zn(II) ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10):0.159 (10), 0.802 (10):0.198 (10) and 0.457 (13):0.543 (13). Weak intra-molecular C-H⋯N and C-H⋯S inter-actions contribute to the stability of the mol-ecular conformation. Inter-molecular C-H⋯S contacts, weak C-H⋯π inter-actions and π-π stacking inter-actions [centroid-centriod distances = 3.832 (4) and 3.850 (5) Å] contribute to the stabilization of the crystal structure.

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

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Tuncer Hökelek

2009-07-01

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

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.

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 Csp3—H...Cl hydrogen bonds, H...S contacts and π–π stacking interactions between phenothiazine units.

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.

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.

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.

15-00368_SI_NP.docx

Indian Academy of Sciences (India)

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Figure S1. The correlation graphs between calculated and observed geometrical parameters of the studied compound. Figure S2. 1H NMR of the title compound. Figure S3. 13C NMR of the title compound. Figure S4. IR of the title compound. Table S1. Hydrogen bonding information (Å, °) of the title compound. Table S2.

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

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].

Rietveld refinement of the structures of 1.0 C-S-H and 1.5 C-S-H

KAUST Repository

Battocchio, Francesco; Monteiro, Paulo J.M.; Wenk, Hans-Rudolf

2012-01-01

Low-Q region Rietveld analyses were performed on C-S-H synchrotron XRD patterns, using the software MAUD. Two different crystal structures of tobermorite 11 Å were used as a starting model: monoclinic ordered Merlino tobermorite, and orthorhombic

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

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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].

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

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Augusto Rivera

2012-10-01

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

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-(Prop-2-ynyl-10H-phenothiazine

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Younas Aouine

2010-11-01

Full Text Available In the molecule of the title compound, C15H11NS, the butterfly angle between the two planes defined by the two wings of the phenothiazine unit is 33.5 (8°. The dihedral angles between the two benzene rings and the propynyl group are 85 (4 and 63 (4°.

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].

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.

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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}].

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

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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.

(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.

(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°.

[2,3,7,8,13,14,17,18-Octa?kis(ethyl?sulfan?yl)-5,10,15,20-porphyrazinato]zinc(II)

OpenAIRE

Akkurt, Mehmet; Co?kun, Naciye Y?lmaz; K?l??aslan, Fatma Aytan; Yal??n, Sabiha Manav; B?y?kg?ng?r, Orhan; G?l, Ahmet

2010-01-01

In the title compound, [Zn(C32H40N8S8)], the ZnII ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn...S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the ZnII ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10):0.159 (10), 0.802 (10):0.198 (10) and 0.457 (...

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

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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%.

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.

Hexaaquamagnesium(II bis(d-camphor-10-sulfonate

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Dejan Jeremić

2008-07-01

Full Text Available The structure of the title complex, [Mg(H2O6](C10H15O4S2, consists of regular octahedral [Mg(H2O6]2+ cations and d-camphor-10-sulfonate anions. A three-dimensional supramolecular architecture is formed via hydrogen-bond interactions [O—H...O = 2.723 (2–2.833 (2 Å] to give alternating layers of [Mg(H2O6]2+ cations and d-camphor-10-sulfonate anions. The title compound is isomorphous with the zinc, copper, cadmium and nickel analogues.

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.

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...

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.

Anastomose arterial com fio de polidioxanona e fio de polipropileno. Estudo comparativo em cães Arterial anastomose with polydioxanone and polypropilene suture. Comparative study in dogs

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Eloísa de Brida Tormena

2002-03-01

Full Text Available Este estudo teve por objetivo comparar os efeitos do fio absorvível de polidioxanona com o fio inabsorvível de polipropileno, em anastomoses término-terminais, em artérias femorais de cães. Foram utilizados 20 cães, separados em dois grupos, para observação no 7º e no 30º dia de pós-operatório. Cada cão teve suas artérias femorais seccionadas e aproximadas em um lado com pontos separados de fio de polidioxanona 6-0, e no lado contralateral com o fio de polipropileno 6-0. A escolha do fio foi feita por sorteio, totalizando 40 anastomoses. Para análise estatística dos resultados aplicaram-se os testes de Fisher, Mac Nemar, Wilcoxon, Mann-Witney e o teste T de Student (a ≤ 0,05. Nas avaliações clínicas não foram observadas diferenças significantes entre os fios utilizados. Os resultados obtidos nas avaliações arteriográfica e macroscópica dos segmentos arteriais foram semelhantes, assim como na análise histológica morfológica. Na análise histológica morfométrica o fio de polipropileno apresentou número de células gigantes de corpo estranho significativamente maior que o fio de polidioxanona aos 7 e 30 dias de pós-operatório. Os resultados nos permitem concluir que, apesar da maior reação de corpo estranho observada com o fio de polipropileno, o fio de polidioxanona apresentou resultados semelhantes ao fio de polipropileno, em anastomoses arteriais em cães.The objetive of this study was to compare the effects of the absorbable polidioxanone suture to the nonabsorbable polypropylene suture, in end-to-end anastomoses, using dog’s femoral arteries. Twenty dogs were separated in two groups for observation on the 7th and 30th post-operatory day. Each dog had its femoral arteries seccioned and then aproximated one side with separate stitches of polidioxanone 6-0 suture, and the other side with polypropylene 6-0 suture. For the statistical studies Fisher, Mac nemar, Wilsoxon, Mann-Witney and T of Student tests (a �

Syntheses, crystal structures, and properties of the isotypic pair [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O

Energy Technology Data Exchange (ETDEWEB)

Van, Nguyen-Duc; Kleeberg, Fabian M.; Schleid, Thomas [Institut fuer Anorganische Chemie, Universitaet Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart (Germany)

2015-11-15

Single crystals of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O were obtained by reactions of aqueous solutions of the acid (H{sub 3}O){sub 2}[B{sub 12}H{sub 12}] with chromium(III) hydroxide and indium metal shot, respectively. The title compounds crystallize isotypically in the trigonal system with space group R anti 3c (a = 1157.62(3), c = 6730.48(9) pm for the chromium, a = 1171.71(3), c = 6740.04(9) pm for the indium compound, Z = 6). The arrangement of the quasi-icosahedral [B{sub 12}H{sub 12}]{sup 2-} dianions can be considered as stacking of two times nine layers with the sequence..ABCCABBCA.. and the metal trications arrange in a cubic closest packed..abc.. stacking sequence. The metal trications are octahedrally coordinated by six water molecules of hydration, while another fifteen H{sub 2}O molecules fill up the structures as zeolitic crystal water or second-sphere hydrating species. Between these free and the metal-bonded water molecules, bridging hydrogen bonds are found. Furthermore, there is also evidence of hydrogen bonding between the anionic [B{sub 12}H{sub 12}]{sup 2-} clusters and the free zeolitic water molecules according to B-H{sup δ-}..{sup δ+}H-O interactions. Vibrational spectroscopy studies prove the presence of these hydrogen bonds and also show slight distortions of the dodecahydro-closo-dodecaborate anions from their ideal icosahedral symmetry (I{sub h}). Thermal decomposition studies for the example of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O gave no hints for just a simple multi-stepwise dehydration process. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

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.

4-[(5R*,10bR*-2-Methyl-1,10b-dihydropyrazolo[1,5-c][1,3]benzoxazin-5-yl]benzoic acid

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Jan Světlík

2008-03-01

Full Text Available In the title compound, C18H16N2O3, a potential inhibitor of the cyclooxygenase-2 isoenzyme, the pyrazoline ring exists in a flattened envelope conformation with one C atom deviating by 0.463 Å from the mean plane of the remaining four atoms. The puckering of the central oxazine ring is more severe, with one N atom and one C atom displaced by 0.235 (6 and 0.370 (2 Å, respectively, on opposite sides of the mean plane defined by the other four atoms; the conformation is that of a half-chair. As a result, the molecule as a whole is not planar. The carboxyl group is involved in an intermolecular O—H...N hydrogen bond, which links the molecules into centrosymmetric dimers.

Production of 15N-enriched nitric acid (H15NO3

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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.

(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.

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.

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°.

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.

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.

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].

Observation of $S=+1$ Narrow Resonances in the System $pK^0_s$ from $p+\\rm {C_3H_8}$ Collision at 10 GeV/$c$

CERN Document Server

Aslanyan, P Zh; Rikhvitskaya, G G

2004-01-01

Experimental data from a 2 m propane bubble chamber have been analyzed to search for an exotic baryon state, the $\\Theta^+$ baryon, in the $pK^0_s$ decay mode for the reaction $p+{\\rm C_3H_8}$ at 10 GeV/$c$. The $pK^0_s$ invariant mass spectrum shows resonant structures with $M_{p K_s^0}=1540\\pm 8$, $1613\\pm10$, $1821\\pm11$ MeV/$c^2$ and $\\Gamma_{p K_s^0}= 9.2\\pm1.8$, $16.1\\pm4.1$, $28.0\\pm9.4$ MeV/$c^2$. The statistical significance of these peaks has been estimated as $5.5$, $4.8$ and $5.0$ s.d., respectively. There are also small peaks in mass regions of 1487 (3.0 s.d.), 1690 (3.6 s.d.) and 1980 (3.0 s.d.) MeV/$c^2$.

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

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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.

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

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.

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.

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

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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.

1-[5-(Anthracen-9-yl-3-(4-nitrophenyl-4,5-dihydro-1H-pyrazol-1-yl]ethan-1-one

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Bao-Li Dong

2011-02-01

Full Text Available In the title compound, C25H19N3O3, steric repulsion between the methine H atom and one of the anthryl H atoms seems to be concomitant with the considerable distortion of the anthryl fragment from planarity. The side rings of the anthryl subtend an angle of 9.57 (8°, which is an extreme value among the known reliably determined structures. This angle correlates with the length of the bond by which the anthryl is attached to the rest of the molecule. In the anthryl fragment, the maximum deviation of one of the C atoms from the mean plane is 0.126 (3 Å and regards the carrier C atom involved in the repulsion between the anthryl and the methine H atoms. The interplanar angle between the pyrazoline ring and the anthryl fragment is 88.36 (5° and that between the pyrazoline and 4-nitrophenyl rings is 8.80 (15°. Weak intermolecular C—H...N, C—H...π and π–π interactions [centroid–centroid distances of 3.7659 (17, 3.9477 (15 and 3.8972 (15 Å] are pesent in the structure.

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

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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.

(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.

Synthesis and structure of PbBipy2(1-B10H9S(CH3)2)2

International Nuclear Information System (INIS)

Orlova, A.M.; Sivaev, I.B.; Lagun, V.L.; Katser, S.B.; Solntsev, K.A.; Kuznetsov, N.T.

1993-01-01

Lead complex with B 10 H 9 S(CH 3 ) 2 - anion and 2,2'-bipyridine was synthesized and characterized. According to the data of X-ray diffraction analysis the crystals belong to monoclinic crystal system, sp. gr. P2 1 /a: a = 9.940(4), b 31.568(4), c = 13.458(2) A, β = 111.09(2) deg, V = 3940(2) A 3 , Z = 4. The structure consists of monomer units PbBipy 2 (1-B 10 H 9 S(CH 3 ) 2 ) 2 . The Pb-B distances are within 3.24-3.55 A. 15 refs., 1 fig., 2 tabs

1-(3-Methoxyphenyl-2-(phenylsulfonylethan-1-one

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Sammer Yousuf

2012-08-01

Full Text Available In the title compound, C15H14O4S, the dihedral angle between the benzene and phenyl rings is 88.74 (10°. In the crystal, molecules are linked into a three-dimensional network by C—H...O hydrogen bonds and π–π stacking interactions [centroid–centroid distances = 3.6092 (13–3.8651 (13 Å].

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

{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.

Racemic methyl 3,10-dioxa-2-azatricyclo[6.2.1.02,6]undecane-4- carboxylate

KAUST Repository

Moosa, Basem; Fazal, Atif; Ali, Shaikh A.; Fettouhi, Mohammed

2011-01-01

The structure of the racemic title compound, C10H 15NO4, consists of a tricyclic skeleton comprising a six-membered piperidine ring and five-membered isoxazolidine and tetrahydrofuran rings. The piperidine ring adopts a distorted chair conformation

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

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

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Vladimir P. Zaytsev

2014-12-01

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

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.

Synthesis, characterization, crystal structure, and thermal analysis of 2-chloro-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl) acetamide

Energy Technology Data Exchange (ETDEWEB)

Sharma, R. [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India); Nayak, P. S.; Narayana, B. [Mangalore University, Mangalagangotri, Department of Studies in Chemistry (India); Kant, R., E-mail: rkvk.paper11@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India)

2015-12-15

The title compound, C{sub 13}H{sub 14}O{sub 2}N{sub 3}Cl, has been synthesized by the reaction of chloroacetyl chloride with 4-aminoantipyrine in basic media and characterized by FT-IR, CHN elemental analysis, UV-Vis, TGA, DTA, DSC and single crystal X-ray diffraction. crystals are monoclinic, sp. gr. P2{sub 1}/c, a = 6.9994(6), b = 12.4035(13), c = 15.836(2) Å, β = 100.367(9)°, Z = 4. The crystal structure is stabilized by N–H···O and C–H···O interactions, the former interactions result in the formation of dimers corresponding to R{sub 2}{sup 2} (10) graphset motif and the dimers are further connected by C–H···O hydrogen bonding forming chains. In addition, the thermal stability of the compound was determined by TGA, DTA, DSC analysis, and absorption at λ{sub max} = 298 nm was determined by UV-Vis spectrophotometer.

Rethinking Sensitized Luminescence in Lanthanide Coordination Polymers and MOFs: Band Sensitization and Water Enhanced Eu Luminescence in [Ln(C15H9O5)3(H2O)3]n (Ln = Eu, Tb).

Science.gov (United States)

Einkauf, Jeffrey D; Kelley, Tanya T; Chan, Benny C; de Lill, Daniel T

2016-08-15

A coordination polymer [Ln(C15H9O9)3(H2O)3]n (1-Ln = Eu(III), Tb(III)) assembled from benzophenonedicarboxylate was synthesized and characterized. The organic component is shown to sensitize lanthanide-based emission in both compounds, with quantum yields of 36% (Eu) and 6% (Tb). Luminescence of lanthanide coordination polymers is currently described from a molecular approach. This methodology fails to explain the luminescence of this system. It was found that the band structure of the organic component rather than the molecular triplet state was able to explain the observed luminescence. Deuterated (Ln(C15H9O9)3(D2O)3) and dehydrated (Ln(C15H9O9)3) analogues were also studied. When bound H2O was replaced by D2O, lifetime and emission increased as expected. Upon dehydration, lifetimes increased again, but emission of 1-Eu unexpectedly decreased. This reduction is reasoned through an unprecedented enhancement effect of the compound's luminescence by the OH/OD oscillators in the organic-to-Eu(III) energy transfer process.

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].

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)

5-Bromo-3-(4-chlorophenylsulfinyl-2-methyl-1-benzofuran

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Hong Dae Choi

2010-11-01

Full Text Available In the title compound, C15H10BrClO2S, the 4-chlorophenyl ring is oriented approximately perpendicular to the mean plane of the benzofuran ring [dihedral angle = 89.55 (9°]. In the crystal, molecules are linked through weak intermolecular C—H...O hydrogen bonds and and a Br...Br contact [3.783 (3 Å].

Preparation of 15N-13C-fulminic acid

International Nuclear Information System (INIS)

Wilmes, R.; Winnewisser, M.

1993-01-01

The precursor for the title compound was prepared in a three-step synthesis. The 13 C-label was incorporated in the first step employing 2- 13 C-ethyl acetate and the 15 N-label in the last step, using 15 N-sodium nitrite. Upon pyrolysis the precursor forms three fragments, one of them being the title compound. (Author)

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

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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.

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

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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].

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.

(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

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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.

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.

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.

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.

Estudo da ação dos fios de categute cromado e poliglecaprone 25, na ileocistoplastia em ratos, destacando a formação de cálculos

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Schauffert Marli Doroti

2000-01-01

Full Text Available Realizou-se um estudo da ação dos fios de categute cromado 6-0 e de poliglecaprone 25, 5-0, para determinar o fio ideal na ileocistoplastia em ratas. O maior objetivo, foi a profilaxia litiásica. Utilizaram-se 51 ratos de Wistar, que participaram de dois grupos experimentais: grupo do plano piloto (27 ratos, que foi o grupo categute (GC e grupo da tese do mestrado (24 ratos, que foi o grupo poliglecaprone (GP. Sob anestesia intraperitonial com pentobarbital sódico a 3%, todos os animais foram submetidos a ileocistoplastia, após laparotomia mediana longitudinal. Nos ratos do GC, a anastomose da bexiga urinária (aberta 0,5 cm sagitalmente no seu ápice, com a extremidade distal do segmento ileal ,era realizada por meio de pontos separados em plano único, com fio de categute cromado 6-0, e nas ratas do GP, com fio de poliglecaprone 25, 5-0. Seguiu-se a síntese da parede abdominal e recuperação anestésica. O estudo era realizado em 27, 42 e 57 dias nos animais do GC, que eram divididos em 3 subgrupos de 9 ratos. No GP, os animais eram analisados em 28 e 84 dias, por subgrupos de 12 animais. Transcorrido o tempo determinado para cada subgrupo, eram reoperados e observados os aspectos macroscópicos da cicatrização, aderências e formação de cálculos. A bexiga urinária ampliada pelo segmento ileal, era ressecada, aberta, lavada em solução salina isotônica, fixada no Líquido de Boüin, e processada , para histologia. A eutanásia era consumada com dose mínima letal anestésica. Os resultados apresentados, foram 29,6% de litíase, nas ratas do GC: 5,4% em 27dias; 10% em 42 dias e 14,25 em 57 dias do pós operatório (p.o.. Nas ratas do GP, não foram encontrados cálculos. Os estudos microscópicos, foram submetidos à análise estatística (a £ a 0,05, e utilizados para outro trabalho científico. Conclui-se: na ileocistoplastia com categute cromado 6-0, há 29,6% de cálculos, do 27o ao 57o dia p.o. e com o uso do fio de

(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.

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.

Nqrs Data for C3H2Cl10N2PSb[C3HCl4N2P·Cl6HSb](Subst. No. 0601)

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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 C3H2Cl10N2PSb [C3HCl4N2P·Cl6HSb] (Subst. No. 0601)

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.

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.

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.

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

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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.

(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

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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.

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.

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.

(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.

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

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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.

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

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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.

Racemic methyl 3,10-dioxa-2-azatricyclo[6.2.1.02,6]undecane-4- carboxylate

KAUST Repository

Moosa, Basem

2011-04-29

The structure of the racemic title compound, C10H 15NO4, consists of a tricyclic skeleton comprising a six-membered piperidine ring and five-membered isoxazolidine and tetrahydrofuran rings. The piperidine ring adopts a distorted chair conformation, while the isoxazolidine and tetrahydrofuran rings have envelope conformations.

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

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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.

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.

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.

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

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Hoong-Kun Fun

2012-08-01

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

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.

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.

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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.

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

Science.gov (United States)

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

2018-06-14

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

{2-[Bis(2,4-di-tert-butylphenoxyphosphanyloxy-κP]-3,5-di-tert-butylphenyl-κC1}[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I toluene monosolvate

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Detlef Selent

2012-02-01

Full Text Available The reaction of (η3-allyl[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I with tris(2,4-di-tert-butylphenylphosphite in toluene produces the title compound, [Rh(C42H62O3P(C8H12]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2 and 0.190 (2.

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.

(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].

Racemic methyl 3,10-dioxa-2-azatricyclo[6.2.1.02,6]undecane-4-carboxylate

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Basem A. Moosa

2011-05-01

Full Text Available The structure of the racemic title compound, C10H15NO4, consists of a tricyclic skeleton comprising a six-membered piperidine ring and five-membered isoxazolidine and tetrahydrofuran rings. The piperidine ring adopts a distorted chair conformation, while the isoxazolidine and tetrahydrofuran rings have envelope conformations.

Enthalpy increment measurements of Sr3Zr2O7(s) and Sr4Zr3O10(s)

International Nuclear Information System (INIS)

Banerjee, A.; Dash, S.; Prasad, R.; Venugopal, V.

1998-01-01

Enthalpy increment measurements on Sr 3 Zr 2 O 7 (s) and Sr 4 Zr 3 O 10 (s) were carried out using a Calvet micro-calorimeter. The enthalpy increment values were least squares analyzed with the constraints that H 0 (T)-H 0 (298.15 K) at 298.15 K equals to zero and C p 0 (298.15 K) equals to the estimated value. The dependence of enthalpy increment with temperature is given. (orig.)

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

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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.

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

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Salman A. Khan

2010-03-01

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

[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.

Crystal structure of 3-methyl-1-phenyl-5-(1H-pyrrol-1-yl-1H-pyrazole-4-carbaldehyde

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Joel T. Mague

2014-10-01

Full Text Available In the title compound, C15H13N3O, the pyrrolyl and phenyl rings make dihedral angles of 58.99 (5 and 34.95 (5°, respectively, with the central pyrazole ring. In the crystal, weak, pairwise C—H...O interactions across centers of symmetry form dimers, which are further associated into corrugated sheets running approximately parallel to (100 via weak C—H...N interactions.

(1-Phenyl-1H-1,2,3-triazol-4-ylmethyl pyridine-3-carboxylate

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Zakirjon Karimov

2010-07-01

Full Text Available In the title compound, C15H12N4O2, the dihedral angle between the planes of the nicotinoyloxy fragment and triazole ring is 88.61 (5°. The dihedral angle between the planes of triazole and benzene rings is 16.54 (11°. The crystal structure is stabilized by intermolecular C—H...N, C—H...O and C—H...π(triazole hydrogen bonds and aromatic π–π stacking interactions between the benzene and triazole rings [centroid–centroid distance = 3.895 (1 Å

H3S10ph broadly marks early-replicating domains in interphase ESCs and shows reciprocal antagonism with H3K9me2.

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Chen, Carol C L; Goyal, Preeti; Karimi, Mohammad M; Abildgaard, Marie H; Kimura, Hiroshi; Lorincz, Matthew C

2018-01-01

Phosphorylation of histone H3 at serine 10 (H3S10ph) by Aurora kinases plays an important role in mitosis; however, H3S10ph also marks regulatory regions of inducible genes in interphase mammalian cells, implicating mitosis-independent functions. Using the fluorescent ubiquitin-mediated cell cycle indicator (FUCCI), we found that 30% of the genome in interphase mouse embryonic stem cells (ESCs) is marked with H3S10ph. H3S10ph broadly demarcates gene-rich regions in G1 and is positively correlated with domains of early DNA replication timing (RT) but negatively correlated with H3K9me2 and lamin-associated domains (LADs). Consistent with mitosis-independent kinase activity, this pattern was preserved in ESCs treated with Hesperadin, a potent inhibitor of Aurora B/C kinases. Disruption of H3S10ph by expression of nonphosphorylatable H3.3S10A results in ectopic spreading of H3K9me2 into adjacent euchromatic regions, mimicking the phenotype observed in Drosophila JIL-1 kinase mutants . Conversely, interphase H3S10ph domains expand in Ehmt1 (also known as Glp ) null ESCs, revealing that H3S10ph deposition is restricted by H3K9me2. Strikingly, spreading of H3S10ph at RT transition regions (TTRs) is accompanied by aberrant transcription initiation of genes co-oriented with the replication fork in Ehmt1 -/- and Ehmt2 -/- ESCs, indicating that establishment of repressive chromatin on the leading strand following DNA synthesis may depend upon these lysine methyltransferases. H3S10ph is also anti-correlated with H3K9me2 in interphase murine embryonic fibroblasts (MEFs) and is restricted to intragenic regions of actively transcribing genes by EHMT2. Taken together, these observations reveal that H3S10ph may play a general role in restricting the spreading of repressive chromatin in interphase mammalian cells. © 2018 Chen et al.; Published by Cold Spring Harbor Laboratory Press.

(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-[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.

[2,3,7,8,13,14,17,18-Octa­kis(ethyl­sulfan­yl)-5,10,15,20-porphyrazinato]zinc(II)

Science.gov (United States)

Akkurt, Mehmet; Coşkun, Naciye Yılmaz; Kılıçaslan, Fatma Aytan; Yalçın, Sabiha Manav; Büyükgüngör, Orhan; Gül, Ahmet

2010-01-01

In the title compound, [Zn(C32H40N8S8)], the ZnII ion is coordinated by four N atoms in a slightly distorted square-planar environment. In addition, there is a Zn⋯S contact involving a symmetry-related S atom which, when considered, forms a pseudo-square-pyramidal coordination with respect to the ZnII ion. Three of the ethyl groups are disordered over two sites with occupancy ratios of 0.841 (10):0.159 (10), 0.802 (10):0.198 (10) and 0.457 (13):0.543 (13). Weak intra­molecular C—H⋯N and C—H⋯S inter­actions contribute to the stability of the mol­ecular conformation. Inter­molecular C—H⋯S contacts, weak C—H⋯π inter­actions and π–π stacking inter­actions [centroid–centriod distances = 3.832 (4) and 3.850 (5) Å] contribute to the stabilization of the crystal structure. PMID:21588217

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.

48 CFR 15.403-4 - Requiring certified cost or pricing data (10 U.S.C. 2306a and 41 U.S.C. 254b).

Science.gov (United States)

2010-10-01

... or pricing data (10 U.S.C. 2306a and 41 U.S.C. 254b). 15.403-4 Section 15.403-4 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION CONTRACTING METHODS AND CONTRACT TYPES CONTRACTING BY NEGOTIATION Contract Pricing 15.403-4 Requiring certified cost or pricing data (10 U.S.C. 2306a and 41 U.S.C...

Disease: H00713 [KEGG MEDICUS

Lifescience Database Archive (English)

Full Text Available H00713 Beckwith-Wiedemann syndrome Beckwith-Wiedemann syndrome (BWS) is an imprint...CD-10: Q87.3 MeSH: D001506 OMIM: 130650 PMID:20803657 ... AUTHORS ... Choufani S, Shuman C, Weksberg R ... TITLE ... Beckwith-Wiedema...ajmg.c.30267 ... PMID:19407494 ... AUTHORS ... Eggermann T ... TITLE ... Silver-Russell and Beckwith-Wiedema...re V, Colleaux L ... TITLE ... Paradoxical NSD1 mutations in Beckwith-Wiedemann syndrome and 11p15 anomalies i

Chlorido[1-diphenylphosphanyl-3-(phenylsulfanylpropane-κ2P,S](η5-pentamethylcyclopentadienyliridium(III chloride monohydrate

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Gerd Ludwig

2012-06-01

Full Text Available The crystal structure of the title compound, [Ir(C10H15Cl(C21H21PS]Cl·H2O, consists of discrete [Ir(η5-C5Me5Cl{Ph2P(CH23SPh-κP,κS}]+ cations, chloride anions and water molecules. The IrIII atom is coordinated by an η5-C5Me5 ligand, a chloride and a Ph2P(CH23SPh-κP,κS ligand, leading to a three-legged piano-stool geometry. In the crystal, two water molecules and two chloride anions are linked by weak O—H...Cl hydrogen bonding into tetramers that are located on centers of inversion. The H atoms of one of the methyl groups are disordered and were refined using a split model.

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.

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.

Ring rearrangements and reactivity of 3-((4-oxo-4H-chromen-3-ylmethylene-4-phenyl-1H-[1,5]benzodiazepin-2(3H-one toward some nucleophiles

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Hanan Salah

2017-05-01

Full Text Available Condensation of 4-phenyl-1H-[1,5]benzodiazepin-2(3H-one (1 with 3-formylchromone (2 afforded a mixture of 3-(chromenylmethylene[1,5]benzodiazepinone 3 and 14-chromenylbenzodiazepino[2,3:6,5]pyrano[2,3-b]benzodiazepine 4. Ring rearrangements of compound 3 with different nucleophilic reagents, such as potassium hydroxide and/or ammonium acetate led to rearrangement into pyranobenzodiazepine 5 and pyridobenzodiazepine 6, respectively. Treatment of compound 3 with hydrazine hydrate, hydroxylamine hydrochloride, malononitrile, cyanothioacetamide, 2-cyano-3,3-disufanylacrylonitrile, and/or 2-cyano-3-phenylamino-3-sufanylacrylonitrile, has been carried out at different conditions, leading to versatile heterocyclic substituted benzodiazepines at position 3, viz. pyrazole 8, isoxazole 9, pyridines 10 and 11, 1,3-dithiine 12, and 1,3-thiazine 13 derivatives.

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

Solid-state synthesis, structure and properties of a novel open-framework cadmium selenite bromide: [Cd10(SeO3)8Br4]·HBr·H2O

International Nuclear Information System (INIS)

Chen, Wen-Tong; Wang, Ming-Sheng; Wang, Guan-E; Chen, Hui-Fen; Guo, Guo-Cong

2013-01-01

A novel open-framework cadmium selenite bromide, [Cd 10 (SeO 3 ) 8 Br 4 ]·HBr·H 2 O (1), has been obtained by a solid-state reaction at 450 °C, and the structure has been determined by single-crystal X-ray diffraction analysis. Compound 1 crystallizes in Pbcm of the orthorhombic system: a=10.882(3), b=16.275(5), c=18.728(6) Å, V=3317(2) Å 3 , R1/wR2=0.0411/0.0659. Compound 1 is characteristic of a novel 3-D open-framework structure, composing ∞ 2 [CdSeO 3 ] layers and the pillars of edge-shared CdO 3 Br 2 square pyramids. The lattice water molecules and the HBr molecules locate in the voids of the framework. Optical absorption spectrum of 1 reveals the presence of an optical gap of 1.65 eV. Solid-state photoluminescent study indicates that compound 1 exhibits strong violet emission. TG–DSC measurement shows that compound 1 is thermally stable up to 200 °C. - Graphical abstract: A metal selenite halide has been synthesized and features a 3-D open-framework structure, composing edge-shared CdO 8 decahedra and pillars of edge-sharing pentahedra. UV–vis, TG–DSC and luminescent measurements are also reported. Highlights: • This paper reports a novel cadmium selenite bromide obtained by an intermediate-temperature solid-state reaction. • The title compound is characteristic of a novel 3-D open-framework structure, composing ∞ 2 [CdSeO 3 ] layers and the pillars of edge-shared CdO 3 Br 2 square pyramids. • The title compound is thermally stable up to 200 °C. • The title compound has an optical gap of 1.65 eV and exhibits strong violet emission

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.

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.

(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°.

N-(3-Chlorophenylmaleamic acid

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B. Thimme Gowda

2010-07-01

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

Disordered crystal structure of 20H-AlON, Al10O3N8

International Nuclear Information System (INIS)

Banno, Hiroki; Funahashi, Shiro; Asaka, Toru; Hirosaki, Naoto; Fukuda, Koichiro

2015-01-01

The disordered crystal structure of 20H-AlON (Al 10 O 3 N 8 ) was determined by combined use of X-ray powder diffraction and transmission electron microscopy. The title compound is hexagonal with space group P6 3 /mmc (Z=2) and the unit-cell dimensions are a=0.307082(5) nm, c=5.29447(8) nm and V=0.432376(12) nm 3 . The structural model showed the positional disordering of three of the six Al sites in the unit cell. The reliability indices calculated from the Rietveld method were R wp =6.97%, S (=R wp /R e )=1.68, R p =5.45%, R B =5.13% and R F =4.56%. We interpreted the disordered structure of 20H-AlON as a statistical average of six different types of ordered structural configurations, which are composed of an octahedral [Al(O, N) 6 ] layer and tetrahedral [Al(O, N) 4 ] layers. We demonstrated the high correlations between the hexagonal unit-cell dimensions and the octahedral layer concentrations for AlON and SiAlON polytypoids. - Graphical abstract: Variations of a and c/(n O +n T ) with n O /(n O +n T ). The a and c are the hexagonal unit-cell dimensions of AlON, SiAlON and AlN. The n O and n T are, respectively, the numbers of octahedral and tetrahedral layers in the unit cells. The unit-cell dimensions in literature are plotted in black plus for AlON and black cross for SiAlON. The unit-cell dimensions of AlN are a=0.3110 nm and c=0.4980 nm. - Highlights: • Crystal structure of Al10O3N8 is determined by laboratory X-ray powder diffraction. • The atom arrangements are represented by the split-atom model. • Six types of ordered atom arrangements are derived from the disordered structure. • Hexagonal unit-cell dimensions changed systematically for AlON and SiAlON compounds

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

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

2012-11-15

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

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

International Nuclear Information System (INIS)

Feng Meiling; Mao Jianggao

2005-01-01

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

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.

Butane-1,2,3,4-tetracarboxylic acid–1,10-phenanthroline–water (1/2/2

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Hong-lin Zhu

2011-07-01

Full Text Available The asymmetric unit of the title compound, 2C12H8N2·C8H10O8·2H2O, contains one 1,10-phenanthroline molecule, one half-molecule of butane-1,2,3,4-tetracarboxylic acid (H4BTC and a water molecule, with the complete tetra-acid generated by crystallographic inversion symmetry. Intermolecular O—H...O hydrogen bonds and π–π stacking interactions [centroid–centroid distances = 3.672 (2 and 3.708 (2 Å form an extensive three-dimensional network, which consolidates the crystal packing.

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

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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.

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

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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.

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

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Yu-Hua Ge

2012-01-01

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

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.

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

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Jin-Xia Mu

2015-12-01

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

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

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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.

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.

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

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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.

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...

2-Hydroxy-16-[(E-4-methylbenzylidene]-13-(4-methylphenyl-12-phenyl-1,11-diazapentacyclo[12.3.1.02,10.03,8.010,14]octadeca-3(8,4,6-triene-9,15-dione

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Raju Suresh Kumar

2010-08-01

Full Text Available In the title compound, C37H32N2O3, an intramolecular O—H...N hydrogen bond generates a five-membered ring, producing an S(5 motif. The piperidone ring adopts a half-chair conformation. The two fused pyrrolidine rings have similar envelope conformations. The interplanar angles between the benzene rings A/B and C/D are 75.68 (7 and 30.22 (6°, respectively. In the crystal structure, adjacent molecules are interconnected into chains propagating along the [010] direction via intermolecular C—H...O hydrogen bonds. Further stabilization is provided by weak C—H...π interactions.

Modelling of phase equilibria in CH4–C2H6–C3H8–nC4H10–NaCl–H2O systems

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Li, Jun; Zhang, Zhigang; Luo, Xiaorong; Li, Xiaochun

2015-01-01

Highlights: • A new model was established for the phase equilibria of C1–C2–C3–nC4–brine systems. • The model can reproduce of hydrocarbon–brine equilibria to high T&P and salinity. • The model can well predict H 2 O solubility in light hydrocarbon rich phases. - Abstract: A thermodynamic model is presented for the mutual solubility of CH 4 –C 2 H 6 –C 3 H 8 –nC 4 H 10 –brine systems up to high temperature, pressure and salinity. The Peng–Robinson model is used for non-aqueous phase fugacity calculations, and the Pitzer model is used for aqueous phase activity calculations. The model can accurately reproduce the experimental solubilities of CH 4 , C 2 H 6 , C 3 H 8 and nC 4 H 10 in water or NaCl solutions and H 2 O solubility in the non-aqueous phase. The experimental data of mutual solubility for the CH 4 –brine subsystem are sufficient for temperatures exceeding 250 °C, pressures exceeding 1000 bar and NaCl molalities greater than 6 molal. Compared to the CH 4 –brine system, the mutual solubility data of C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine are not sufficient. Based on the comparison with the experimental data of H 2 O solubility in C 2 H 6 -, C 3 H 8 - or nC 4 H 10 -rich phases, the model has an excellent capability for the prediction of H 2 O solubility in hydrocarbon-rich phases, as these experimental data were not used in the modelling. Predictions of hydrocarbon solubility (at temperatures up to 200 °C, pressures up to 1000 bar and NaCl molalities greater than 6 molal) were made for the C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine systems. The predictions suggest that increasing pressure generally increases the hydrocarbon solubility in water or brine, especially in the lower-pressure region. Increasing temperature usually decreases the hydrocarbon solubility at lower temperatures but increases the hydrocarbon solubility at higher temperatures. Increasing water salinity dramatically decreases

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].

Synthesis of 5-Substituted 3-Amino-1H-Pyrazole-4-Carbonitriles as Precursors for Microwave Assisted Regiospecific Syntheses of Pyrazolo[1,5-a]Pyrimidines

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Fawzia Al-Qalaf

2008-12-01

Full Text Available A simple route to 3-oxoalkanonitrile 5, aprecursor of the title compounds is described. Reaction of enaminones 2 with hydroxylamine hydrochloride in ethanol yielded aldoximes 3 that were converted readily into 5 in basic medium. This method has been successfully applied with a number of substrates and resulted in excellent yields of the products. Reacting 5 with trichloroacetonitrile afforded 3-amino-2-aroyl-4,4,4-trichloro-2-butenenitriles 6 that condensed with hydrazines to yield 3-amino-1H-pyrazole-4-carbonitrilederivatives 8. Substituted pyrazolo[1,5-a]pyridmidines have been prepared with regioselective condensation reactions of 8 with nonsymmetrical dielectrophiles. The structures of compounds obtained were deduced based on 1H-NMR, 1H-15N HMBC- measurements.

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.

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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.

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

International Nuclear Information System (INIS)

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

2001-01-01

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

(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.

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

International Nuclear Information System (INIS)

Polyanskaya, T.M.

2006-01-01

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

Instability of TiC and TiAl3 compounds in Al-10Mg and Al-5Cu alloys by addition of Al-Ti-C master alloy

Institute of Scientific and Technical Information of China (English)

无

2006-01-01

The performance of Al-Ti-C master alloy in refining Al-10Mg and A1-5Cu alloys was studied by using electron probe micro-analyzer (EPMA) and X-ray diffractometer (XRD) analysis.The results indicate that there are obvious fading phenomena in both Al-10Mg and Al-5Cu alloys with the addition of Al-5Ti-0.4C refiner which contains TiC and TiAl3 compounds.Mg element has no influence on the stability of TiC and TiAl3, while TiC particles in Al-10Mg alloy react with Al to form Al4C3 particles, resulting in the refinement fading.However, TiC particles are relatively stable in Al-5Cu alloy, while TiAl3 phase reacts with Al2Cu to produce a new phase Ti(Al, Cu)2, which is responsible for the refinement fading in Al-5Cu alloy.These indicate that the refinement fading will not occur only when both the TiC particles and TiAl3 compound of Al-Ti-C refiner are stable in Al alloys.

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

Science.gov (United States)

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

2018-06-01

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

4-[3-(4-Methylpiperidin-1-ylpropanamido]benzenesulfonamide monohydrate

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Hasan Türkmen

2012-12-01

Full Text Available In the title compound, C15H23N3O3S·H2O, the piperidine ring has a chair conformation. In the crystal, the sulfonamide molecules are linked by N—H...O hydrogen bonds, forming a layer parallel to (10-1. The layers are interconnected via N—H...Ow, Ow—H...N and Ow—H...O (w = water hydrogen bonds, forming a three-dimensional network.

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.

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

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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.

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.

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].

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.

(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.

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.

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.

The synthesis of Org 3770 labelled with 3H, 13C and 14C

International Nuclear Information System (INIS)

Kaspersen, F.M.; Rooij, F.A.M. van; Sperling, E.G.M.; Wieringa, J.H.

1989-01-01

The syntheses of 1,2,3,4,10,14b-hexahydro-2-methylpyrazino[2,1-a]pyrido[2,3-c][2]benazepine (Org 3770) labelled with 3 H (and 2 H), 13 C and 14 C are described. Tritiated Org 3770 was prepared either by exchange under alkaline conditions with tritiated water or catalytic reductive dehalogenation of a chloro analogue with 3 H 2 . 13 C-labelled material was obtained in a seven-step synthesis starting from 13 C-labelled benzene whereas 14 C-Org 3770 was prepared in a three-step synthesis starting with 14 CO 2 . All labelled compounds were analyzed by TLC, HPLC, MS and NMR. (author)

Phosphorus-31, 15N, and 13C NMR of glyphosate: Comparison of pH titrations to the herbicidal dead-end complex with 5-enolpyruvoylshikimate-3-phosphate synthase

International Nuclear Information System (INIS)

Castellino, S.; Leo, G.C.; Sammons, R.D.; Sikorski, J.A.

1989-01-01

The herbicidal dead-end ternary complex (E S3P Glyph ) of glyphosate [N-(phosphonomethyl)glycine] with 5-enolpyruvoylshikimate-3-phosphate synthase (EPSPS) and the substrate shikimate 3-phosphate (S3P) has been characterized by 31 P, 15 N, and 13 C NMR. The NMR spectra of EPSPS-bound glyphosate show unique chemical shifts (δ) for each of the three nuclei. By 31 P NMR, glyphosate in the dead-end complex is a distinct species 3.5 ppm downfield from free glyphosate. The 13 C signal of glyphosate in the dead-end complex is shifted 4 ppm downfield from that of free glyphosate. The 15 N signal for glyphosate (99%) in the dead-end complex is 5 ppm further downfield than that of any free zwitterionic species and 10 ppm downfield from that of the average free species at pH 10.1. The structures of each ionic state of glyphosate are modeled with force field calculations by using MacroModel. A correlation is made for the 31 P δ and the C-P-O bond angle, and the 13 C and 15 N δ values are postulated to be related to C-C-O and C-N-C bond angles, respectively. The downfield 31 P chemical shift perturbation for S3P in the EPSPS binary complex is consistent with ionization of the 3-phosphate of S3P upon binding. Comparison with the S3P 31 P δ vs pH titration curve specifies predominantly the dianion of the 3-phosphate in the E S3P binary complex, while the E S3P Glyph complex indicates net protonation at the 3-phosphate. Chemical shift perturbations of this latter type may be explained by changes in the O-P-O bond angle

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

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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°.

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.

1,5-Diamino-2,6-dibromo-9,10-anthraquinone

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Wilhelm Seichter

2012-03-01

Full Text Available In the title compound, C14H8Br2N2O2, the molecular structure features intramolecular N—H...O [2.639 (2 Å and 130°] and N—H...Br [3.053 (2 Å and 114°] hydrogen bonding. Due to inversion symmetry, the asymmetric part of the unit cell consits of one half-molecule. In the crystal, inversion dimers linked by pairs of N—H...O [2.955 (2 Å and 135°] hydrogen bonds occur. The structure also features C=O...π [3.228 (2 Å] and Br...Br [3.569 (1 Å] contacts.

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

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Jinpeng Zhang

2012-08-01

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

The supramolecular architecture of tris(naphthalene-1,5-diaminium) bis(5-aminonaphthalen-1-aminium) octakis[hydrogen (5-carboxypyridin-3-yl)phosphonate].

Science.gov (United States)

Wilk, Magdalena; Janczak, Jan; Videnova-Adrabinska, Veneta

2012-09-01

The asymmetric unit of the title compound, 3C(10)H(12)N(2)(2+)·2C(10)H(11)N(2)(+)·8C(6)H(5)NO(5)P(-), contains one and a half naphthalene-1,5-diaminium cations, in which the half-molecule has inversion symmetry, one 5-aminonaphthalen-1-aminium cation and four hydrogen (5-carboxypyridin-3-yl)phosphonate anions. The crystal structure is layered and consists of hydrogen-bonded anionic monolayers between which the cations are arranged. The acid monoanions are organized into one-dimensional chains along the [101] direction via hydrogen bonds established between the phosphonate sites. (C)O-H···N(py) hydrogen bonds (py is pyridine) crosslink the chains to form an undulating (010) monolayer. The cations serve both to balance the charge of the anionic network and to connect neighbouring layers via multiple hydrogen bonds to form a three-dimensional supramolecular architecture.

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

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Assem Barakat

2016-09-01

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

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.

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

1-(4,5-Dinitro-10-azatricyclo[6.3.1.02,7]dodeca-2,4,6-trien-10-yl-2,2,2-trifluoroethanone

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Jin-Tang Wang

2008-12-01

Full Text Available In the title compound, C13H10F3N3O5, a derivative of andrographolide, the five-membered ring adopts an envelope conformation, while the non-planar six-membered ring has a chair conformation. An intramolecular C—H...F hydrogen bond results in the formation of a non-planar six-membered ring adopting a twisted conformation. In the crystal structure, intermolecular C—H...O hydrogen bonds link the molecules into centrosymmetric dimers.

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.

(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].

Ethyl 2-{4-[(1,5-dibenzyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-3-ylmethyl]-1H-1,2,3-triazol-1-yl}acetate

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Hind Jabli

2010-01-01

Full Text Available The reaction of 1,5-dibenzyl-3-propargyl-1,5-benzodiazepine-2,4-dione with ethyl azidoacetate in the presence of copper sulfate pentahydrate and sodium ascorbate leads to the formation of the title regioisomer, C30H29N5O4, which features a phenylene ring fused with a seven-membered diazepinyl ring. The latter ring adopts a boat conformation (with the methyltriazolylacetate-bearing C atom as the prow and the fused-ring C atoms as the stern. The benzyl groups connected to the diazepinyl ring jprotrude from the sides; the methyltriazolylacetate substituent occupies an axial position.

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

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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

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

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Hong Dae Choi

2012-04-01

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

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

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Peter W. Dibble

2008-09-01

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

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.

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.

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

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Feng-Ling Yang

2008-12-01

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

4-Methyl-N-(1-methyl-1H-indazol-5-ylbenzenesulfonamide

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Hakima Chicha

2013-09-01

Full Text Available In the title compound, C15H15N3O2S, the fused ring system is close to planar, the largest deviation from the mean plane being 0.030 (2 Å, and makes a dihedral angle of 48.84 (9° with the benzene ring belonging to the methylbenzenesulfonamide moiety. In the crystal, molecules are connected through N—H...N hydrogen bonds and weak C—H...O contacts, forming a two-dimensional network parallel to (001.

3-Methyl-4-(3-methylphenyl-5-(2-pyridyl-4H-1,2,4-triazole

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Dun-Ru Zhu

2009-05-01

Full Text Available In the molecule of the title compound, C15H14N4, the triazole ring is oriented at dihedral angles of 30.8 (2 and 67.4 (2° with respect to the pyridine and benzene rings, respectively. The crystal structure is stabilized by C—H...N hydrogen-bonding interactions, forming chains of molecules along [overline{1}01].

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

Ionic fragmentation of a natural product, limonene (C10H16), following core [C 1s] photoionization

International Nuclear Information System (INIS)

Castilho, R.B. de; Nunez, C.V.; Coutinho, L.H.; Lago, A.F.; Bernini, R.B.; Souza, G.G.B. de

2007-01-01

Photoionization of the limonene [C 10 H 16 ] molecule was studied for the first time following C 1s ionization, using synchrotron radiation and time-of-fight mass spectrometry. As a reference for further analysis of the photon induced fragmentation of the limonene molecule, the He(I) mass spectrum was also obtained. Previously unreported singly charged species have been observed at 310 eV: H + , C + , CH + , CH 2 + , CH 3 + . A close similarity has been observed between the high photon energy mass spectrum and the standard electron impact mass spectrum of limonene, obtained at 70 eV. In particular, the base peak [C 5 H 8 + , m/q = 68], known to result from a Retro Diels-Alder reaction, remains the same in both cases. Approximate values for the mean kinetic energy were determined for all ionic species

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

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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.

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

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Yong-Hong Lu

2012-01-01

Full Text Available In the title compound, C11H10N2O, the cyanide group is twisted away from the indole-ring plane [Ccy—Cme—Car—Car = 70.7 (2°; cy = cyanide, me = methylene, ar = aromatic], whereas the methoxy C atom is almost coplanar with the ring system [displacement = 0.014 (5 Å]. In the crystal, N—H...N hydrogen bonds link the molecules into C(7 chains propagating in [100].

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.

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.

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

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YuanQi Yu

2011-10-01

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

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.

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

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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.

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

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Sergey A. Smolnikov

2017-12-01

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

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

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Michael J. Ferguson

2008-10-01

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

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.

Tricarbonyl[tris(1-methyl-1H-imidazol-2-yl-κN3methanol]manganese(I trifluoromethanesulfonate

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Guido J. Reiss

2012-09-01

Full Text Available In the title compound, [Mn(C13H16N6O(CO3](CF3O3S, the MnI atom has a slightly distorted octahedral geometry. The three CO ligands have C—Mn—C angles in the range 89.44 (10–92.31 (9°, while the three N atoms of the tripodal ligand form significantly smaller N—Mn—N angles of 82.76 (2–85.51 (6°. The three N atoms of the tripodal ligand and the three carbonyl ligands coordinate facially. In the crystal, the trifluoromethanesulfonate counter anion is connected by a medium-strength O—H...O hydrogen bond to the hydroxyl group of the manganese complex.

5-Methyl-2-phenyl-2H-pyrazol-3-ol

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Feng Zhi

2008-10-01

Full Text Available The title compound, C10H10N2O, known as Edaravone (MCI-186, was crystallized from methanol. The two independent molecules in the asymmetric unit are linked through an O—H...O hydrogen bond. One molecule adopts a ketone form, while the other adopts an enol form. In the crystal structure, molecules are linked through intermolecular N—H...O hydrogen bonds, forming chains running along the b axis.

[3-(5-Nitro-2-furyl-1-phenyl-1H-pyrazol-4-yl](phenylmethanone

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Jia Hao Goh

2010-05-01

Full Text Available In the title pyrazole compound, C20H13N3O4, an intramolecular C—H...O hydrogen bond generates a seven-membered ring, producing an S(7 ring motif. The essentially planar furan and pyrazole rings [maximum deviations of 0.002 (1 and 0.007 (1 Å, respectively] are coplanar with each other, forming a dihedral angle of 3.06 (10°. The pyrazole ring forms dihedral angles of 8.51 (9 and 56.81 (9° with the two benzene rings. The nitro group is coplanar with the attached furan ring, as indicated by the dihedral angle of 2.5 (3°. In the crystal packing, intermolecular C—H...O hydrogen bonds link adjacent molecules into two-molecule-wide chains along the a axis. The crystal packing is further stabilized by weak intermolecular C—H...π and π–π interactions [centroid–centroid distance = 3.4441 (10 Å].

Chlorido(1,3-dimethylthiourea-κSbis(triphenylphosphine-κPcopper(I acetonitrile hemisolvate

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Brian W. Skelton

2009-08-01

Full Text Available The title compound, [CuCl(C3H8N2S(C18H15P2]·0.5CH3CN, was prepared by the reaction of copper(I chloride with 1,3-dimethylthiourea (dmtu and triphenylphosphine (PPh3 in acetonitrile. The CuI atom has a distorted tetrahedral environment formed by two P atoms from triphenylphosphine, one S atom from the dmtu ligand and one Cl atom. In addition, the molecules exhibit intra- and intermolecular N—H...Cl interactions.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-12-01

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

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.

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.

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

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S. Santhiya

2013-11-01

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

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.

(S-N-Phenyl-tert-butanesulfinamide

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Xiaofei Sun

2012-06-01

Full Text Available The asymmetric unit of the title compound, C10H15NOS, contains two independent molecules with similar conformations. In the crystal, molecules are linked in a head-to-tail fashion by N—H...O hydrogen bonds into chains running along the b axis. The absolute configuration was assigned on the basis of known chirality of the parent compound.

Structure and magnetic properties of Ba5Ce1.25Mn3.75O15, a new 10H-polytype in the Ba–Ce–Mn–O system

International Nuclear Information System (INIS)

Macías, Mario A.; Mentré, Olivier; Colis, Silviu; Cuello, Gabriel J.; Gauthier, Gilles H.

2013-01-01

Based on the peculiar magnetic properties that are observed in pseudo one-dimensional manganites, we decided to synthesize the new Ba 5 Ce 1.25 Mn 3.75 O 15 compound. The preparation was performed by solid state reaction in air at about 1350 °C, for which we found that the compound crystallizes in a hexagonal symmetry with space group P6 3 /mmc (No-194) and cell parameters a=b=5.7861(2) Å and c=23.902(1) Å. The structural description was correlated with neutron diffraction and bond valence calculations, confirming the presence of Ce 4+ and Mn 4+ segregated in the different crystallographic positions. Ba 5 Ce 1.25 Mn 3.75 O 15 displays evidence for strong AFM couplings already set at room temperature. The main arrangement of Mn 4+ in magnetically isolated tetramers of face-sharing octahedra is responsible for a metamagnetic-like transition around 50 K. - Graphical abstract: The new Ba 5 Ce 1.25 Mn 3.75 O 15 polytype shows strong AFM couplings in magnetically isolated [Ce 0.25 Mn 3.75 O 15 ] tetramers of face-sharing octahedral, resulting in a metamagnetic-like transition around 50 K. Highlights: ► Ba 5 Ce 1.25 Mn 3.75 O 15 , a new 10H polytype, has been prepared in the Ba–Ce–Mn–O system. ► The compound crystallizes in the P6 3 /mmc space group with (cchhh) 2 stacking sequence. ► [Ce 0.25 Mn 3.75 O 15 ] tetramers are separated by [CeO 6 ] octahedra in the structure. ► Instead of robust AFM ordering, a metamagnetic-like transition is found around 50 K.

Synthesis and Electronic Structure of Dissymmetrical, Naphthalene-Bridged Sandwich Complexes [Cp ' Fe(mu-C10H8)MCp*](x) (x=0,+1; M = Fe, Ru; Cp ' = eta(5)-C5H2-1,2,4-tBu(3); Cp* = eta(5)-C5Me5)

NARCIS (Netherlands)

Malberg, J.; Lupton, E.; Schnöckelborg, E.M.; de Bruin, B.; de Sutter, J.; Meyer, K.; Hartl, F.; Wolf, R.

2013-01-01

The dissymmetrical naphthalene-bridged complexes [Cp'Fe(mu-C10H8)FeCp*] (3; Cp* = eta(5)-C5Me5, Cp' = eta(5)-C5H2-1,2,4-tBu(3)) and [Cp'Fe(mu-C10H8)RuCp*] (4) were synthesized via a one-pot procedure from FeCl2(thf)(1.5), Cp'K, KC10H8, and [Cp*FeCl(tmeda)] (tmeda =

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

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Rajamani Raja

2015-09-01

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

(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.

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.

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.

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.

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

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S. Sriman Narayanan

2008-09-01

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

1-[(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.

(C2N2H10)[Fe xV1-x(HPO3)F3] (x = 0.44, 0.72): Two new organically templated phosphites

International Nuclear Information System (INIS)

Cisneros, Jose L.; Fernandez-Armas, Sergio; Mesa, Jose L.; Pizarro, Jose L.; Arriortua, Maria I.; Rojo, Teofilo

2006-01-01

(C 2 N 2 H 10 )[Fe x V 1-x (HPO 3 )F 3 ] (x = 0.44, 0.72) have been synthesized using mild solvothermal conditions under autogenous pressure and the ethylenediamine molecule as templating agent. The crystal structures have been determined from X-ray single-crystal diffraction data. The compounds crystallize in the orthorhombic P2 1 2 1 2 1 space group with Z = 4 and unit-cell parameters a = 12.8494(9), b = 9.5430(6), c = 6.4372(5) A, and a = 12.8578(1), b = 9.5342(1), c = 6.4370(7) A for (C 2 N 2 H 10 )[Fe 0.44 V 0.56 (HPO 3 )F 3 ] and (C 2 N 2 H 10 )[Fe 0.72 V 0.28 (HPO 3 )F 3 ] (1) and (2), respectively. These isostructural compounds exhibit a monodimensional crystal structure formed by pillared double anionic chains with the formula [M(HPO 3 )F 3 ] 2- , extended along the [0 0 1] direction. These doubled ionic chains are the result of the linking of two simple chains in which there are alternating octahedral [MO 3 F 3 ] and tetrahedral groups [HPO 3 ]. The ethylendiammonium cations are placed in the space delimited by three different chains. The metallic ions are interconnected by the pseudo-pyramidal (HPO 3 ) 2- phosphite oxoanions, adopting a slightly distorted octahedral geometry. The IR spectra show bands corresponding to the phosphite oxoanion and the ethylendiamonium cation at 2400 and 1600 cm -1 , respectively. The thermogravimetric analyses show that these phases are stable up to ca. 280 deg. C, at higher temperatures, the decomposition of the crystal structure begins by calcination of the organic cation and the elimination of the fluoride anions. The diffuse reflectance spectra show bands of the V 3+ ion (d 2 ) in octahedral symmetry. The values of the Dq (1540, 1540 cm -1 ), and Racah parameters, B (560, 535 cm -1 ) and C (3055, 3140 cm -1 ) for (1) and (2), respectively, correspond with those usually found for octahedrically coordinated V(III) compounds. Magnetic measurements, performed on a powered sample from 5.0 to 300 K at 1000 G, in the ZFC and

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.

(10R,13R-17-(6-Hydroxy-5-methylheptan-2-yl-10,13-dimethyl-2,3,4,7,8,9,10,11,12,13,14,15,16,17-tetradecahydro-1H-cyclopenta[a]phenanthren-3-ol hemihydrate: a bioactive steroid isolated from the Indian herb Artemisia reticulata

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A. K. Bauri

2017-08-01

Full Text Available The title tetracyclic steroidal compound, C27H46O2·0.5H2O, crystallized as a monohydrate with two independent molecules (1 and 2 in the asymmetric unit. In both molecules, the conformations of the three cyclohexane rings (A, B and C are chair, half-chair and chair, respectively. The fourth ring, D, has a twisted conformation on the bond linking the D and C rings. The crystal structure is stabilized by hydrogen bonding with the two independent molecules being linked through the solvent water molecule via various O—H...O hydrogen bonds, forming layers parallel to (-101.

(4-Nitrophenylmethyl 2,3-dihydro-1H-pyrrole-1-carboxylate: crystal structure and Hirshfeld analysis

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Julio Zukerman-Schpector

2018-03-01

Full Text Available In the title compound, C12H12N2O4, the dihydropyrrole ring is almost planar (r.m.s. deviation = 0.0049 Å and is nearly coplanar with the adjacent C2O2 residue [dihedral angle = 4.56 (9°], which links to the 4-nitrobenzene substituent [dihedral angle = 4.58 (8°]. The molecule is concave, with the outer rings lying to the same side of the central C2O2 residue and being inclined to each other [dihedral angle = 8.30 (7°]. In the crystal, supramolecular layers parallel to (10-5 are sustained by nitrobenzene-C—H...O(carbonyl and pyrrole-C—H...O(nitro interactions. The layers are connected into a three-dimensional architecture by π(pyrrole–π(nitrobenzene stacking [inter-centroid separation = 3.7414 (10 Å] and nitro-O...π(pyrrole interactions.

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.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

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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.

Electronic structure of A15 compounds

International Nuclear Information System (INIS)

Pickett, W.E.

1980-01-01

For the past twenty-five years compounds with the A15 crystal structure have dominated the class of high temperature superconductors. The crystal structure of an A15 compound A 3 B is cubic (space group O/sub h/ 3 ). However, the site symmetry (D/sub 2d/) of the A atoms is much lower than cubic, an unusual occurrence in cubic binary compounds. Variations on this theme have supplied the basis of many theoretical models of the anomalous temperature (T) dependence of normal state properties and the low temperature cubic reversible tetragonal structural transformations which accompany high values of T/sub c/ in A15 compounds. In this paper results of self-consistent pseudopotential band structure calculations are used to assess some important aspects of the unique and unusual behavior in A15 compounds: (1) the role of the B atom in determining the overall electronic structure will be shown to be important; (2) the effect of the low site symmetry of the A atom on the charge density and potential will be assessed; and (3) the bonding will be shown to be metallic-covalent with no significant A-B charge transfer

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.

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

1-(3-Fluorophenyl-3-(4-nitrophenylurea

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Mu-Sen Lin

2012-07-01

Full Text Available In the title compound, C13H10FN3O3, the dihedral angle between the fluorophenyl and nitrophenyl ring planes is 6.51 (9°. The crystal structure features N—H...O hydrogen bonds.

N-(2-Methylphenyl-1,2-benzoselenazol-3(2H-one

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Xu Zhu

2013-10-01

Full Text Available In the title Ebselen [systematic name: (2-phenyl-1,2-benzoisoselenazol-3-(2H-one] analogue, C14H11NOSe, the benzisoselenazolyl moiety (r.m.s. deviation = 0.0209 Å is nearly perpendicular to the N-arenyl ring, making a dihedral angle of 78.15 (11°. In the crystal, molecules are linked by C—H...O and Se...O interactions into chains along the c-axis direction. The Se...O distance [2.733 (3 Å] is longer than that in Ebselen (2.571 (3 Å].

Crystal structure of 1-{4-hydroxy-3-[(pyrrolidin-1-ylmethyl]phenyl}-3-phenylprop-2-en-1-one

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Abdullah Aydın

2016-05-01

Full Text Available In the title compound, C20H21NO2, the pyrrolidine ring adopts an envelope conformation with the N atom at the flap position. The central benzene ring makes dihedral angles of 21.39 (10 and 80.10 (15° with the phenyl ring and the mean plane of the pyrrolidine ring, respectively. The molecular conformation is stabilized by an intramolecular O—H...N hydrogen bond, which closes an S(6 ring. A weak C—H...π interaction is observed in the crystal.

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.

Synthesis of trifluoromethyl-substituted pyrazolo[4,3-c]pyridines – sequential versus multicomponent reaction approach

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Barbara Palka

2014-07-01

Full Text Available A straightforward synthesis of 6-substituted 1-phenyl-3-trifluoromethyl-1H-pyrazolo[4,3-c]pyridines and the corresponding 5-oxides is presented. Hence, microwave-assisted treatment of 5-chloro-1-phenyl-3-trifluoromethylpyrazole-4-carbaldehyde with various terminal alkynes in the presence of tert-butylamine under Sonogashira-type cross-coupling conditions affords the former title compounds in a one-pot multicomponent procedure. Oximes derived from (intermediate 5-alkynyl-1-phenyl-3-trifluoromethyl-1H-pyrazole-4-carbaldehydes were transformed into the corresponding 1H-pyrazolo[4,3-c]pyridine 5-oxides by silver triflate-catalyzed cyclization. Detailed NMR spectroscopic investigations (1H, 13C, 15N and 19F were undertaken with all obtained products.

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.

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)

Carbonate hydrates of the heavy alkali metals: preparation and structure of Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O und Cs{sub 2}CO{sub 3} . 3 H{sub 2}O; Carbonat-Hydrate der schweren Alkalimetalle: Darstellung und Struktur von Rb{sub 2}CO{sub 3} . 1,5 H{sub 2}O und Cs{sub 2}CO{sub 3} . 3 H{sub 2}O

Energy Technology Data Exchange (ETDEWEB)

Cirpus, V.; Wittrock, J.; Adam, A. [Koeln Univ. (Germany). Inst. fuer Anorganische Chemie

2001-03-01

Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O and Cs{sub 2}CO{sub 3} . 3 H{sub 2}O were prepared from aqueous solution and by means of the reaction of dialkylcarbonates with RbOH and CsOH resp. in hydrous alcoholes. Based on four-circle diffractometer data, the crystal structures were determined (Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O: C2/c (no. 15), Z = 8, a = 1237.7(2) pm, b = 1385.94(7) pm, c = 747.7(4) pm, {beta} = 120.133(8) , V{sub EZ} = 1109.3(6) . 10{sup 6} pm{sup 3}; Cs{sub 2}CO{sub 3} . 3 H{sub 2}O: P2/c (no. 13), Z = 2, a = 654.5(2) pm, b = 679.06(6) pm, c = 886.4(2) pm, {beta} = 90.708(14) , V{sub EZ} = 393.9(2) . 10{sup 6} pm{sup 3}). Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O is isostructural with K{sub 2}CO{sub 3} . 1.5 H{sub 2}O. In case of Cs{sub 2}CO{sub 3} . 3 H{sub 2}O no comparable structure is known. Both structures show {sub {infinity}}{sup 1}[(CO{sub 3}{sup 2-})(H{sub 2}O)]-chains, being connected via additional H{sub 2}O forming columns (Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O) and layers (Cs{sub 2}CO{sub 3} . 3 H{sub 2}O), respectively. (orig.)

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.

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

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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.

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

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Naki Çolak

2013-07-01

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

1-(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.

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].

Synthesis, structure and magnetic behavior of a new three-dimensional Manganese phosphite-oxalate: [C2N2H10][Mn2II(OH2)2(HPO3)2(C2O4)

International Nuclear Information System (INIS)

Ramaswamy, Padmini; Mandal, Sukhendu; Natarajan, Srinivasan

2009-01-01

A novel manganese phosphite-oxalate, [C 2 N 2 H 10 ][Mn 2 II (OH 2 ) 2 (HPO 3 ) 2 (C 2 O 4 )] has been hydothermally synthesized and its structure determined by single-crystal X-ray diffraction. The structure consists of neutral manganese phosphite layers, [Mn(HPO 3 )] ∞ , formed by MnO 6 octahedra and HPO 3 units, cross-linked by the oxalate moieties. The organic cations occupy the middle of the 8-membered one-dimensional channels. Magnetic studies indicate weak antiferromagnetic interactions between the Mn 2+ ions. - Abstract: A new antiferromagnetic three-dimensional inorganic-organic hybrid compound, [C 2 N 2 H 10 ][Mn 2 II (OH 2 ) 2 (HPO 3 ) 2 (C 2 O 4 )] has been prepared hydrothermally. The compound has neutral manganese layers pillared by oxalate units. The neutral manganese layers are shown here. Display Omitted

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.

Ethyl 2-{4-[(1,5-dibenzyl-2,4-dioxo-2,3,4,5-tetra-hydro-1H-1,5-benzo-diazepin-3-yl)meth-yl]-1H-1,2,3-triazol-1-yl}acetate.

Science.gov (United States)

Jabli, Hind; Kandri Rodi, Y; Ladeira, Sonia; Essassi, El Mokhtar; Ng, Seik Weng

2009-12-12

The reaction of 1,5-dibenzyl-3-propargyl-1,5-benzodiazepine-2,4-dione with ethyl azido-acetate in the presence of copper sulfate pentahydrate and sodium ascorbate leads to the formation of the title regioisomer, C(30)H(29)N(5)O(4), which features a phenyl-ene ring fused with a seven-membered diazepinyl ring. The latter ring adopts a boat conformation (with the methyl-triazolylacetate-bearing C atom as the prow and the fused-ring C atoms as the stern). The benzyl groups connected to the diazepinyl ring jprotrude from the sides; the methyl-triazolylacetate substituent occupies an axial position.

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

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Zhensheng Li

2013-07-01

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

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.

Serendipitous preparation of fac-(acetonitrile-κNtrichlorido[(1,2,5,6-η-cycloocta-1,5-diene]iridium(III

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David M. Morris

2015-04-01

Full Text Available A reaction between [(CODIrCl]2 (COD is cycloocta-1,5-diene, HCl and indene failed to provide the hoped for chloridoindenyliridium dimer, but instead produced the title compound, [IrCl3(CH3CN(C8H12], which is an octahedral complex of iridium(III with a chelating cycloocta-1,5-diene ligand, three chloride ligands in a fac arrangement, and one acetonitrile ligand. Attempts to devise a rational synthesis for the title compound were unsuccessful.

1-Methyl-4-phenyl-1H-pyrazolo[3,4-d]pyrimidine

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Mohamed El Hafi

2017-09-01

Full Text Available In the crystal, molecules of the title compound, C12H10N4, stack in a head-to-tail manner along the b direction through π–π stacking interactions between both portions of the pyrazolopyrimidine ring system.

Measurement of 2J(H,C)- and 3J(H,C)-coupling constants by α/β selective HC(C)H-TOCSY

International Nuclear Information System (INIS)

Duchardt, Elke; Richter, Christian; Reif, Bernd; Glaser, Steffen J.; Engels, Joachim W.; Griesinger, Christian; Schwalbe, Harald

2001-01-01

A new heteronuclear NMR pulse sequence for the measurement of n J(C,H) coupling constants, the α/βselective HC(C)H-TOCSY, is described. It is shown that the S 3 E element (Meissner et al., 1997a,b) can be used to obtain spin state selective coherence transfer in molecules, in which adjacent CH moieties are labeled with 13 C. Application of the α/β selective HC(C)H-TOCSY to a 10nt RNA tetraloop 5'-CGCUUUUGCG-3', in which the four uridine residues are 13 C labeled in the sugar moiety, allowed measurement of two bond and three bond J(C,H) coupling constants, which provide additional restraints to characterize the sugar ring conformation of RNA in cases of conformational averaging

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.