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

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Giuseppe Daidone

2008-05-01

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

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

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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.

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.

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.

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

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Alexander Briceño

2010-03-01

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

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

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A. C. Santos

2009-11-01

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

(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

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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.

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.

Axial zero-field splitting in mononuclear Co(ii) 2-N substituted N-confused porphyrin: Co(2-NC3H5-21-Y-CH2C6H4CH3-NCTPP)Cl (Y = o, m, p) and Co(2-NC3H5-21-CH2C6H5-NCTPP)Cl.

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Lai, Ya-Yuan; Chang, Yu-Chang; Chen, Jyh-Horung; Wang, Shin-Shin; Tung, Jo-Yu

2016-03-21

The inner C-benzyl- and C-o-xylyl (or m-xylyl, p-xylyl)-substituted cobalt(ii) complexes of a 2-N-substituted N-confused porphyrin were synthesized from the reaction of 2-NC3H5NCTPPH (1) and CoCl2·6H2O in toluene (or o-xylene, m-xylene, p-xylene). The crystal structures of diamagnetic chloro(2-aza-2-allyl-5,10,15,20-tetraphenyl-21-hydrogen-21-carbaporphyrinato-N,N',N'')zinc(ii) [Zn(2-NC3H5-21-H-NCTPP)Cl; 3 ] and paramagnetic chloro(2-aza-2-allyl-5,10,15,20-tetraphenyl-21-benzyl-21-carbaporphyrinato-N,N',N'')cobalt(ii) [Co(2-NC3H5-21-CH2C6H5NCTPP)Cl; 7], and chloro(2-aza-2-allyl-5,10,15,20-tetraphenyl-21-Y-xylyl-21-carbaporphyrinato-N,N',N'')cobalt(ii) [Co(2-NC3H5-21-Y-CH2C6H4CH3NCTPP)Cl] [Y = o (8), m (9), p (10)] were determined. The coordination sphere around the Zn(2+) (or Co(2+)) ion in 3 (or 7-10) is a distorted tetrahedron (DT). The free energy of activation at the coalescence temperature Tc for the exchange of phenyl ortho protons o-H (26) with o-H (22) in 3 in a CDCl3 solvent is found to be ΔG = 61.4 kJ mol(-1) through (1)H NMR temperature-dependent measurements. The axial zero-field splitting parameter |D| was found to vary from 35.6 cm(-1) in 7 (or 30.7 cm(-1) in 8) to 42.0 cm(-1) in 9 and 46.9 cm(-1) in 10 through paramagnetic susceptibility measurements. The magnitude of |D| can be related to the coordination sphere at the cobalt sites.

Antimicrobial and antifungal activity of 2-(1H-tetrazolo-5-ylanilines and products of their structural modifications

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O. M. Antypenko

2016-08-01

Full Text Available Virtually any molecule of antibiotic can be inactivated in the microbial cell by particular resistance mechanism. In this regard, each antibiotic effectiveness starts to decrease, which necessitates the synthesis of new antimicrobial agents. Aim. To examine the previously synthesized substituted 2-(1H-tetrazolo-5-ylanilines and products of their structural modification for antimicrobial and antifungal activity. Materials and methods. The study of biological activity was conducted by disco-diffusion method on Mueller-Hinton agar on these strains of microorganisms: Gram-positive cocci (Staphylococcus aureus ATCC 25923, Enterococcus aeruginosa, E. faecalis ATCC 29212, Gram-negative bacteria (Pseudomonas aeruginosa PSS27853, Escherichia coli ATCC 25922, facultative anaerobic gram-negative bacteria (Klebsiella pneumonia and fungi (Candida albicans ATCC 885653. Results. The studies showed, that the antifungal activity was characteristic only for S-substituted of tetrazolo[1,5-c]quinazoline-(6H-5-ones(thiones. The growth of gram-positive cocci Staphylococcus aureus and Enterococcus faecalis, more effectively detained 5-(N,N-dialkylaminoethylthio-tetrazolo[1,5-c]quinazolines (4.4-4.6. 1-(2- (1H-tetrazolo-5-yl-R1-phenyl-3-R2-phenyl(ethylureas (2.1-2.31 were more selective against Staphylococcus aureus and Enterococcus faecalis. Analysis of «structure-activity relationship» showed, that the introduction of halogen to the aniline fragment leads to increase of activity. Thus, the compound 2.3 with fluorine stopped the growth of Escherichia coli and Klebsiella pneumonia for 31 mm and 21 mm, respectively. Structures with chlorine (2.4 and bromine (2.5 stopped the growth of Pseudomonas aeruginosa at 20 mm and 23 mm, respectively. And the presence of trifluoromethyl group in the phenylureide fragment and chlorine in aniline fragment of compound 2.27 led to the highest growth delay zone 25 mm. Among the investigated compounds only 1-(4-methoxyphenyl-2

A new class of anticonvulsants possessing 6 Hz psychomotor seizure test activity: 2-(1H-benzotriazol-1-yl)-N'-[substituted] acetohydrazides.

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Kumar, Praveen; Tripathi, Laxmi

2012-05-01

A series of 2-(1H-Benzotriazol-1-yl)-N'-[substituted]acetohydrazides were designed & synthesized keeping in view the structural requirement of pharmacophore and evaluated for anticonvulsant activity and neurotoxicity. The new compounds were characterized using FT-IR, 1H NMR, mass spectral data and elemental analysis. The anticonvulsant activity of the titled compounds was assessed using the 6 Hz psychomotor seizure test. The neurotoxicity was assessed using the rotorod method. The most active compound of the series was N'-[4-(1,3-Benzodioxol-5-yloxy)benzylidene]-2-(1H-benzotriazol-1-yl)acetohydrazide (BTA 9), which showed good activity with 75 % protection (3/4, 0.5 h) at a dose of 100 mg/kg in mice. All the compounds exhibited no neurotoxicity. A computational study was carried out for calculation of pharmacophore pattern and prediction of pharmacokinetic properties. Titled compounds have also exhibited good binding properties with epilepsy molecular targets such as glutamate, GABA (A) delta, GABA (A) alpha-1 receptors and Na/H exchanger, in Lamarckian genetic algorithm based flexible docking studies.

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.

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

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Hoong-Kun Fun

2011-02-01

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

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

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Jan Světlík

2009-05-01

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

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.

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.

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

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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)

Formation of C21 bile acids from plant sterols in the rat

International Nuclear Information System (INIS)

Boberg, K.M.; Lund, E.; Olund, J.; Bjoerkhem, I.

1990-01-01

Formation of bile acids from sitosterol in bile-fistulated female Wistar rats was studied with use of 4-14C-labeled sitosterol and sitosterol labeled with 3H in specific positions. The major part (about 75%) of the 14C radioactivity recovered as bile acids in bile after intravenous administration of [4-14C]sitosterol was found to be considerably more polar than cholic acid, and only trace amounts of radioactivity had chromatographic properties similar to those of cholic acid and chenodeoxycholic acid. It was shown that polar metabolites were formed by intermediate oxidation of the 3 beta-hydroxyl group (loss of 3H from 3 alpha-3H-labeled sitosterol) and that the most polar fraction did not contain a hydroxyl group at C7 (retention of 3H in 7 alpha,7 beta-3H2-labeled sitosterol). Furthermore, the polar metabolites had lost at least the terminal 6 or 7 carbon atoms of the side chain (loss of 3H from 22,23-3H2- and 24,28-3H2-labeled sitosterol). Experiments with 3H-labeled 7 alpha-hydroxysitosterol and 4-14C-labeled 26-hydroxysitosterol showed that none of these compounds was an efficient precursor to the polar metabolites. By analysis of purified most polar products of [4-14C] sitosterol by radio-gas chromatography and the same products of 7 alpha,7 beta-[2H2]sitosterol by combined gas chromatography-mass spectrometry, two major metabolites could be identified as C21 bile acids. One metabolite had three hydroxyl groups (3 alpha, 15, and unknown), and one had two hydroxyl groups (3 alpha, 15) and one keto group. Considerably less C21 bile acids were formed from [4-14C]sitosterol in male than in female Wistar rats. The C21 bile acids formed in male rats did not contain a 15-hydroxyl group. Conversion of a [4-14C]sitosterol into C21 bile acids did also occur in adrenalectomized and ovariectomized rats, indicating that endocrine tissues are not involved

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

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

2005-02-08

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

cis-Aquadichlorido[pyrimidin-2(1H-one-κN3]copper(II

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A. Guy Orpen

2008-07-01

Full Text Available In the title compound, [CuCl2(C4H4N2O(H2O], the CuII cation is coordinated by two chloride anions, one pyrimidin-2-one N atom and one water molecule, giving a slightly distorted square-planar geometry. In the crystal structure, the pyrimidin-2-one rings stack along the b axis, with an interplanar distance of 3.306 Å, as do the copper coordination planes (interplanar spacing = 2.998 Å. The coordination around the Jahn–Teller-distorted CuII ion is completed by long Cu...O [3.014 (5 Å] and Cu...Cl [3.0194 (15 Å] interactions with adjacent molecules involved in this stacking. Several N—H...Cl, O—H...Cl and O—H...O intermolecular hydrogen bonds form a polar three-dimensional network.

[4,6-Dimethyl­pyrimidine-2(1H)-thione-κS]iodidobis(triphenyl­phosphane-κP)copper(I)

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Pakawatchai, Chaveng; Wattanakanjana, Yupa; Choto, Patcharanan; Nimthong, Ruthairat

2012-01-01

In the mononuclear title complex, [CuI(C6H8N2S)(C18H15P)2], the CuI ion is in a slightly distorted tetra­hedral coordination geometry formed by two P atoms from two triphenyl­phosphane ligands, one S atom from a 4,6-dimethyl­pyrimidine-2(1H)-thione ligand and one iodide ion. There is an intra­molecular N—H⋯I hydrogen bond. In the crystal, π–π stacking inter­actions [centroid–centroid distance = 3.594 (1) Å] are observed. PMID:22719327

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

International Nuclear Information System (INIS)

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

1979-01-01

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

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

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Raymond Schinazi

2008-02-01

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

2-(1-Amino-4-tert-butylcyclohexylacetic acid (tBu-β3,3-Ac6c hemihydrateIIIM communication number IIIM/1552/2013.

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Naiem Ahmad Wani

2013-06-01

Full Text Available The title compound, C12H23NO2·0.5H2O, crystallized with two 2-(1-amino-4-tert-butylcyclohexylacetic acid molecules, which are present as zwitterions, and one water molecule in the asymmetric unit. The molecular structure of each zwitterion is stabilized by an intramolecular six-membered (C6 N—H...O hydrogen bond. In the crystal, the two independent zwitterions are linked head-to-head by N—H...O hydrogen bonds. Further O—H...O and N—H...O hydrogen bonds link the zwitterions and the water molecules, forming sandwich-like layers, with a hydrophilic filling and a hydrophobic exterior, lying parallel to the ab plane.

1-Benzyl-3-methylquinoxalin-2(1H-one

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Youssef Ramli

2018-03-01

Full Text Available The asymmetric unit of the title compound, C16H14N2O, contains three independent molecules differing primarily in the orientations of the benzyl groups. Each independent molecule forms inversion related dimers via offset π-stacking interactions. For two of these dimers, stacks are formed approximately along the a-axis direction by a combinations of C—H...N and C—H...π(ring contacts, in addition to the offset π-stacking interactions. The third set of dimers are also stacked in the same direction but only by pairwise C—H...N hydrogen bonds.

Aquachloridobis[5-(2-pyridyl-1H-tetrazolato-κN1]iron(III

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Bo Wang

2009-08-01

Full Text Available The title compound, [Fe(C6H4N52Cl(H2O], was synthesized by hydrothermal reaction of FeCl3 with 2-(1H-tetrazol-5-ylpyridine. The iron(III metal centre exhibits a distorted octahedral coordination geometry provided by four N atoms from two bidentate organic ligands, one water O atom and one chloride anion. The pyridine and tetrazole rings are nearly coplanar [dihedral angles = 4.32 (15 and 5.04 (14°]. In the crystal structure, intermolecular O—H...N hydrogen bonds link the complex molecules into a two-dimensional network parallel to (100.

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.

3-Chloro-4-methyl­quinolin-2(1H)-one

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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

10-Benzyl-10H-phenothiazine 9-oxide

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Zhouqing Xu

2009-08-01

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

Applications of stable isotopes of 2H, 13C and 15N to clinical problems

International Nuclear Information System (INIS)

Klein, P.D.; Szczepanik, P.A.; Hachey, D.L.

1974-01-01

The function of the Argonne Program is to provide synthetic, analytical instrumental capability in a core facility for the clinical investigator who needs to use 2 H, 13 C, or 15 N labelled compounds for metabolic or clinical research on pregnant women, newborn infants, young children, or for mass screening. To carry out such application development, there were six stages which were recurrent steps in every application. Five fundamental strategies should be adopted to establish the use of stable isotopes in clinical work. The instrument required for measurements was a combined gas chromatograph-mass spectrometer, and its use was schematically illustrated. Some of the successful experiences with compounds labelled by stable isotopes, such as deuterium labelled chenodeoxycholic acid, and respective 13 C and 15 N-labelled glycine were described. Deutrium labelled bile acid enabled easy and safe determination of the size of the bile acid pool and the replacement rate, providing clearer diagnoses for cholestatic liver disease and gallstones. 13 C and 15 N labelled compounds were used in clinical studies, of children with genetic disorders of amino acid metabolism, i.e., non ketotic hyperflycinemia, B 12 -responsive methyl malonic acidemia, and Lesch-Nyhan syndrome. 15 N-labelled glycine was also studied in a child with Lesch-Nyhan syndrome. (Mukohata, S.)

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.

2-(1H-Benzotriazol-1-yl-1-phenylethanol

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Özden Özel Güven

2010-04-01

Full Text Available In the title compound, C14H13N3O, the benzotriazole ring is oriented at a dihedral angle of 13.43 (4° with respect to the phenyl ring. In the crystal structure, intermolecular O—H...N hydrogen bonds link the molecules into chains along the b axis. Aromatic π–π contacts between benzene rings and between triazole and benzene rings [centroid–centroid distances = 3.8133 (8 and 3.7810 (8 Å, respectively], as well as a weak C—H...π interaction involving the phenyl ring, are also observed.

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

(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°.

2,5,11,14-Tetraoxa-8-azadispiro[13.4.0]nonadeca-15,17,19-triene

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Quanying Gan

2010-05-01

Full Text Available The title compound, C14H21NO4, has been synthesized from o-dihydroxybenzene by a three-step reaction. There are two chemically equal but crystallographically independent molecules in the asymmetric unit. The crystal packing is governed by C—H...O hydrogen bonds and C—H...π interactions, forming an infinite network.

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

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Hoong-Kun Fun

2010-07-01

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

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

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

2018-06-01

Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C8H12NO)·[NO3] (I), and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C8H14N4)·[ClO4]2(II), have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a = 15.7908 (7), b = 6.8032 (3), c = 8.7091 (4) Å, V = 935.60 (7) Å3 with Z = 4. Full-matrix least-squares refinement converged at R = 0.038 and wR(F2) = 0.115. Compound (II) belongs to the monoclinic system, space group P21/c with the following parameters: a = 10.798(2), b = 7.330(1), c = 21.186(2) Å, β = 120.641 (4)°, V = 1442.7 (3) Å3and Z = 4. The structure was refined to R = 0.044, wR(F2) = 0.132. In the structures of (I) and (II), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands.

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

International Nuclear Information System (INIS)

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

1996-01-01

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

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.

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.

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

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Hai-Wei Kuai

2011-11-01

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

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.

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.

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.

1-(Prop-2-en-1-yl-3-[(prop-2-en-1-yloxy]quinoxalin-2(1H-one

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Khadija El Bourakadi

2017-05-01

Full Text Available In the title compound, C14H14N2O2, the dihydroquinoxaline moiety deviates slightly from planarity. In the crystal, zigzag chains are formed by inversion-related C—H...O hydrogen bonds. Adjacent chains are associated through pairwise C—H...π(ring and π-stacking interactions.

Synthesis and NMR characterization of ( sup 15 N)taurine (2-( sup 15 N)aminoethanesulfonic acid)

Energy Technology Data Exchange (ETDEWEB)

Philippossian, G.; Welti, D.H.; Fumeaux, R.; Richli, U.; Anantharaman, K. (Nestle Research Centre, Nestec Ltd., Lausanne (Switzerland))

1989-11-01

The title compound was prepared in three steps with 55% overall yield starting from potassium ({sup 15}N)phthalimide. The synthetic route involved reaction with 1,2-dibromoethane, hydrolysis of the resulting N-(2-bromoethyl) ({sup 15}N)phthalimide with HBr and treatment of the 2-bromoethyl({sup 15}N)amine thus formed with sodium sulphite. The product was characterized by {sup 13}C, {sup 1}H and {sup 15}N NMR spectroscopy. The absolute coupling constants of {sup 15}N with the {sup 13}C nuclei and the non-exchanging protons were determined and an unambiguous assignment of the proton signals obtained. (author).

{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.

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.

1-(4-Fluorophenyl-2-(1H-1,2,4-triazol-1-ylethanone hemihydrate

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Dong-liang Liu

2011-12-01

Full Text Available In the title compound, C10H8FN3O·0.5H2O, the dihedral angle between the mean planes of the rings is 99.80 (4°. The water molecule lies on a twofold axis. Weak intermolecular O—H...N and C—H...O hydrogen bonds link one water molecule with four phenylethanone molecules, while intermolecular C—H...O hydrogen bonds involving the ketone group link phenylethanone molecules into layers parallel to (100.

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

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Hakan Kargılı

2013-02-01

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

A monoclinic polymorph of (1E,5E)-1,5-bis-(2-hy-droxy-benzyl-idene)thio-carbono-hydrazide.

Science.gov (United States)

Schmitt, Bonell; Gerber, Thomas; Hosten, Eric; Betz, Richard

2011-08-01

The title compound, C(15)H(14)N(4)O(2)S, is a derivative of thio-ureadihydrazide. In contrast to the previously reported polymorph (ortho-rhom-bic, space group Pbca, Z = 8), the current study revealed monoclinic symmetry (space group P2(1)/n, Z = 4). The mol-ecule shows non-crystallographic C(2) as well as approximate C(s) symmetry. Intra-molecular bifurcated O-H⋯(N,S) hydrogen bonds, are present. In the crystal, inter-molecular N-H⋯S hydrogen bonds and C-H⋯π contacts connect the mol-ecules into undulating chains along the b axis. The shortest centroid-centroid distance between two aromatic systems is 4.5285 (12) Å.

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.

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.

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

Science.gov (United States)

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

2015-10-05

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

Bioactive 2(1H-Pyrazinones and Diketopiperazine Alkaloids from a Tunicate-Derived Actinomycete Streptomyces sp.

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Lamiaa A. Shaala

2016-08-01

Full Text Available As a part of our ongoing effort to allocate marine microbial bioactive leads, a tunicate-derived actinomycete, Streptomyces sp. Did-27, was investigated. Three new 2(1H-pyrazinones derivatives, (S-6-(sec-butyl-3-isopropylpyrazin-2(1H-one (1, (S-3-(sec-butyl-6-isopropylpyrazin-2(1H-one (2 and (S-6-(sec-butyl-3-isobutylpyrazin-2(1H-one (3, together with the known (1H-pyrazinones analogues deoxymutaaspergillic acid (4, 3,6-diisobutyl-2(1H-pyrazinone (5 and 3,6-di-sec-butyl-2(1H-pyrazinone (6, and the diketopiperazine alkaloids cyclo(6-OH-d-Pro-l-Phe (7, bacillusamide B (8, cyclo(l-Pro-l-Leu and cyclo(l-Pro-l-Ile (10 were isolated from this strain. The structures of the compounds were determined by study of their one- and two-dimensional NMR spectra as well as high-resolution mass spectral determinations. Compound 4 was reported previously as a synthetic product, while compound 6 was reported as 2-hydroxy-3,6-di-sec-butylpyrazine. Herein, we report the complete NMR data for compounds 4 and 6. The compounds were evaluated for their cytotoxic activities against three cell lines. Compound 5 showed potent and selective activity against HCT-116 cell line with IC50 of 1.5 μg/mL, while 1–10 showed variable cytotoxic activities against these cancer cell lines. These results provide further understanding about the chemistry and bioactivities of the alkylated 2(1H-pyrazinone derivatives.

Synthesis, molecular structure, FT-IR, Raman, XRD and theoretical investigations of (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one.

Science.gov (United States)

Chidan Kumar, Chandraju Sadolalu; Fun, Hoong Kun; Parlak, Cemal; Rhyman, Lydia; Ramasami, Ponnadurai; Tursun, Mahir; Chandraju, Siddegowda; Quah, Ching Kheng

2014-11-11

A novel (2E)-1-(5-chlorothiophen-2-yl)-3-(naphthalen-2-yl)prop-2-en-1-one [C17H11ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The isomers, optimized geometrical parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of the density functional theory method, employing, the Becke-3-Lee-Yang-Parr functional and the 6-311+G(3df,p) basis set. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the monoclinic space group P2₁/c with the unit cell parameters a=5.7827(8)Å, b=14.590(2)Å, c=16.138(2)Å and β=89.987 (°). The CC bond of the central enone group adopts an E configuration. There is a good agreement between the theoretically predicted structural parameters and vibrational frequencies and those obtained experimentally. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

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

Institute of Scientific and Technical Information of China (English)

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

2011-01-01

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

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.

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.

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

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Ankur Trigunait

2010-08-01

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

Crystal structures of salen-type ligands 2-[(1E-({1-(3-chlorophenyl-2-[(E-(2-hydroxybenzylideneamino]propyl}iminomethyl]phenol and 2-[(1E-({1-(4-chlorophenyl-2-[(E-(2-hydroxybenzylideneamino]propyl}iminomethyl]phenol

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A. Gayathri

2017-12-01

Full Text Available The title compounds, C23H21ClN2O2, differ from each other only by the position of the Cl atom on the corresponding benzene ring: meta relative to the central sp3 C atom for (I and para for (II. In (I, the hydroxyphenyl rings are almost parallel, the dihedral angle between the mean planes being 9.2 (2°, but in (II, the relative position of the ring is different, characterized by a dihedral angle of 48.5 (1°. Compound (I features intramolecular O—H...N and intermolecular C—H...O hydrogen bonds, while in (II, intramolecular O—H...N, C—H...N hydrogen bonds and weak intermolecular C—H...π interactions are observed. Compound (I was refined as an inversion twin.

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

International Nuclear Information System (INIS)

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

1979-01-01

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

Preventing Out-of-Sequence for Multicast Input-Queued Space-Memory-Memory Clos-Network

DEFF Research Database (Denmark)

Yu, Hao; Ruepp, Sarah Renée; Berger, Michael Stübert

2011-01-01

This paper proposes an out-of-sequence (OOS) preventative cell dispatching algorithm, the multicast flow-based round robin (MFRR), for multicast input-queued space-memory-memory (IQ-SMM) Clos-network architecture. Independently treating each incoming cell, such as the desynchronized static round...

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

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S. Smaoui

2018-02-01

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

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.

1,3-Bis(4-bromophenylpropane

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Andrew J. Peloquin

2018-04-01

Full Text Available The title compound, C15H14Br2, obtained through the reduction of 4,4′-dibromochalcone, has monoclinic P21 symmetry at 100 K. No directional interactions could be identified in the crystal.

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

Science.gov (United States)

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

2015-03-21

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

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

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Bing Hong

2011-04-01

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

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°.

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.

15,17-Di-2-propenylcalix[4]arene-25,26,27,28-tetrol: self-complexation and C-H...O interactions

NARCIS (Netherlands)

Harkema, Sybolt; van Loon, Jan-Dirk; van Loon, Jan-Dirk; Verboom, Willem; Reinhoudt, David

1998-01-01

The crystal structure of 15,17-di-2-propenylcalix[4]arene-25,26,27,28-tetrol [systematic name: 15,17-di-2-propenylpentacyclo[19.3.1.13,7.19,13.115,19]octacosa-1(25), 3,5,7(26),9,11,13 (27),15,17,19 (28),21,23-dodecaene-25,26,27,28-tetrol], C34H32O4, was determined. The calix[4]arene molecule shows a

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.

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.

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.

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

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Imtiaz Khan

2012-07-01

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

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

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Xuan Liu

2011-08-01

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

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.

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.

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

Code of Federal Regulations Title 21

Data.gov (United States)

U.S. Department of Health & Human Services — This database contains the most recent revision from the Government Printing Office (GPO) of the Code of Federal Regulations (CFR) Title 21 - Food and Drugs.

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.

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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

DEFF Research Database (Denmark)

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

2003-01-01

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

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

International Nuclear Information System (INIS)

Jagannatha Swamy, S.

2002-01-01

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

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

Science.gov (United States)

Inamoto, Kiyofumi

2013-01-01

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

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.

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

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Zheng Tang

2009-04-01

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

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.

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)

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

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

OpenAIRE

Xu, Sheng-Zhen

2007-01-01

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

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

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N. Sureshbabu

2013-11-01

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

(4Z-1-Dodecyl-4-(2-oxopropylidene-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one

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Jihad Sebhaoui

2016-11-01

Full Text Available In the title compound, C24H36N2O2, the orientation of the 2-oxopropylidene substituent is determined by the formation of an intramolecular N—H...O hydrogen bond. The benzodiazepine seven-membered ring adopts a slightly twisted boat conformation. The molecules pack in a bilayer fashion with the dodecyl chains intercalated to form the inner portion, and the benzodiazepine moieties on the outer surfaces.

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.

Out-of-Sequence Preventative Cell Dispatching for Multicast Input-Queued Space-Memory-Memory Clos-Network

DEFF Research Database (Denmark)

Yu, Hao; Ruepp, Sarah Renée; Berger, Michael Stübert

2011-01-01

This paper proposes two out-of-sequence (OOS) preventative cell dispatching algorithms for the multicast input-queued space-memory-memory (IQ-SMM) Clos-network switch architecture, i.e. the multicast flow-based DSRR (MF-DSRR) and the multicast flow-based round-robin (MFRR). Treating each cell...

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

International Nuclear Information System (INIS)

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

2012-01-01

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

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

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Mohd Mustaqim Rosli

2012-05-01

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

A monoclinic polymorph of (1E,5E)-1,5-bis­(2-hy­droxy­benzyl­idene)thio­carbono­hydrazide

Science.gov (United States)

Schmitt, Bonell; Gerber, Thomas; Hosten, Eric; Betz, Richard

2011-01-01

The title compound, C15H14N4O2S, is a derivative of thio­ureadihydrazide. In contrast to the previously reported polymorph (ortho­rhom­bic, space group Pbca, Z = 8), the current study revealed monoclinic symmetry (space group P21/n, Z = 4). The mol­ecule shows non-crystallographic C 2 as well as approximate C s symmetry. Intra­molecular bifurcated O—H⋯(N,S) hydrogen bonds, are present. In the crystal, inter­molecular N—H⋯S hydrogen bonds and C—H⋯π contacts connect the mol­ecules into undulating chains along the b axis. The shortest centroid–centroid distance between two aromatic systems is 4.5285 (12) Å. PMID:22091213

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.

Heat-capacity analysis of a large number of A15-type compounds

International Nuclear Information System (INIS)

Junod, A.; Jarlborg, T.; Muller, J.

1983-01-01

We analyze the low- and medium-temperature specific heat of 25 samples based on eleven A15 binary compounds, with T/sub c/'s ranging from less than 0.015 to 18 K. Experimentally determined ''moments'' of the phonon spectra (omega-bar,omega-bar 2 ,#betta#/sub log/) are included in the analysis. Values are tabulated for T-bar/sub c/, 2 , eta, 2 >, N/sub bs/(E/sub F/), Momega-bar 2 2 , H/sub c/(0), and 2δ(0)/k/sub B/T/sub c/. We note the following: (i) The Debye temperature is generally a bad estimate of #betta#/sub log/. (ii) lambda is governed mainly by the ''electronic parameter'' eta; lambda = 0.175eta(eV/A 2 ) +- 0.2 for all A15 compounds studied. (iii) eta is proportional to the density of states at the Fermi level and this density of states agrees well with band-structure calculations of Jarlborg in Nb-based compounds. In V-based compounds, the observed bad correlation may reflect the presence of spin fluctuations. (iv) The values for the reduced gap 2δ(0)/k/sub B/T/sub c/ range from 3.4 to 4.9 and they are correlated with T/sub c//#betta#/sub log/

Application of unsymmetrical indirect covariance NMR methods to the computation of the (13)C (15)N HSQC-IMPEACH and (13)C (15)N HMBC-IMPEACH correlation spectra.

Science.gov (United States)

Martin, Gary E; Hilton, Bruce D; Irish, Patrick A; Blinov, Kirill A; Williams, Antony J

2007-10-01

Utilization of long-range (1)H--(15)N heteronuclear chemical shift correlation has continually grown in importance since the first applications were reported in 1995. More recently, indirect covariance NMR methods have been introduced followed by the development of unsymmetrical indirect covariance processing methods. The latter technique has been shown to allow the calculation of hyphenated 2D NMR data matrices from more readily acquired nonhyphenated 2D NMR spectra. We recently reported the use of unsymmetrical indirect covariance processing to combine (1)H--(13)C GHSQC and (1)H--(15)N GHMBC long-range spectra to yield a (13)C--(15)N HSQC-HMBC chemical shift correlation spectrum that could not be acquired in a reasonable period of time without resorting to (15)N-labeled molecules. We now report the unsymmetrical indirect covariance processing of (1)H--(13)C GHMBC and (1)H--(15)N IMPEACH spectra to afford a (13)C--(15)N HMBC-IMPEACH spectrum that has the potential to span as many as six to eight bonds. Correlations for carbon resonances long-range coupled to a protonated carbon in the (1)H--(13)C HMBC spectrum are transferred via the long-range (1)H--(15)N coupling pathway in the (1)H--(15)N IMPEACH spectrum to afford a much broader range of correlation possibilities in the (13)C--(15)N HMBC-IMPEACH correlation spectrum. The indole alkaloid vincamine is used as a model compound to illustrate the application of the method. (c) 2007 John Wiley & Sons, Ltd.

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.

(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.

(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.

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].

A facile route towards the synthesis of 2-(1H-indol-3-yl)-acetamides using 1,1-carbonyldiimidazole

International Nuclear Information System (INIS)

Kanwal, F.; Khan, K.M.; Fatima, B.; Bano, B.; Salar, U.

2016-01-01

A base-catalyzed one pot reaction has been developed for the synthesis of 2-(1H-indol-3-yl)-acetamides via coupling of 1,1-carbonyldiimidazole with 2-(1H-indol-3-yl) acetic acid resulting in the formation of a reactive intermediate which on treatment with different substituted anilines afford 2-(1H-indol-3-yl)-acetamides in good yield. The use of base along with coupling reagent eases the formation of intermediate in minimum time. All the synthetic compounds were obtained in good to moderate yields, the use of various substituted anilines effects the yields of the products. Compounds 4-30 were synthesized and the structures of all the synthetic compounds were determined by using spectroscopic techniques such as 1H-, 13C-NMR, EIMS and HRMS. (author)

3,6-Dibromo-9-(4-tert-butylbenzyl-9H-carbazole

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Duan-Lin Cao

2008-08-01

Full Text Available In the title compound, C23H21Br2N, which was synthesized by the N-alkylation of 1-tert-butyl-4-(chloromethylbenzene with 3,6-dibromo-9H-carbazole, the asymmetric unit contains two unique molecules. Each carbazole ring system is essentially planar, with mean deviations of 0.0077 and 0.0089 Å for the two molecules. The carbazole planes make dihedral angles of 78.9 (2 and 81.8 (2° with the planes of the respective benzene rings.

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}].

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

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S. Samundeeswari

2017-01-01

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

4-Allyl-6-bromo-2-phenyl-4H-imidazo[4,5-b]pyridine monohydrate

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Younès Ouzidan

2010-08-01

Full Text Available In the molecule of the title compound, C15H12BrN3·H2O, the phenyl ring is coplanar with the imidazopyridine ring system [dihedral angle = 0.4 (1°]. The water molecule is disordered over two positions with occupancies of 0.58 (1 and 0.42 (1, and it is linked to the main molecule via an O—H...N hydrogen bond.

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

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Jasim Alshawi

2016-01-01

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

Crystal structure of cis-1-phenyl-8-(pyridin-2-ylmethyldibenzo[1,2-c:2,1-h]-2,14-dioxa-8-aza-1-borabicyclo[4.4.0]deca-3,8-diene

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Gabriela Ledesma

2017-12-01

Full Text Available The title compound, C26H23BN2O2, was obtained as by product during synthetic attempts of a complexation reaction between the tripodal ligand H2L [N,N-bis(2-hydroxybenzyl(pyridin-2-ylmethylamine] and manganese(III acetate in the presence of NaBPh4. The isolated B-phenyl dioxazaborocine contains an N→B dative bond with a cis conformation. In the crystal, C—H...O hydrogen bonds define chains parallel to the b-axis direction. A comparative analysis with other structurally related derivatives is also included, together with a rationalization of the unexpected production of this zwitterionic heterocycle.

α-Tris(2,4-pentanedionato-κ2O,O')cobalt(III) at 240, 210, 180, 150 and 110 K

NARCIS (Netherlands)

von Chrzanowski, L.S.; Lutz, M.; Spek, A.L.

2007-01-01

The crystal structure of the title compound, [Co(C5H7O2)3], has been investigated by a multi-temperature measurement. In contrast to the isomorphous Al compound, the title compound exists in the studied temperature range as its monoclinic α polymorph (space group P21/c) and does not undergo a phase

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.

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

OpenAIRE

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

2009-01-01

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

Phenazine–naphthalene-1,5-diamine–water (1/1/2

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Maria Gdaniec

2009-12-01

Full Text Available The asymmetric unit of the title compound, C12H8N2·C10H10N2·2H2O, contains one half-molecule of phenazine, one half-molecule of naphthalene-1,5-diamine and one water molecule. The phenazine and naphthalene-1,5-diamine molecules are located on inversion centers. The water molecules serve as bridges between the naphthalene-1,5-diamine molecules and also between the naphthalene-1,5-diamine and phenazine molecules. The naphthalene-1,5-diamine and water molecules are connected via N—H...O and O—H...N hydrogen bonds, forming a T4(2 motif. They are arranged into a two-dimensional polymeric structure parallel to (10overline{1} in which the water molecule is a single donor and a double acceptor, whereas the amino group is a double donor and a single acceptor in the hydrogen bonding. These two-dimensional assemblies alternate with the layers of phenazine molecules arranged into a herringbone motif. Each phenazine molecule is hydrogen bonded to two water molecules and thus a three-dimensional framework of hydrogen-bonded molecules is generated.

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.

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

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Hong-Mei Wang

2009-12-01

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

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.

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

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Chi-Heon Lee

2016-12-01

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

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.)

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

Science.gov (United States)

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

2017-04-07

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

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

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Yaghoub Sarrafi

2008-08-01

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

Debye classes in A15 compounds

International Nuclear Information System (INIS)

Staudenmann, J.; DeFacio, B.; Testardi, L.R.; Werner, S.A.; Fluekiger, R.; Muller, J.

1981-01-01

The comparison between electron charge-density distribution of V 3 Si, Cr 3 Si, and V 3 Ge at room temperature leads us to study the Debye temperatures at 0 0 K THETA 0 from specific-heat measurements for over 100 A15 compounds. A phenomenological THETA 0 (M), M the molecular mass, is obtained from the static scaling relation THETA 0 (M) = aM/sup b/ and this organizes all of the data into five Debye classes: V(V 3 Si), V-G, G(V 3 Ge), G-C, and C(Cr 3 Si). In contrast, the Debye temperature THETA 0 (V), with V as the unit-cell volume does not relate alloys as THETA 0 (M) does, with the exception of the C class. This latter case leads to the surprising result MproportionalV/sup approximately1/3/ and to a Grueneisen constant of 1.6 +- 0.1 for all compounds of this class. In the V class where V 3 Si and Nb 3 Sn are found, THETA 0 (V) labels these two alloys differently, as does their martensitic c/a ratios. With T-bar/sub c/ denoting the average superconducting transition temperature within a Debye class, interesting correlations are shown. One is the maximum of T-bar/sub c/ which exists in the V class where the strongest anharmonicity occurs. Another is the case of compounds formed only by transition elements up to and including Au. This interesting case shows that approx.3.2< T-bar/sub c/< approx.5.0 K in all of the five classes and that there is no correlation between T/sub c/ and the thermal properties. The implications of these observations for creating better models for the A15 compounds are briefly discussed

trans-Carbonylchloridobis(tri-p-tolylphosphinerhodium(I acetone solvate

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Brian R. James

2008-03-01

Full Text Available The title compound, [RhCl(C21H21P2(CO]·C3H6O, was precipitated in trace yield from a reaction of RhCl(cod(THP with P(p-tol3 in a 1:1 acetone-d6/CD3OD solution under a hydrogen atmosphere [p-tol = p-tolyl, THP = tris(hydroxymethylphosphine, P(CH2OH3, and cod = 1,5-cyclooctadiene]. The complex displays a square-planar geometry around the RhI atom. The complex molecules and the acetone molecules are linked into a chain along the a axis by intermolecular C—H...Cl and C—H...O hydrogen bonds.

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.

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

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Al-Wahaibi Lamya H.

2018-02-01

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

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.

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

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Sibi Narayanan

2012-12-01

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

7-Hydroxy-8-isopropyl-1,1,4a-trimethyl-4a,9,10,10a-tetrahydro-phenanthren-2(1H-one

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Ahmed Benharref

2011-04-01

Full Text Available The title compound, C20H26O2, was isolated from a chloroform extract of Tetraclinis articulata wood. The molecule contains three fused rings which exhibit different conformations. The non-aromatic oxo-substituted ring has a screw-boat conformation, while the central ring has a half-chair conformation. In the crystal, molecules are linked to each other by intermolecular O—H...O hydrogen bonds involving the carbonyl and hydroxy groups.

(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

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

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Michal Dušek

2010-10-01

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

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

Science.gov (United States)

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

2009-07-01

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

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

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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 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

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

Science.gov (United States)

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

2015-12-18

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

Assessment of off-stoichiometric Zr33-xFe52+xSi15 C14 Laves phase compounds as permanent magnet materials

Science.gov (United States)

Gabay, A. M.; Hadjipanayis, G. C.

2018-05-01

Recently, Fe-based rare-earth-free compounds with non-cubic crystal structures were proposed as a base for permanent magnets which would not rely on critical elements. In this work, two series of alloys, Zr27Fe73-wSiw (0 ≤ w ≤ 15) and Zr33-xFe52+xSi15 (0 ≤ x ≤ 11), were prepared and characterized after annealing at 1538 K in order to determine the fundamental magnetic properties of the C36 and C14 hexagonal Laves phase compounds. A mixture of the cubic C15 and Zr6Fe23 structures was observed instead of the expected C36 structure. The hexagonal C14 was found in all Zr33-xFe52+xSi15 alloys with its lattice parameters linearly decreasing as the Fe(Si) atoms occupy the Zr sites in the Laves phase crystal structure. The solubility limit of Fe in the C14 structure at 1538 K corresponds to x = 9.5. The Curie temperature of the C14 compounds increases with deviation from the Laves phase stoichiometry from 290 K to 530 K. The room-temperature spontaneous magnetization also increases reaching, after correcting for the non-magnetic impurities, a value of 6.7 kG. The magnetocrystalline anisotropy of the off-stoichiometric C14 Laves phase was found to be uniaxial with the easy magnetization direction parallel to the hexagonal axis. Unfortunately, the anisotropy field, which does not exceed 10 kOe, is not sufficiently high to make the compounds interesting as permanent magnet materials.

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

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Najat Abbassi

2013-04-01

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

(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.

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

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Lin Li

2008-01-01

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

(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.

(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.

pH-dependent equilibrium isotope fractionation associated with the compound specific nitrogen and carbon isotope analysis of substituted anilines by SPME-GC/IRMS.

Science.gov (United States)

Skarpeli-Liati, Marita; Turgeon, Aurora; Garr, Ashley N; Arnold, William A; Cramer, Christopher J; Hofstetter, Thomas B

2011-03-01

Solid-phase microextraction (SPME) coupled to gas chromatography/isotope ratio mass spectrometry (GC/IRMS) was used to elucidate the effects of N-atom protonation on the analysis of N and C isotope signatures of selected aromatic amines. Precise and accurate isotope ratios were measured using polydimethylsiloxane/divinylbenzene (PDMS/DVB) as the SPME fiber material at solution pH-values that exceeded the pK(a) of the substituted aniline's conjugate acid by two pH-units. Deviations of δ(15)N and δ(13)C-values from reference measurements by elemental analyzer IRMS were small (IRMS. Under these conditions, the detection limits for accurate isotope ratio measurements were between 0.64 and 2.1 mg L(-1) for δ(15)N and between 0.13 and 0.54 mg L(-1) for δ(13)C, respectively. Substantial inverse N isotope fractionation was observed by SPME-GC/IRMS as the fraction of protonated species increased with decreasing pH leading to deviations of -20‰ while the corresponding δ(13)C-values were largely invariant. From isotope ratio analysis at different solution pHs and theoretical calculations by density functional theory, we derived equilibrium isotope effects, EIEs, pertinent to aromatic amine protonation of 0.980 and 1.001 for N and C, respectively, which were very similar for all compounds investigated. Our work shows that N-atom protonation can compromise accurate compound-specific N isotope analysis of aromatic amines.

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.

2-(1-Adamantyl-1-(3-aminophenylethanol

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Michal Rouchal

2011-09-01

Full Text Available In the crystal structure of the title compound, C18H25NO, molecules are linked via O—H...N hydrogen bonds, forming chains parallel to the c axis. Additional weak N—H...O interactions stabilize the crystal packing. The adamantane cage consists of three fused cyclohexane rings in almost ideal chair conformations, with C—C—C angles in the range 107.9 (10–111.3 (11°.

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.

48 CFR 32.503-15 - Application of Government title terms.

Science.gov (United States)

2010-10-01

... Application of Government title terms. (a) Property to which the Government obtains title by operation of the... Property; and (2) The termination clauses at 52.249, for termination inventory. (c) The contractor may sell... the scrap disposition. (d) When the title to materials or other inventories is vested in the...

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.

N,N′-Bis(4-bromophenyl-N,N′-dimethylurea

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Alexandre Pocinho

2018-02-01

Full Text Available The structure of the title compound, C15H14Br2N2O, at 180 K has monoclinic (P21/n symmetry. It was obtained unexpectedly from the decomposition of the parent 4-bromo-N-tert-butoxycarbonyl-N-methyl-aniline. It exhibits an `endo' conformation with angles between the two aromatic rings slightly lower than the average values found for similar compounds on the Cambridge Structural Database. In the crystal, C—H...O hydrogen bonds and short Br...Br halogen bonds [3.444 (1 Å] are observed.

Synthesis of organic compounds 15 N enriched

International Nuclear Information System (INIS)

Oliveira, Claudineia Raquel de; Bendassolli, Jose Albertino; Prestes, Clelber Vieira; Tavares, Glauco Arnold

2002-01-01

The aim of this work was to develop urea- 15 N and glycine- 15 N synthesis for agronomic and biological studies. The production of these compounds was evaluated due to the fact of increasing use of urea, comparing to others solid fertilizers and the importance of glycine in the studies of protein metabolism. A non-conventional method was carried out to synthesize urea. The process involved reaction among Co, NH 3 anidrid and S at low temperature (100 deg C) and of pressure (0,81 mPa) compared to the conventional method. Monolise halets reaction was carried out for glycine synthesis with chloroacetic and ammonia 2 deg C. Both compounds are economic viable, they can be produced at a lower price than the trade market one. (author)

1H, 13C and 13N chemical shifts and 1H-15N and 13C-15N heteronuclear spin-spin coupling constants n the NMR spectra of 5-substituted furfural oximes

International Nuclear Information System (INIS)

Popelis, Yu.Yu.; Liepin'sh, E.E.; Lukevits, E.Ya.

1986-01-01

The 1 H, 13 C, and 15 N NMR spectra of 15 N-enriched 5-substituted furfural oximes were investigated. It was shown that the chemical shifts of the ring atoms and the oxime group correlate satisfactorily with the F and R substituent constants, whereas their sensitivity to the effect of the substituents is lower than in monosubstituted furan derivatives. The constants of spin-spin coupling between the ring protons and the oxime group were determined. An analysis of the 1 H- 1 H spin-spin coupling constants (SSCC) on the basis of their stereospecificity indicates that the E isomers have primarily an s-trans conformation in polar dimethyl sulfoxide, whereas the Z isomers, on the other hand, have an s-cis conformation. The signs of the direct and geminal 13 C- 15 N SSCC were determined for 5-trimethylsilylfurfural oxime

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

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Augusto Rivera

2011-09-01

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

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.

2-([1,2,4]triazolo[1,5-c]quinazolin-2-yl-alkyl-(alkaryl-, aryl--amines and their derivatives. (3Н-quinazolin-4-ylidenhydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-ylalkyl-(alkaryl-, aryl-carboxylic acids: features of synthesis, modification and ant

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Yu. V. Martynenko

2016-08-01

the synthesized compounds have never been active against St. aureus, E. aerogenes, P. aeruginosa, E. coli, K. pneumoniaе (growth inhibition zone 6 mm. However, compounds 2.1, 2.2 are found among the (3H-quinazoline-4-ylidenehydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl-alkyl-(aralkyl-, aryl-carboxylic acids (2.1–2.9 and inhibit the growth of E. faecalis zone 7 mm. Conducted cyclocondensation of 2.1–2.9 compounds does not lead to increase of antibacterial activity of corresponding [1,2,4]triazolo[1,5-c]quinazoline-2-yl-alkyl-(alkaryl-, aryl--isoindol-1,3(2H-diones (3.1–3.9 against E. faecalis. Thus, the antibacterial effect against E. faecalis is characteristic only for compounds 3.2, 3.3 and 3.4 (growth inhibition zone 7 mm and is slightly lower than the corresponding activity of ampicillin.

The ‘sub’ metallide oxide hydrides Sr{sub 21}Si{sub 2}O{sub 5}H{sub 12+x} and Ba{sub 21}M{sub 2}O{sub 5}H{sub 12+x} (M = Zn, Cd, Hg, In, Tl, Si, Ge, Sn, Pb, As, Sb, Bi)

Energy Technology Data Exchange (ETDEWEB)

Jehle, Michael; Hoffmann, Anke [Institut für Anorganische und Analytische Chemie, Albert-Ludwigs-Universität Freiburg, Albertstr. 21, D-79104 Freiburg (Germany); Kohlmann, Holger [Institut für Anorganische Chemie, Universität Leipzig, Johannisallee 29, D-04103 Leipzig (Germany); Scherer, Harald [Institut für Anorganische und Analytische Chemie, Albert-Ludwigs-Universität Freiburg, Albertstr. 21, D-79104 Freiburg (Germany); Röhr, Caroline, E-mail: caroline@ruby.chemie.uni-freiburg.de [Institut für Anorganische und Analytische Chemie, Albert-Ludwigs-Universität Freiburg, Albertstr. 21, D-79104 Freiburg (Germany)

2015-02-25

Highlights: • The sub metallide oxide hydrides (Sr/Ba){sub 21}M{sub 2}O{sub 5}H{sub 12+x} were prepared for 14 M elements. • M covers a wide range of elements, from the Zn group to the pentels. • The ionic partial structure contains isolated M anions and suboxide clusters [O{sub 5}A{sub 18}]. • The H-content was determined by neutron diffraction and {sup 1}H/{sup 2}D MAS-NMR spectroscopy. • Band structure calculations support the H/D content and distribution. - Abstract: The title compounds sporting a great variety of anions M of different formal charges have been synthesized from melts of the composition A:M:O:H/D = 21:2:5:24, using BaH{sub 2}/SrH{sub 2} as hydrogen sources. All phases were characterized by means of single crystal X-ray data [cubic, space group Fd3{sup ¯}m; Sr{sub 21}Si{sub 2}O{sub 5}H{sub 12+x}: a = 1911.90(1) pm, R1 = 0.0201; for the barium phases with Zn (a = 2041.7(3) pm, R1 = 0.077), Cd (a = 2063.3(1) pm, R1 = 0.051), Hg (a = 2050.7(1) pm, R1 = 0.059), In (a = 2060.7(1) pm, R1 = 0.101), Tl (a = 2068.1(10) pm, R1 = 0.0485), Si (a = 2033.6(1) pm, R1 = 0.045), Ge (a = 2035.6(1) pm, R1 = 0.037), Sn (a = 2053.2(2) pm, R1 = 0.054), Pb (a = 2059.7(1) pm, R1 = 0.056), As (a = 2023.0(3) pm, R1 = 0.087), Sb (a = 2041.9(1) pm, R1 = 0.067) and Bi (a = 2045.9(1) pm, R1 = 0.075)]. Neutron powder diffraction data collected for the Ba silicide (both H and D compound) were refined by the Rietveld method (a = 2037.0(1), R{sub p} = 0.0173; wR{sub p} = 0.0304, R(F{sup 2}) = 0.086). The statistically occupied (H/D)(1) site 96g, which corresponds to the carbon position inSr{sub 21}Si{sub 2}O{sub 5}C{sub 6}, together with two further sparsely occupied sites (H/D)(2,3), yields the overall composition Ba{sub 21}Si{sub 2}O{sub 5}D{sub 14}. The hydrogen content, its chemical character and the distribution among the three H/D positions was evaluated by {sup 1}H/{sup 2}H MAS NMR spectroscopy for the Si, Ge and Sb compound. The crystal structure exhibits two

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

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Abdullah M. Asiri

2009-10-01

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

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

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Hoong-Kun Fun

2011-11-01

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

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.

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)

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)

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

1H, 15N and 13C NMR Assignments of Mouse Methionine Sulfoxide Reductase B2

Science.gov (United States)

Breivik, Åshild S.; Aachmann, Finn L.; Sal, Lena S.; Kim, Hwa-Young; Del Conte, Rebecca; Gladyshev, Vadim N.; Dikiy, Alexander

2011-01-01

A recombinant mouse methionine-r-sulfoxide reductase 2 (MsrB2ΔS) isotopically labeled with 15N and 15N/13C was generated. We report here the 1H, 15N and 13C NMR assignments of the reduced form of this protein. PMID:19636904

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.

36 CFR 254.15 - Title standards.

Science.gov (United States)

2010-07-01

...) Conveyances of lands from the United States are made by patent, quitclaim deed, or deed and without express or implied warranties, except as to hazardous substances pursuant to § 254.3 of this subpart. (c) Title... of the existing use(s) authorized under the terms of the grant, permit, easement, or lease. The non...

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

Densities, viscosities, and refractive indexes for {C2H5CO2(CH2)2CH3+C6H13OH+C6H6} at T=308.15 K

International Nuclear Information System (INIS)

Casas, Herminio; Garcia-Garabal, Sandra; Segade, Luisa; Cabeza, Oscar.; Franjo, Carlos; Jimenez, Eulogio

2003-01-01

In this work we present densities, kinematic viscosities, and refractive indexes of the ternary system {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 13 OH+C 6 H 6 } and the corresponding binary mixtures {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 6 }, {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 13 OH}, and {C 6 H 13 OH+C 6 H 6 }. All data have been measured at T=308.15 K and atmospheric pressure over the whole composition range. The excess molar volumes, dynamic viscosity deviations, and changes of the refractive index on mixing were calculated from experimental measurements. The results for binary mixtures were fitted to a polynomial relationship to estimate the coefficients and standard deviations. The Cibulka equation has been used to correlate the experimental values of ternary mixtures. Also, the experimental values obtained for the ternary mixture were used to test the empirical methods of Kohler, Jacob and Fitzner, Colinet, Tsao and Smith, Toop, Scatchard et al., and Hillert. These methods predict excess properties of the ternary mixtures from those of the involved binary mixtures. The results obtained for dynamic viscosities of the binary mixtures were used to test the semi-empirical relations of Grunberg-Nissan, McAllister, Auslaender, and Teja-Rice. Finally, the experimental refractive indexes were compared with the predicted results for the Lorentz-Lorenz, Gladstone-Dale, Wiener, Heller, and Arago-Biot equations. In all cases, we give the standard deviation between the experimental data and that calculated with the above named relations

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

Science.gov (United States)

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

2000-11-01

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

Crystal structure of 1-[2-(4-chlorophenyl-4,5-diphenyl-1H-imidazol-1-yl]propan-2-ol

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Shaaban K. Mohamed

2017-01-01

Full Text Available The title compound, C24H21ClN2O, crystallizes with two unique molecules in the asymmetric unit. In each molecule, the central imidazole ring is substituted at the 2-, 4- and 5-positions by benzene rings. The 2-substituted ring carries a Cl atom at the 4-position. One of the imidazole N atoms in each molecule has a propan-2-ol substituent. In the crystal, a series of O—H...N, C—H...O and C—H...Cl hydrogen bonds, augmented by several C—H...π(ring interactions, generate a three-dimensional network of molecules stacked along the a-axis direction.

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.

[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.

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.

4-Methyl-N-(1-methyl-1H-indazol-5-yl)benzene­sulfonamide

Science.gov (United States)

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

2013-01-01

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). PMID:24427093

Structures, physicochemical and cytoprotective properties of new oxidovanadium(IV) complexes -[VO(mIDA)(dmbipy)]·1.5H2O and [VO(IDA)(dmbipy)]·2H2O

Science.gov (United States)

Drzeżdżon, Joanna; Jacewicz, Dagmara; Wyrzykowski, Dariusz; Inkielewicz-Stępniak, Iwona; Sikorski, Artur; Tesmar, Aleksandra; Chmurzyński, Lech

2017-09-01

New oxidovanadium(IV) complexes with a modification of the ligand in the VO2+ coordination sphere were synthesized. [VO(mIDA)(dmbipy)]•1.5H2O and [VO(IDA)(dmbipy)]•2H2O were obtained as dark green crystals and grey-green powder, respectively (mIDA = N-methyliminodiacetic anion, IDA = iminodiacetic anion, dmbipy = 4,4‧-dimethoxy-2,2‧-dipyridyl). The crystal structure of [VO(mIDA)(dmbipy)]·1.5H2O has been determined by the X-ray diffraction method. The studies of structure of [VO(mIDA)(dmbipy)]•1.5H2O have shown that this compound occurs in the crystal as two rotational conformers. Furthermore, the stability constants of [VO(mIDA)(dmbipy)]•1.5H2O and [VO(IDA)(dmbipy)]•2H2O complexes in aqueous solutions were studied by using the potentiometric titration method and, consequently, determined using the Hyperquad2008 program. Moreover, the title complexes were investigated as antioxidant substances. The impact of the structure modification in the VO2+ complexes on the radical scavenging activity has been studied. The ability to scavenge the superoxide radical by two complexes - [VO(mIDA)(dmbipy)]·1.5H2O and [VO(IDA)(dmbipy)]·2H2O was studied by cyclic voltammetry (CV) and nitrobluetetrazolium (NBT) methods. The title complexes were also examined by the spectrophotometric method as scavengers of neutral organic radical - 1,1-diphenyl-2-picrylhydrazyl (DPPH•) and radical cation - 2,2'-azinobis-(3-ethylbenzothiazoline)-6-sulfonic acid (ABTS•+). Furthermore, the biological properties of two oxidovanadium(IV) complexes were investigated in relation to its cytoprotective properties by the MTT and LDH tests based on the hippocampal HT22 neuronal cell line during the oxidative damage induced by hydrogen peroxide. Finally, the results presented in this paper have shown that the both new oxidovanadium(IV) complexes with the 4,4‧-dimethoxy-2,2‧-dipyridyl ligand can be treated as the cytoprotective substances.

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

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Samra Rahmouni

2016-05-01

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

2-Chloroquinazolin-4(3H-one

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Dong-Lei Cao

2012-06-01

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

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

African Journals Online (AJOL)

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

Applications of stable isotopes of /sup 2/H, /sup 13/C and /sup 15/N to clinical problems. Experience of a collaborative program at Argonne National Laboratory

Energy Technology Data Exchange (ETDEWEB)

Klein, P D; Szczepanik, P A; Hachey, D L [Argonne National Lab., Evanston, Ill. (USA)

1974-08-01

The function of the Argonne Program is to provide synthetic, analytical instrumental capability in a core facility for the clinical investigator who needs to use /sup 2/H, /sup 13/C, or /sup 15/N labelled compounds for metabolic or clinical research on pregnant women, newborn infants, young children, or for mass screening. To carry out such application development, there were six stages which were recurrent steps in every application. Five fundamental strategies should be adopted to establish the use of stable isotopes in clinical work. The instrument required for measurements was a combined gas chromatograph-mass spectrometer, and its use was schematically illustrated. Some of the successful experiences with compounds labelled by stable isotopes, such as deuterium labelled chenodeoxycholic acid, and respective /sup 13/C and /sup 15/N-labelled glycine were described. Deutrium labelled bile acid enabled easy and safe determination of the size of the bile acid pool and the replacement rate, providing clearer diagnoses for cholestatic liver disease and gallstones. /sup 13/C and /sup 15/N labelled compounds were used in clinical studies, of children with genetic disorders of amino acid metabolism, i.e., non ketotic hyperflycinemia, B/sub 12/-responsive methyl malonic acidemia, and Lesch-Nyhan syndrome. /sup 15/N-labelled glycine was also studied in a child with Lesch-Nyhan syndrome.

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°.

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.

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.

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

Science.gov (United States)

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

2016-01-05

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

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.

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.

Stereocomplexation, Thermal and Mechanical Properties of Conetworks Composed of Star-Shaped l-Lactide, d-Lactide and ε-Caprolactone Oligomers Utilizing Sugar Alcohols as Core Molecules

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Kaito Sugane

2017-11-01

Full Text Available It is important to develop tailor-made biodegradable/biocompatible polymer networks usable for biomaterials whose thermal and mechanical properties are easily controlled by changing the composition. We synthesized sugar-alcohol-based polymer networks (SPN-mscLAO/3CLO, m = 4, 5 or 6 by the crosslinking reactions of erythritol, xylitol or sorbitol-based m-armed star-shaped l-lactide and d-lactide oligomers (HmSLLAO and HmSDLAO, a glycerol-based 3-armed star-shaped ε-caprolactone oligomer (H3SCLO and hexamethylene diisocyanate (HDI at the weight ratios of HmSLLAO/HmSDLAO = 1/1 and (HmSLLAO + HmSDLAO/H3CLO = 100/0, 75/25, 50/50, 25/75 or 0/100. The influence of the arm number on the crystallization behavior, thermal and mechanical properties of SPN-mscLAO/3CLOs were systematically investigated by comparing with those of sugar-alcohol-based homochiral polymer network (SPN-mLLAO, m = 4, 5 or 6 prepared by the reaction of HmSLLAO and HDI. Stereocomplex (sc crystallites are dominantly formed for SPN-mscLAO/3CLOs 100/0–25/75, whereas SPN-mLLAOs were amorphous. The higher order of melting temperature of sc-crystals for SPN-mscLAO/3CLOs 100/0–25/75 was m = 5 > m = 6 > m = 4. The sc-crystallinities of SPN-4scLAO/3CLOs 100/0–50/50 were significantly lower than those of SPN-mscLAO/3CLOs 100/0–50/50 (m = 5 and 6. The larger order of the sc-spherulite size at crystallization temperature of 110 °C was m = 5 > m = 6 > m = 4 for SPN-mscLAO/3CLO 100/0. The size and number of sc-spherulites decreased with increasing crystallization temperature over the range of 110–140 °C and with increasing CLO fraction. Among all the networks, SPN-5scLAO/3CLOs 75/25 and 50/50 exhibited the highest and second highest tensile toughnesses (21.4 and 20.3 MJ·m−3, respectively.

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

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S. Antony Inglebert

2011-11-01

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

In Vitro Antifungal, Anticancer Activities and POM Analyses of a Novel Bioactive Schiff Base 4-(((E)-furan-2-ylmethylidene)amino)p-henol: Synthesis, Characterization and Crystal Structure

International Nuclear Information System (INIS)

Tighadouni, S.; Radi, S.; Sirajuddin, M.; Akkurt, M.; Ozdemir, N.; Mabkhot, Y. N.; Hadda, T. B.

2016-01-01

The title compound (1), C/sub 11/H/sub 9/NO/sub 2/, was synthesized and characterized by FT-IR, 1H NMR, /sup 13/C NMR spectroscopy, mass spectrometry and single crystal analysis. It was crystallized in a monoclinic system with a space group P21/n. The dihedral angle between the planes of furan and benzene ring is 21.24 (11)Degree. The torsion angle of bridge C-C-N-C is -177.81(15) Degree. The crystal structure is stabilized by intermolecular hydrogen bonds between O-H-N and C-H-O forming a three dimensional network. The synthesized compound was screened for the in vitro antifungal against the Fusarium oxysporum f.sp albedinis FAO fungal strains and showed good activity. It was also tested for the anticancer activities against breast (MDA-MB231) and colorectal (LOVO) cancer cell lines and exhibited IC50 values of 6.9 μg/mL and 14.6 μg/mL, respectively. POM calculations of molecular properties of 1 are in good agreement with the mode of antifungal action of the compound bearing (XδYδ) pharmacophore site. Also it shows a drug score of 43 percent which is an important parameter for the compound possessing the drug character. (author)

COP21: a 1.5 deg. C or 2 deg. C target?

International Nuclear Information System (INIS)

Huet, Sylvestre

2015-01-01

This article discusses and somehow criticises the definition of a limitation for temperature increase to 1.5 degree rather than 2 degree. Even though this objective is grounded on a positive motivation, notably to support countries which are the most threatened by sea level rise, the article shows that this 1.5 degree objective cannot be met, and is even about to be already reached due to the level of already emitted greenhouse gases, notably CO 2 . Then it discusses the interest of COP21 debate and agreement as it defines an unreachable objective. This leads to the observation of an insufficiency of policies expressed at the COP21, with however the merit to admit the truth: the impossibility to define a route which would allow the 2 degree limit not to be overcome, as it is shown by various data of evolution of emissions

2-(1H-Benzimidazol-2-ylphenol

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S. M. Prakash

2014-02-01

Full Text Available The title molecule, C13H10N2O, is essentially planar, the maximum deviation from the plane of the non-H atoms being 0.016 (2 Å. The imidazole ring makes a dihedral angle of 0.37 (13° with the attached benzene ring. An intramolecular O—H...N hydrogen bond generates an S(6 ring motif. In the crystal, molecules are linked through N—H...O hydrogen bonds, forming chains propagating in [001]. The crystal packing also features four π–π stacking interactions involving the imidazole ring, fused benzene ring and attached benzene ring system [centroid–centroid distances = 3.6106 (17, 3.6108 (17, 3.6666 (17 and 3.6668 (17 Å].

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

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.

Measurement of {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C residual dipolar couplings in nucleic acids from TROSY intensities

Energy Technology Data Exchange (ETDEWEB)

Ying Jinfa [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Wang Jinbu [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Grishaev, Alex [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Yu Ping; Wang Yunxing [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Bax, Ad, E-mail: bax@nih.gov [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)

2011-09-15

Analogous to the recently introduced ARTSY method for measurement of one-bond {sup 1}H-{sup 15}N residual dipolar couplings (RDCs) in large perdeuterated proteins, we introduce methods for measurement of base {sup 13}C-{sup 1}H and {sup 15}N-{sup 1}H RDCs in protonated nucleic acids. Measurements are based on quantitative analysis of intensities in {sup 1}H-{sup 15}N and {sup 13}C-{sup 1}H TROSY-HSQC spectra, and are illustrated for a 71-nucleotide adenine riboswitch. Results compare favorably with those of conventional frequency-based measurements in terms of completeness and convenience of use. The ARTSY method derives the size of the coupling from the ratio of intensities observed in two TROSY-HSQC spectra recorded with different dephasing delays, thereby minimizing potential resonance overlap problems. Precision of the RDC measurements is limited by the signal-to-noise ratio, S/N, achievable in the 2D TROSY-HSQC reference spectrum, and is approximately given by 30/(S/N) Hz for {sup 15}N-{sup 1}H and 65/(S/N) Hz for {sup 13}C-{sup 1}H. The signal-to-noise ratio of both {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C spectra greatly benefits when water magnetization during the experiments is not perturbed, such that rapid magnetization transfer from bulk water to the nucleic acid, mediated by rapid amino and hydroxyl hydrogen exchange coupled with {sup 1}H-{sup 1}H NOE transfer, allows for fast repetition of the experiment. RDCs in the mutated helix 1 of the riboswitch are compatible with nucleotide-specifically modeled, idealized A-form geometry and a static orientation relative to the helix 2/3 pair, which differs by ca 6 Degree-Sign relative to the X-ray structure of the native riboswitch.

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

International Nuclear Information System (INIS)

Ke, W.; Sun, N.B.

2013-01-01

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

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

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Daisuke Urakami

2009-10-01

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

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

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Y. Z. Guo

2013-02-01

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

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

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.

An Efficient Synthesis of 3,4-Dihydro-3-substituted-2H-naphtho[2,1-e][1,3]oxazine Derivatives Catalyzed by Zirconyl(IV) Chloride and Evaluation of its Biological Activities

Energy Technology Data Exchange (ETDEWEB)

Kategaonkar, Amol H.; Sonar, Swapnil S.; Pokalwar, Rajkumar U.; Shingate, Bapurao B.; Shingare, Murlidhar S. [Babasaheb Ambedkar Marathwada University, Maharashtra (India); Kategaonkar, Atul H. [Maharashtra Institute of Pharmacy, Maharashtra (India)

2010-06-15

An efficient and novel one-pot synthesis of new 3,4-dihydro-3-substituted-2H-naphtho[2,1-e][1,3]oxazine derivatives from 1-naphthol, various anilines and formalin at room temperature grinding is presented. The six-membered N,O-heterocyclic skeleton was constructed via zirconyl(IV) chloride promoted Mannich type reaction. In vitro antimicrobial activities of synthesized compounds have been investigated against Gram-positive Bacillus subtilis, Gram negative Escherichia coli and two fungi Candida albicans and Aspergillus niger in comparison with standard drugs. The results of preliminary bioassay indicate that some of title compounds possess significant antibacterial and antifungal activity.

Influence of day length and temperature on the content of health-related compounds in broccoli (Brassica oleracea L. var. italica).

Science.gov (United States)

Steindal, Anne Linn Hykkerud; Mølmann, Jørgen; Bengtsson, Gunnar B; Johansen, Tor J

2013-11-13

Vegetables grown at different latitudes are exposed to various temperatures and day lengths, which can affect the content of health- and sensory-related compounds in broccoli florets. A 2 × 2 factorial experiment was conducted under controlled growth conditions, with contrasting temperatures (15/9 and 21/15 °C) and day lengths (12 and 24 h), to investigate the effect on glucosinolates, vitamin C, flavonols, and soluble sugars. Aliphatic glucosinolates, quercetin, and kaempferol were at their highest levels at high temperatures combined with a 12 h day. Levels of total glucosinolates, d-glucose, and d-fructose were elevated by high temperatures. Conversely, the content of vitamin C was highest with a 12 h day length combined with 15/9 °C. Our results indicate that temperature and day length influence the contents of health-related compounds in broccoli florets in a complex way, suggesting no general superiority of any of the contrasting growth conditions.

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

Science.gov (United States)

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

2017-01-23

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

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.

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.

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.

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

NARCIS (Netherlands)

Duchateau, R; Meetsma, A; Teuben, JH

1996-01-01

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

2-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.

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

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Augusto Rivera

2011-06-01

Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, the two N atoms of the imidazolidine moiety are linked to the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. The crystal studied was a racemic mixture of RR and SS enatiomers. The cyclohexane ring adopts a chair conformation and the imidazolidine group to which it is fused has a twisted envelope conformation.

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

Science.gov (United States)

Diwaker

2014-07-01

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

C-H functionalization directed by transformable nitrogen heterocycles: synthesis of ortho-oxygenated arylnaphthalenes from arylphthalazines.

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Rastogi, Shiva K; Medellin, Derek C; Kornienko, Alexander

2014-01-21

Two protocols for oxygenation of aromatic C-H bonds ortho-positioned to the phthalazine ring were developed. The transannulation of the phthalazine ring to a naphthalene moiety by an Inverse Electron Demand Diels-Alder (IEDDA) reaction led to the synthesis of naphtho[2,1-c]chromenes, 1-(ortho-hydroxyaryl)naphthalenes and 6,7-dihydrobenzo[b]naphtho[1,2-d]oxepine. This new strategy based on the utilization of transformable nitrogen heterocycles in C-H functionalization chemistry can be potentially applicable to the synthesis of a broad range of biaryl compounds.

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.

Two new two-dimensional organically templated phosphite compounds: (C6H16N2)0.5[M(HPO3)F], M=Fe(II) and Co(II): Solvothermal synthesis, crystal structures, thermal, spectroscopic, and magnetic properties

International Nuclear Information System (INIS)

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

2005-01-01

The organically templated (C 6 H 16 N 2 ) 0.5 [M(HPO 3 )F] [M(II)=Fe (1) and Co (2)] compounds have been synthesized by using mild hydrothermal conditions under autogeneous pressure. The crystal structures have been determined from X-ray single-crystal diffraction data. The compounds are isostructural and crystallize in the C2/c monoclinic space group. The unit-cell parameters are a=5.607(1), b=21.276(4), c=11.652(1)A, β=93.74(1) deg. for the iron phase and a=5.5822(7), b=21.325(3), c=11.4910(1)A, β=93.464(9) o for the cobalt compound with Z=4. The crystal structure of these compounds consists of [M(HPO 3 )F] - anionic sheets. The layers are constructed from chains which contain [M 2 O 6 F 3 ] dimeric units linked by fluoride ions. The trans-1,4-diaminocyclohexane cations are placed in the interlayer space. The IR and Raman spectra show the bands corresponding to the phosphite oxoanion and organic dication. The Dq and Racah (B and C) parameters have been calculated from the diffuse reflectance spectra in the visible region. Dq parameter is 790cm -1 for compound (1). For phase (2) the Dq value is 725cm -1 and B and C are 930 and 4100cm -1 , respectively. The thermal evolution of the molar magnetic susceptibilities of these compounds show maxima at 20.0 and 6.0K for the iron(II) and cobalt(II) phases, respectively. These results indicate the existence of antiferromagnetic interactions in both compounds

8-{1-[(4′-Fluoro-[1,1′-biphenyl]-4-ylmethyl]piperidin-4-yl}-3,4-dihydroquinolin-2(1H-one chloroform 0.25-solvate

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Nisar Ullah

2014-02-01

Full Text Available In the asymmetric unit of the title compound, C27H27FN2O·0.25CHCl3, there are two independent molecules (A and B together with a partially disordered chloroform molecule situated about an inversion center. The conformation of the two molecules is very similar. The bridging piperidine rings each have a chair conformation while the piperidin-2-one rings of the quinoline moiety have screw-boat conformations. The benzene rings of the biphenyl moiety are inclined to one another by 26.37 (4 and 23.75 (15° in molecules A and B, respectively. The mean plane of the central piperidine ring [r.m.s. deviation = 0.241 (2 Å in both molecules A and B] is inclined to the benzene ring of the quinoline moiety by 80.06 (4 in A and 83.75 (15° in B, while it is inclined to the adjacent benzene ring of the biphenyl group by 73.623 (15 in A and 75.65 (14° in B. In the crystal, individual molecules are linked by pairs of N—H...O hydrogen bonds, forming A–A and B–B inversion dimers with R22(8 ring motifs. The dimers are stabilized by C—H...O hydrogen bonds and linked via C—H...F and C—H...N hydrogen bonds into a three-dimensional network. Several C—H...π interactions are also present.

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

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Özden Özel Güven

2014-04-01

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

Within-wing isotopic (δ2H, δ13C, δ15N variation of monarch butterflies: implications for studies of migratory origins and diet

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Hobson Keith A.

2017-02-01

Full Text Available Increasingly, stable isotope measurements are being used to assign individuals to broad geographic origins based on established relationships between animal tissues and tissue-specific isoscapes. In particular, the eastern North American population of the monarch butterfly (Danaus plexippus has been the subject of several studies using established δ2H and δ13C wingtissue isoscapes to infer natal origins of migrating and overwintering individuals. However, there has been no study investigating potential variance that can derive from subsampling different regions of the wings, especially those regions differing in pigmentation (orange versus black. Within-wing isotopic (δ2H, δ13C, δ15N variance of 40 monarch butterflies collected from natural overwinter mortality on Mexican roost sites were split evenly into two groups: unwashed samples and those washed in a 2:1 chloroform:methanol solvent. Isotopic variance in δ2H and δ13C was related to pigment (within-wing range 5‰ and 0.5‰, respectively, but not region of subsampling. This variance was reduced 3 to 4 fold through solvent washing that removed pigmented surface scales and any adhered oils. Wing δ15N was similarly influenced by pigment (range 0.3‰, but this effect was not reduced through washing. We recommend future isotopic studies of monarchs and other butterflies for migration research to use the same region for subsampling consistently and to wash samples with solvent to reduce isotopic variance related to uncontrolled variance in discrimination (δ2H, δ13C, δ15N and/or adsorbed water vapor (δ2H. These data also need to be included in description of methods.

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

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Li-Cheng Sun

2012-03-01

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

Rh(III)-Catalyzed C-H Activation of Benzoylacetonitriles and Tandem Cyclization with Diazo Compounds to Substituted Benzo[ de]chromenes.

Science.gov (United States)

Fang, Feifei; Zhang, Chunmei; Zhou, Chaofan; Li, Yazhou; Zhou, Yu; Liu, Hong

2018-04-06

Rh (III)-catalyzed C-H activation of benzoylacetonitriles in coupling with diazo compounds was developed to synthesize diversified substituted benzo[ de]chromenes via a formal (4 + 2) cycloaddition with a diazo compound and subsequent tandem (4 + 2) cycloaddition with another diazo compound. Intriguingly, synthesis of substituted benzo[ de]chromenes and their decarboxylation products could be realized by controlling the reaction conditions. These reactions have a broad range of substrates, moderate to good yields, and high regioselectivity.

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

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

2016-04-01

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

4,4′-Dibromo-2,2′-{[(3aS,7aS-2,3,3a,4,5,6,7,7a-octahydro-1H-1,3-benzimidazole-1,3-diyl]bis(methylidene}diphenol

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Augusto Rivera

2011-04-01

Full Text Available The cyclohexane ring in the title compound, C21H24Br2N2O2, adopts a chair conformation and the five-membered ring to which it is fused has a twisted envelope conformation. The asymmetric unit contains one half-molecule, which is related to the other half by a twofold rotation axis. The two N atoms of the five-membered ring are linked to the hydroxy groups by intramolecular O—H...N hydrogen bonds. In the crystal, intermolecular C—H...O and C—H...π interactions occur.

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

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Abbassi, Najat; Bassou, Oulemda; Rakib, El Mostapha; Saadi, Mohamed; El Ammari, Lahcen

2013-04-01

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

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.

Electrochemical Cobalt-Catalyzed C-H Activation.

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Sauermann, Nicolas; Meyer, Tjark H; Ackermann, Lutz

2018-06-19

Carbon-heteroatom bonds represent omnipresent structural motifs of the vast majority of functionalized materials and bioactive compounds. C-H activation has emerged as arguably the most efficient strategy to construct C-Het bonds. Despite of major advances, these C-H transformations were largely dominated by precious transition metal catalysts, in combination with stoichiometric, toxic metal oxidants. Herein, we discuss the recent evolution of cobalt-catalyzed C-H activations that enable C-Het formations with electricity as the sole sustainable oxidant until May 2018. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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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.

Relationship between C2H2 reduction, H2 evolution and 15N2 fixation in root nodules of pea (Pisum sativum)

DEFF Research Database (Denmark)

Skøt, Leif

1983-01-01

for N2 reduction, is often stated as the relative efficiency (1-H2/C2H2). This factor varied significantly (P 2 and N2, expressed as the H2/N2 ratio, was independent of plant age, however. This discrepancy and the observation......The quantitative relationship between C2H2 reduction, H2 evolution and 15N2 fixation was investigated in excised root nodules from pea plants (Pisum sativum L. cv. Bodil) grown under controlled conditions. The C2H2/N2 conversion factor varied from 3.31 to 5.12 between the 32nd and the 67th day...... after planting. After correction for H2 evolution in air, the factor (C2H2-H2)/N2 decreased to values near the theoretical value 3, or in one case to a value significantly (P 2 production but used...

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

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Najat Abbassi

2011-07-01

Full Text Available In the title compound, C19H21N3O3S, the C—SO2—NH—C torsion angle is 103.72 (11°. The almost planar indazole ring [r.m.s. deviation = 0.0202 (14 Å] is twisted away from the methylbenzene ring by 76.87 (7°. The vinyl group is disordered over two orientations with site occupancies of 0.622 (10 and 0.378 (10. The S atom has a distorted tetrahedral geometry [maximum deviation: O—S—O = 119.18 (11°]. An intramolecular C—H...O hydrogen bond occurs. In the crystal, two molecules are linked about a center of inversion by pairs of N—H...O hydrogen bonds, generating a dimer. C—H...π interactions are also observed.

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

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Oulemda Bassou

2017-02-01

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

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.

rac-6-Hydroxy-4-(4-nitrophenyl-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

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Jian-Li Zhang

2010-11-01

Full Text Available The title compound, C16H12F3N3O5S·H2O, was prepared by reaction of 4-nitrobenzaldehyde, 4,4,4-trifluoro-1-(thiophen-2-ylbutane-1,3-dione and urea. The asymmetric unit contains two independent molecules, with essentially identical geometries and conformations. The dihydropyrimidine rings adopt a half-chair conformation. The dihedral angles between the benzene ring and the thiophene ring are 54.82 (8 and 58.72 (8° in the two molecules. The molecular conformation of one of the molecules is stabilized by two intramolecular O—H...O hydrogen bonds, generating an S(6 ring. The crystal structure is stabilized by intermolecular O—H...O and N—H...O hydrogen bonds.

(E-4-Amino-N′-(2-hydroxy-5-methylbenzylidenebenzohydrazide

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Hadi Kargar

2012-07-01

Full Text Available The asymmetric unit of the title compound, C15H15N3O2, comprises two crystallographically independent molecules (A and B, each having an E conformation around the C=N bond. In each molecule, there is an intramolecular O—H...N hydrogen bond making an S(6 ring motif. The dihedral angles between the substituted phenyl rings are 17.49 (9 and 10.03 (9°. In the crystal, N—H...O hydrogen bonds link neighbouring independent molecules into infinite chains, of the type –A–B–A–B–, along the a axis, enclosing R21(7 ring motifs. The chains are linked by N—H...O hydrogen bonds and C—H...O interactions, leading to the formation of a three-dimensional network.

Antibacterial properties of 3 H-spiro[1-benzofuran-2,1'-cyclohexane] derivatives from Heliotropium filifolium.

Science.gov (United States)

Urzúa, Alejandro; Echeverría, Javier; Rezende, Marcos C; Wilkens, Marcela

2008-10-01

A re-examination of cuticular components of Heliotropium filifolium allowed the isolation of four new compounds: 3'-hydroxy-2',2',6'-trimethyl-3H-spiro[1-benzo-furan-2,1'-cyclohexane]-5-carboxylic acid(2), methyl 3'-acetyloxy-2',2',6'-trimethyl-3H-spiro[1-benzofuran-2,1'-cyclohexane]-5-carboxylate (3), methyl 3'-isopentanoyloxy-2',2',6'-trimethyl-3H-spiro[1-benzofuran-2,1'-cyclohexane]-5-carboxylate (4) and methyl 3'-benzoyloxy-2',2',6'-trimethyl-3H-spiro[1-benzofuran-2,1'-cyclohexane]-5-carboxylate (5).Compounds 2-5 were identified by their spectroscopic analogies with filifolinol (1), and their structures confirmed by chemical correlation with 1. The antimicrobial properties of the compounds were tested against Gram positive and Gram negative bacteria. Some of them proved to be active against Gram positive, but inactive against Gram negative bacteria. In searching for structure-activity relationships from the obtained MIC values, lipophilicity was shown to be an important variable.

New C sub(21) Delta sup(20) pregnanes, inhibitors of mitochondrial respiratory chain,from Indopacific octocoral Carijoa sp.

Digital Repository Service at National Institute of Oceanography (India)

Ciavatta, M.L.; Gresa, M.P.L.; Manzo, E.; Gavagnin, M.; Wahidullah, S.; Cimino, G.

, m), 1.65 (H-8, m), 1.58 (H-16b, m), 1.28 (H-15b, m), 1.24 (H 3 -19, s), 1.10 (H-9, m), 1.08 (H-7b, m), 1.07 (H-12b, m), 1.02(H-14, m), 0.67 (H 3 -18, s); 13 C NMR (75.13MHz, CDCl 3 ): d 186.5 (C-3, s), 169.0 (C-5, s), 155.9 (C-1, d), 139.3 (C-20, d...), 127.5 (C- 2, d), 123.8 (C-4, d), 114.9 (C-21, t), 55.1 (C-17, d), 54.6 (C-14, d), 52.7 (C-9, d), 43.6 (C-10 and C-13, s·2), 37.1 (C-12, t), 35.7 (C-8, d), 33.7 (C-7, t), 32.9 (C-6, t), 27.1 (C-16, t), 24.9 (C-15, t), 22.5 (C-11, t), 18.7 (C-19, q), 12...

1-[(1-Methyl-1H-imidazol-5-ylmethyl]-1H-indole-5-carbonitrile

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Josephus Jacobus de Jager

2012-12-01

Full Text Available In the title compound, C14H12N4, the dihedral angle between the indole ring system (r.m.s. deviation = 0.010 Å and the imidazole ring is 77.70 (6°. In the crystal, molecules are linked by C—H...N hydrogen bonds. One set of hydrogen bonds forms an undulating chain running parallel to the b-axis direction, while the other undulating chain is parallel to the c-axis direction. In combination, (100 sheets result.

15α,20β-Dihydroxy-6β-methoxy-6,7-seco-6,20-epoxy-1,7-olide-ent-kaur-16-ene

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Fu-Lin Yan

2010-04-01

Full Text Available The title compound, C21H30O6, a natural ent-kaurane diterpenoid, was obtained from the medicinal plant Isodon serra. The five rings in the molecule exhibit the expected cis and trans junctions. The three six-membered rings adopt chair, twist-boat and boat conformations, while two five-membered rings adopt envelope conformations. There are two molecules in the asymmetric unit, related by a non-crystallographic twofold screw axis; the main difference is in the different degrees of distortion of ring B. In the crystal, the molecules are linked by intermolecular O—H...O hydrogen bonds, forming chains along the b axis.

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

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Mao-Ping Song

2008-10-01

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

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

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Alexander E. Anderson

2010-04-01

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

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.

Other compounds isolated from Simira glaziovii and the 1H and 13C NMR chemical shift assignments of new 1-epi-castanopsol

International Nuclear Information System (INIS)

Araujo, Marcelo F. de; Vieira, Ivo J. Curcino; Braz-Filho, Raimundo; Carvalho, Mario G. de

2012-01-01

A new triterpene, 1-epi-castanopsol, besides eleven known compounds: sitosterol, stigmasterol, campesterol, lupeol, lupenone, simirane B, syringaresinol, scopoletin, isofraxidin, 6,7,8-trimethoxycoumarin and harman, were isolated from the wood of Simira glaziovii. The structures of the known compounds were defined by 1D, 2D 1 H, 13 C NMR spectra data analyses and comparison with literature data. The detailed spectral data analyses allowed the definition of the structure of the new 1-epi isomer of castanopsol and performance of 1 H and 13 C NMR chemical shift assignments. (author)

Ethyl 2-(6-bromo-2-phenyl-1H-imidazo[4,5-b]pyridin-1-ylacetate

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Mohammed Yassin Hjouji

2016-05-01

Full Text Available In the title compound, C16H14BrN3O2, the fused-ring system is essentially planar, with the largest deviation from the mean plane being 0.0216 (15 Å for the substituted N atom of the five-membered ring, the plane of which makes dihedral angles of 28.50 (7 and 77.48 (7° with the terminal phenyl ring and the ethoxycarbonylmethyl group mean planes, respectively. In the crystal, C—H...N hydrogen bonds link the molecules into inversion dimers. These combine with weak C—H...N contacts to stack the molecules into columns along the b-axis direction.

Crystal structure of 3,5-dimethoxy-2-[5-(naphthalen-1-yl-4,5-dihydro-1H-pyrazol-3-yl]phenol

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Dongsoo Koh

2015-10-01

Full Text Available In the title compound, C21H20N2O3, the planes of the benzene ring and the naphthalene ring system are inclined to one another by 70.95°, and by 4.99 (6 and 75.93 (5°, respectively, to the mean plane of the pyrazoline ring. The latter has an envelope conformation with the methine (CH C atom as the flap. There is an intramolecular O—H...N hydrogen bond that forms an S(6 ring motif. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming chains along [100]. The chains are linked via C—H...N hydrogen bonds, forming sheets parallel to the ab plane. The sheets are linked by a series of N—H...π and C—H...π interactions forming a three-dimensional structure.

2-Aminopyrimidine-3,3,3-triphenylpropanoic acid (1/1).

Science.gov (United States)

Serafin, Mateusz F; Wheeler, Kraig A

2007-11-01

The title bimolecular compound, C(4)H(5)N(3).C(21)H(18)O(2), constructed from 2-aminopyrimidine and 3,3,3-triphenylpropanoic acid, forms a tetramolecular hydrogen-bonded motif via O-H...N, N-H...O and N-H...N contacts. This aggregate organizes to give crystal-packing motifs with hydrophilic and hydrophobic regions.

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-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.

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

Science.gov (United States)

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

2017-03-01

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

4-(4-Chlorophenyl-6-hydroxy-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

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Mohammad Hossein Mosslemin

2009-06-01

Full Text Available The asymmetric unit of the title compound, C16H12ClF3N2O3S·H2O, contains two crystallographically independent organic molecules and two water molecules. The organic species are linked by an intermolecular O—H...O hydrogen bond, while the water molecules are connected to them through intermolecular O—H...N hydrogen bonds. The thiophene and phenyl rings are oriented at dihedral angles of 62.35 (4 in the first independent molecule and 60.74 (5° in the second, while the pyrimidine rings adopt twisted conformations in both molecules. Intramolecular N—H...F interactions result in the formation of two five-membered rings having envelope conformations. In the crystal structure, further intermolecular O—H...O and N—H...O hydrogen bonds link the molecules into chains.

FTIR time-series of biomass burning products (HCN, C2H6, C2H2, CH3OH, and HCOOH at Reunion Island (21° S, 55° E and comparisons with model data

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D. B. A. Jones

2012-11-01

Full Text Available Reunion Island (21° S, 55° E, situated in the Indian Ocean at about 800 km east of Madagascar, is appropriately located to monitor the outflow of biomass burning pollution from Southern Africa and Madagascar, in the case of short-lived compounds, and from other Southern Hemispheric landmasses such as South America, in the case of longer-lived species. Ground-based Fourier transform infrared (FTIR solar absorption observations are sensitive to a large number of biomass burning products. We present in this work the FTIR retrieval strategies, suitable for very humid sites such as Reunion Island, for hydrogen cyanide (HCN, ethane (C2H6, acetylene (C2H2, methanol (CH3OH, and formic acid (HCOOH. We provide their total columns time-series obtained from the measurements during August–October 2004, May–October 2007, and May 2009–December 2010. We show that biomass burning explains a large part of the observed seasonal and interannual variability of the chemical species. The correlations between the daily mean total columns of each of the species and those of CO, also measured with our FTIR spectrometer at Reunion Island, are very good from August to November (R ≥ 0.86. This allows us to derive, for that period, the following enhancement ratios with respect to CO: 0.0047, 0.0078, 0.0020, 0.012, and 0.0046 for HCN, C2H6, C2H2, CH3OH, and HCOOH, respectively. The HCN ground-based data are compared to the chemical transport model GEOS-Chem, while the data for the other species are compared to the IMAGESv2 model. We show that using the HCN/CO ratio derived from our measurements (0.0047 in GEOS-Chem reduces the underestimation of the modeled HCN columns compared with the FTIR measurements. The comparisons between IMAGESv2 and the long-lived species C2H6 and C2H2 indicate that the biomass burning emissions used in the model (from the GFED3 inventory are probably underestimated in the late September–October period for all years of measurements, and

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-01-15

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

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].

(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.

4-Methoxyphenyl 2,3,4,6-tetra-O-acetyl-1-thio-α-d-mannopyranoside

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Ludovic Drouin

2008-08-01

Full Text Available The title compound, C21H26O10S, was synthesized in a single step from mannose pentaacetate. The molecular structure confirms the α configuration of the anomeric thioaryl substituent. Spectroscopic and melting-point data obtained for the title compound are in disagreement with those previously reported, indicating the previously reported synthesis [Durette & Shen (1980. Carbohydr. Res. 81, 261–274] to be erroneous. The crystal structure is stabilized by weak intermolecular C—H...O hydrogen bonds.

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

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Joo Hwan Cha

2012-01-01

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

Structural analysis and antimicrobial activity of 2[1H]-pyrimidinethione/selenone derivatives

Science.gov (United States)

Żesławska, Ewa; Korona-Głowniak, Izabela; Szczesio, Małgorzata; Olczak, Andrzej; Żylewska, Alicja; Tejchman, Waldemar; Malm, Anna

2017-08-01

Four new crystal structures of sulfur and selenium analogues of 2[1H]-pyrimidinone derivatives were determined with the use of X-ray diffraction method. The molecular geometry and intermolecular interactions of the investigated molecules were analyzed in order to find the structural features and geometrical parameters, which can be responsible for antimicrobial activities. The influence of chalcogen substituents (sulfur and selenium) on the crystal packing was also studied. The main differences in the molecular structures exist in mutual arrangement of two aromatic rings. The intermolecular interactions in all investigated compounds are similar. Furthermore, the in vitro antibacterial and antifungal activities for these compounds were evaluated. Preliminary investigations have identified two highly potent antibacterial compounds containing selenium atom, which display selectivity towards staphylococci and micrococci. This selectivity was not observed for a control compound used as a drug, namely vancomycin. These compounds possess also good antifungal activity. This is the first report of biological activities of 2[1H]-pyrimidineselenone derivatives.

The C-terminus of H-Ras as a target for the covalent binding of reactive compounds modulating Ras-dependent pathways.

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Clara L Oeste

2011-01-01

Full Text Available Ras proteins are crucial players in differentiation and oncogenesis and constitute important drug targets. The localization and activity of Ras proteins are highly dependent on posttranslational modifications at their C-termini. In addition to an isoprenylated cysteine, H-Ras, but not other Ras proteins, possesses two cysteine residues (C181 and C184 in the C-terminal hypervariable domain that act as palmitoylation sites in cells. Cyclopentenone prostaglandins (cyPG are reactive lipidic mediators that covalently bind to H-Ras and activate H-Ras dependent pathways. Dienone cyPG, such as 15-deoxy-Δ(12,14-PGJ(2 (15d-PGJ(2 and Δ(12-PGJ(2 selectively bind to the H-Ras hypervariable domain. Here we show that these cyPG bind simultaneously C181 and C184 of H-Ras, thus potentially altering the conformational tendencies of the hypervariable domain. Based on these results, we have explored the capacity of several bifunctional cysteine reactive small molecules to bind to the hypervariable domain of H-Ras proteins. Interestingly, phenylarsine oxide (PAO, a widely used tyrosine phosphatase inhibitor, and dibromobimane, a cross-linking agent used for cysteine mapping, effectively bind H-Ras hypervariable domain. The interaction of PAO with H-Ras takes place in vitro and in cells and blocks modification of H-Ras by 15d-PGJ(2. Moreover, PAO treatment selectively alters H-Ras membrane partition and the pattern of H-Ras activation in cells, from the plasma membrane to endomembranes. These results identify H-Ras as a novel target for PAO. More importantly, these observations reveal that small molecules or reactive intermediates interacting with spatially vicinal cysteines induce intramolecular cross-linking of H-Ras C-terminus potentially contributing to the modulation of Ras-dependent pathways.

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

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Augusto Rivera

2010-04-01

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

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°.

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.

Converting a C-130 Hercules into a Compound Helicopter: A Conceptual Design Study

Science.gov (United States)

Kottapalli, Anjaney P.; Harris, Franklin D.

2010-01-01

This study presents the performance and weight changes for a Compound C-130 as compared to the Baseline C-130H Hercules, using NDARC as the primary analysis tool. First, the C-130H was modeled within NDARC, from which performance at various conditions and a parametric weight statement were generated. Then, the C-130H NDARC file was modified to represent the Compound C-130, which was then put through the same performance analysis as the C-130H. A parametric weight statement was also calculated for the Compound C-130, which allowed for comparison to the C-130H. As part of the modeling of the Compound C-130, a Rotor Design Spreadsheet was created that would allow the direct calculation of the weight of the main rotors being added. Using composite materials led to considerable weight savings for both the rotor system and the hub weights. These weight savings are reflected in the NDARC Technology Factors which were determined to be 0.71 and 0.5 for the rotor blades and the hub/hinge system, respectively. Such Technology Factors suggest that using composites for other components could drastically lighten the Operating Empty Weight of the aircraft. The weight statements show the weights for each of the components on each aircraft. It is quite evident that the Compound C-130 has a higher Operating Empty Weight due to the addition of the two main rotors and a drive system to connect each engine group on the wing tips. Upon further analysis, the main weight driver is the drive system. While the main rotor/hub/hinge weight increase is to be expected, the weight increase due to the transmission drive and gear boxes are cause for concern. Unless a method can be found of reducing the weight of the drive system, the weight penalty makes the Compound a C-130 an inefficient aircraft in terms of payload/fuel capacity. Possible solutions are either off-loading some of the power requirements through the drive system or using composite materials in the construction of the drive system

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.

3,10,14,21-Tetrakis(4-methoxyphenylpentacyclo[11.8.0.02,11.04,9.015,20]henicosa-1(21,2,4(9,5,7,10,13,15(20,16,18-decaen-12-one chloroform monosolvate

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S. Gopinath

2014-08-01

Full Text Available The asymmetric unit of the title compound, C49H36O6·CHCl3, contains half an organic molecule, the complete molecule being generated by the operation of a crystallographic twofold rotation axis, and half a highly disordered chloroform molecule. The contribution to the diffraction pattern of the latter was removed using the program SQUEEZE in PLATON [Spek (2009. Acta Cryst. D65, 148–155]; the unit-cell characteristics take into account the presence of CHCl3. The dihedral angles between the planes of the naphthalene ring system and the methoxybenzene rings are 71.05 (7 (syn to the central C=O group and 57.27 (6° (anti to the central C=O group. In the crystal, molecules are linked by C—H...O interactions, generating C(12 chains running parallel to the b axis.

Elastic constants of the C15 laves phase compound NbCr2

International Nuclear Information System (INIS)

Chu, F.; He, Y.; Thoma, D.J.; Mitchell, T.E.

1995-01-01

Elastic properties of a solid are important because they relate to various fundamental solid-state phenomena such as interatomic potentials, equations of state, and phonon spectra. Elastic properties are also linked thermodynamically with specific heat, thermal expansion, Debye temperature, and Gruneisen parameter. Most important, knowledge of elastic constants is essential for many practical applications related to the mechanical properties of a solid as well: load-deflection, thermoelastic stress, internal strain (residual stress), sound velocities, dislocation core structure, and fracture toughness. In order to understand better the physical properties and deformation behavior of the C15 compound NbCr 2 , the authors have studied its elastic properties in this paper. In Section 2, the experimental methods are described, including the preparation of the sample and the measurement of the elastic constants. In Section 3, the experimental results are presented and the implications of these experimental results are discussed. Conclusions are drawn in Section 4

Crystal structure of the Ce2Ni2Zn15 compound

International Nuclear Information System (INIS)

Opainich, I.M.; Pavlyuk, V.V.; Bodak, O.I.; Cherny, R.; Yvon, K.

1996-01-01

A structure of a new ternary compound of the composition Ce2Ni2Zn15 (sp.gr.R3-barm,a=0.9080(3) nm, c=1.3294(3) nm) was determined on single-crystal and powder specimens. The study was performed on a Philips PW1100 automatic diffractometer and a DRON-4.07 powder diffractometer. The Ce2Ni2Zn15 compound is crystallized in the Ce2Al2Co15 structure type with the aluminum positions being occupied by nickel and cobalt positions being occupied by zinc

Crystal structure of 2-cyano-N-(furan-2-ylmethyl-3-(3-nitrophenylpropanamide

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Shivanna Subhadramma

2015-08-01

Full Text Available In the title compound, C15H11N3O4, the acetamide group is inclined to the furan ring by 66.5 (1°. The dihedral angle between the furan ring and the benzene ring is 66.8 (1°. In the crystal, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(12 ring motif. The dimers are linked via two pairs of C—H...O hydrogen bonds to the same acceptor oxygen atom, enclosing R21(6 ring motifs, forming chains along the [101] direction.

Effects of stoichiometry and neutron irradiation in superconducting A-15 compounds

International Nuclear Information System (INIS)

Moehlecke, S.

1978-01-01

The A-15 (A 3 B) compounds comprise an important class of superconducting compounds. In order to gain a clearer understanding of the parameters influencing the superconductivity in these materials, several A-15 compounds have been prepared and the effects of varying stoichiometry, heat treatment, and irradiation with high energy neutrons (E > 1 MeV) on the superconducting transition temperature T/sub c/, Bragg--William order parameter S, and the lattice parameter a 0 , have been studied. The systems investigated include Nb 3 Ge, Nb 3 Al, Nb 3 Pt, Nb 3 Ir, V 3 Ga, V 3 Si and Mo 3 Os. Some of the results may be summarized as follows: 1) for Nb 3 Al, Nb 3 Pt and V 3 Ga, T/sub c/ is a strong function of composition, reaching a maximum value at the ideal stoichiometric composition of 3A: 1B, if that composition exists in the equilibrium phase diagram, 2) irradiation with high energy neutrons at temperatures of approx.150 0 C results in drastic lowering of T/sub c/ for Nb 3 Al, Nb 3 Pt and Nb 3 Ge, but not for Mo 3 Os, 3) T/sub c/ can be recovered by annealing, the recovery temperature being in the range 300-800 0 C depends on the particular compound, 4) the order parameter S, decreases with increasing neutron fluence (decreasing T/sub c/), and is also recoverable upon annealing at the appropriate temperature, 5) the lattice parameter a 0 , increases with increasing neutron fluence, and isalso restored to its original value by annealing. A simple hard sphere model is developed to calculate the dependence of a 0 on composition within the A-15 phase. Excellent agreement is obtained for the measured values in the Nb--Al, Nb--Pt and V--Ga systems. The results of both compositionally and irradiation induced disorder can be understood on the basis of site-exchange taking placee between the A and B sites in the A-15 structure

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-11-15

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

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

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Dan-Li Tian

2011-07-01

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

Synthesis of (R)-5-(Di[2,3-3H2]propylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one-([3H]U-86170) and (R)-5-([2,3-3H2]propylamino)-5,6-dihydro-4H-imidazo(4,5,1-ij) quinolin-2(1H)-one ([3H]U-91356)

International Nuclear Information System (INIS)

Moon, M.W.; Hsi, R.S.P.

1992-01-01

(R)-5-(diallylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one (12b) was prepared in 9% overall yield from 3-aminoquinoline. Reaction of 12b in ethyl acetate with tritium gas in presence of a 5% platinum on carbon catalyst afforded a mixture of (R)-5-(di[2,3- 3 H 2 ]propylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]-quinolin-2(1H)-one ([ 3 H]U-86170, 69 Ci/mmol) and (R)-5-([2,3- 3 H 2 ]-propylamino)5,6-dihydro-4H-imidazo-[4,5,1-ij]quinolin-2(1H)-one ( [ 3 H]U-91356, 34 Ci/mmol) which was separated by preparative reverse-phase chromatography. U-86170 and U-91356 are potent dopamine D2 agonists. The labelled compounds are useful for drug disposition studies. [ 3 H]U-86170 is also useful as a dopamine D2 agonist radioligand for receptor binding studies. (author)

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

OpenAIRE

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

2008-01-01

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

Affordable uniform isotope labeling with 2H, 13C and 15N in insect cells

International Nuclear Information System (INIS)

Sitarska, Agnieszka; Skora, Lukasz; Klopp, Julia; Roest, Susan; Fernández, César; Shrestha, Binesh; Gossert, Alvar D.

2015-01-01

For a wide range of proteins of high interest, the major obstacle for NMR studies is the lack of an affordable eukaryotic expression system for isotope labeling. Here, a simple and affordable protocol is presented to produce uniform labeled proteins in the most prevalent eukaryotic expression system for structural biology, namely Spodoptera frugiperda insect cells. Incorporation levels of 80 % can be achieved for 15 N and 13 C with yields comparable to expression in full media. For 2 H, 15 N and 2 H, 13 C, 15 N labeling, incorporation is only slightly lower with 75 and 73 %, respectively, and yields are typically twofold reduced. The media were optimized for isotope incorporation, reproducibility, simplicity and cost. High isotope incorporation levels for all labeling patterns are achieved by using labeled algal amino acid extracts and exploiting well-known biochemical pathways. The final formulation consists of just five commercially available components, at costs 12-fold lower than labeling media from vendors. The approach was applied to several cytosolic and secreted target proteins

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

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Ísmail Çelik

2016-10-01

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

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.

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

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Abdullah Mohamed Asiri

2009-08-01

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

Hydrothermal synthesis, structure and magnetic properties of a new three-dimensional iron arsenate [C6N4H21][FeIII3(HAsO4)6

International Nuclear Information System (INIS)

Rao, Vandavasi Koteswara; Natarajan, Srinivasan

2006-01-01

A hydrothermal reaction of a mixture of iron oxalate, arsenic pentoxide, hydrofluoric acid and triethylenetetramine (TETA) at 150deg. C for 48h gives rise to a new iron arsenate [C 6 N 4 H 21 ][Fe 3 (HAsO 4 ) 6 ], I. The structure consists of a network of FeO 6 and AsO 4 building units connected through their vertices giving rise to a new secondary building unit, SBU-5. The SBU-5 units are through their corners forming a three-dimensional structure possessing one-dimensional channels bound by 8-T atoms (T=Fe, As). The formation of SBU-5 units is noteworthy. Variable temperature magnetic studies indicate antiferromagnetic interactions between the Fe centers with T N of 21.9K. Crystal data: M=1156.36, monoclinic, space group=C2/c (no. 15), a=18.422(3)A, b=8.8527(13)A, c=16.169(2)A, β=111.592(2) o , V=2451.9(6)A 3 , Z=8, ρ calc =3.037gcm -3 , μ(Mo Kα)=9.903mm -1 , R 1 =0.0358, wR 2 =0.0763, S=1.140 for 234 parameters

Effect of L-carnitine and pyruvate on equine sperm maintained at 5 ºC and 15 ºC during 24 h: preliminary results

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Avila G

2016-12-01

Full Text Available The aim of this study was to evaluate if the addition of L-carnitine and pyruvate to two semen transport extenders (Kenney and Kenney modified by Tyrodes is able to maintain sperm parameters for 24 h at 5 ºC and 15 ºC. Semen was obtained from 3 stallions (n=3; r=2 and at time 0 and after 24 h of cooling, the following parameters evaluated: total and progressive motility (CASA, viability and acrosome status (FITC-PNA-PI, membrane function (HOS, and DNA with Toluidine Blue stain (TB and the Sperm Chromatin Dispersion assay (SCD. Each temperature was individually analyzed using a factorial design with a 5% significance level. No interactions were observed. For the moment, the Kenney extender with the addition of L-carnitine and pyruvate showed the best results for maintaining most sperm parameters for 24 h at both 5 ºC and 15 ºC.

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].

6-Hydroxymethyl-4-methoxy-2H-pyran-2-one (Opuntiol

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Muhammad Athar Abbasi

2010-01-01

Full Text Available The title compound, C7H8O4, isolated from Opuntia dillenii Haw (Cactaceae, is almost planar [maximum deviation of 0.027 (2 Å] except for the H atoms of the methylene and methyl groups. The crystal packing is stabilized by C—H...O and O—H...O intermolecular hydrogen bonds, resulting in the formation of a three-dimensional network.

(1)H, (13)C, (15)N backbone and side-chain resonance assignment of Nostoc sp. C139A variant of the heme-nitric oxide/oxygen binding (H-NOX) domain.

Science.gov (United States)

Alexandropoulos, Ioannis I; Argyriou, Aikaterini I; Marousis, Kostas D; Topouzis, Stavros; Papapetropoulos, Andreas; Spyroulias, Georgios A

2016-10-01

The H-NOX (Heme-nitric oxide/oxygen binding) domain is conserved across eukaryotes and bacteria. In human soluble guanylyl cyclase (sGC) the H-NOX domain functions as a sensor for the gaseous signaling agent nitric oxide (NO). sGC contains the heme-binding H-NOX domain at its N-terminus, which regulates the catalytic site contained within the C-terminal end of the enzyme catalyzing the conversion of GTP (guanosine 5'-triphosphate) to GMP (guanylyl monophosphate). Here, we present the backbone and side-chain assignments of the (1)H, (13)C and (15)N resonances of the 183-residue H-NOX domain from Nostoc sp. through solution NMR.

20 CFR 410.561c - Defeat the purpose of title IV.

Science.gov (United States)

2010-04-01

... 20 Employees' Benefits 2 2010-04-01 2010-04-01 false Defeat the purpose of title IV. 410.561c Section 410.561c Employees' Benefits SOCIAL SECURITY ADMINISTRATION FEDERAL COAL MINE HEALTH AND SAFETY..., accident, and health insurance including premiums for supplementary medical insurance benefits under title...

N-Mesityl-C-acylketenimines: 1,5-Sigmatropic Shifts and Electrocyclization to Quinolines.

Science.gov (United States)

Rao, V. V. Ramana; Fulloon, Belinda E.; Bernhardt, Paul V.; Koch, Rainer; Wentrup, Curt

1998-08-21

Flash vacuum thermolysis (FVT) of triazoles 6a-c generates alpha-oxoketenimines 10, the ester 10a being isolable. FVT of pyrroledione 8 generates the isomeric imidoylketene 9a. Ketenes 9 and ketenimines 10 undergo thermal interconversion by 1,3-shifts of methoxy and dimethylamino groups under mild FVT conditions (ca. 350-400 degrees C). Both 9 and 10 are directly observable by IR spectroscopy at either 77 K or on Ar matrix isolation at 12 K. On FVT at temperatures above ca. 400 degrees C, the ketenimines 10 undergo a 1,5-H shift to o-quinoid imines 12/13, followed by electrocyclization to dihydroquinolines 14 (unobserved) and 15 (observed by NMR). The latter are easily oxidized to alkylquinoline-3-carboxylates or quinoline-3-carboxamides 16 by atmospheric oxygen. Ab initio calculations on model compounds 18-23 predict an energy barrier of ca. 38 kcal mol(-)(1) (161 kJ mol(-)(1)) for the 1,5-H shift in N-(o-methylphenyl)ketenimines via the transition state TS19 followed by an electrocyclization barrier to dihydroquinoline 23a via TS22a of ca. 16 kcal mol(-)(1).

1,3,5-Tri-p-tolylpentane-1,5-diol

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A. Thiruvalluvar

2014-02-01

Full Text Available In the title compound, C26H30O2, the central benzene ring forms dihedral angles of 14.85 (15 and 28.17 (14° with the terminal benzene rings. The dihedral angle between the terminal benzene rings is 32.14 (13°. The crystal packing exhibits two strong intermolecular O—H...O hydrogen bonds, forming directed four-membered co-operative rings. A region of disordered electron density, most probably disordered ethyl acetate solvent molecules, occupying voids of ca 519 Å3 for an electron count of 59, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement. The structure was refined as an inversion twin [absolute structure parameter = −0.3 (4].

Synthesis and characterization of new 3-(4,5-dihydro-5-arylisoxazol-3-yl-4-hydroxyquinolin-2(1H-ones and 3-(4-styrylisoxazolo[4,5-c]quinolin-4(5H-one derivatives

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S. Sarveswari

2016-09-01

Full Text Available The 4-hydroxy-3-(3-arylacryloylquinolin-2(1H-ones were synthesized from 3-acetyl-4-hydroxyquinolin-2(1H-one by microwave assisted synthesis, which in turn converted into their corresponding 3-(4,5-dihydro-5-arylisoxazol-3-yl-4-hydroxyquinolin-2(1H-ones and 3-(4-styrylisoxazolo[4,5-c]quinolin-4(5H-one derivatives.

Bis[(1-methyl-1H-tetrazol-5-ylsulfanyl]methane

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Wei Wei

2011-04-01

Full Text Available The molecule of the title compound, C5H8N8S2, lies on a twofold rotation axis that relates on 1-methyltetrazolyl group to the other; the five-membered rings are twisted by 53.1 (1°.

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

Science.gov (United States)

Karczmarzyk, Zbigniew; Pitucha, Monika; Wysocki, Waldemar; Pachuta-Stec, Anna; Stańczuk, Andrzej

2013-02-01

The title compound, C(11)H(13)N(3)S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2):0.23 (2) for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3) Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18) and 86.56 (49)° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15)° and this conformation is stabilized by an intra-molecular C-H⋯S contact. In the crystal, pairs of N-H⋯S hydrogen bonds link mol-ecules into inversion dimers. π-π inter-actions are observed between the triazole and benzene rings, with centroid-centroid separations of 3.547 (4) and 3.544 (12) Å for components A and B, and slippages of 0.49 (6) and 0.58 (15) Å, respectively.

Browse Title Index

African Journals Online (AJOL)

Items 551 - 600 of 1463 ... Issue, Title. Vol 15, No 2 (2015), Evaluation of the diagnostic performance and operational characteristics of four rapid immunochromatographic syphilis tests in Burkina Faso, Abstract PDF. FY Bocoum, H Ouedraogo, G Tarnagda, A Kiba, S Tiendrebeogo, F Bationo, B Liestman, S Diagbouga, ...

Synthesis, single-crystal structure determination and Raman spectra of the tricyanomelaminates NaA{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O (A = Rb, Cs)

Energy Technology Data Exchange (ETDEWEB)

Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Baker Lab.; Schulz, Armin [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

2016-07-01

Transparent colorless crystals of NaA{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O (A = Rb, Cs) were obtained by blending aqueous solutions of Na{sub 3}[C{sub 6}N{sub 9}] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group P2{sub 1}/m (no. 11) with the cell parameters a = 815.56(16), b = 1637.7(4) and c = 1036.4(3) pm, and β = 110.738(12) for NaRb{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O and a = 843.32(6), b = 1708.47(11) and c = 1052.42(7) pm, and β = 112.034(2) for NaCs{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O, respectively. Raman spectra of the title compounds complement our results.

Electrical properties and conduction mechanism of [C2H5NH3]2CuCl4 compound

Science.gov (United States)

Mohamed, C. Ben; Karoui, K.; Jomni, F.; Guidara, K.; Rhaiem, A. Ben

2015-02-01

The [(C2H5)NH3]2CuCl4 compound was prepared and characterized by several technique: the X-ray powder diffraction confirms the purity of the synthetized compound, the differential scanning calorimetric show several phase transitions at 236 K, 330 K, 357 K and 371 K, the dialectical properties confirms the ferroelectric-paraelectric phase transition at 238 K, which is reported by V. Kapustianyk et al. (2007) [1]. The two semi-circles observed in the complex impedance identify the presence of the grain interior and grain boundary contributions to the electrical response in this material. The equivalent circuit is modeled by a combination series of two parallel RP-CPE circuits. The temperature dependence of the alternative current conductivity (σg) and direct current conductivity (σdc) confirm the observed transitions in the calorimetric study. The (AC) electrical conduction in [(C2H5)NH3]2CuCl4 was studied by two processes that can be attributed to a hopping transport mechanism: the non-overlapping small polaron tunneling (NSPT) model in phase III and the correlated barrier hopping (CBH) model in phases I, II, IV, V and VI.

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.

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.

Low cell pH depresses peak power in rat skeletal muscle fibres at both 30 degrees C and 15 degrees C: implications for muscle fatigue.

Science.gov (United States)

Knuth, S T; Dave, H; Peters, J R; Fitts, R H

2006-09-15

Historically, an increase in intracellular H(+) (decrease in cell pH) was thought to contribute to muscle fatigue by direct inhibition of the cross-bridge leading to a reduction in velocity and force. More recently, due to the observation that the effects were less at temperatures closer to those observed in vivo, the importance of H(+) as a fatigue agent has been questioned. The purpose of this work was to re-evaluate the role of H(+) in muscle fatigue by studying the effect of low pH (6.2) on force, velocity and peak power in rat fast- and slow-twitch muscle fibres at 15 degrees C and 30 degrees C. Skinned fast type IIa and slow type I fibres were prepared from the gastrocnemius and soleus, respectively, mounted between a force transducer and position motor, and studied at 15 degrees C and 30 degrees C and pH 7.0 and 6.2, and fibre force (P(0)), unloaded shortening velocity (V(0)), force-velocity, and force-power relationships determined. Consistent with previous observations, low pH depressed the P(0) of both fast and slow fibres, less at 30 degrees C (4-12%) than at 15 degrees C (30%). However, the low pH-induced depressions in slow type I fibre V(0) and peak power were both significantly greater at 30 degrees C (25% versus 9% for V(0) and 34% versus 17% for peak power). For the fast type IIa fibre type, the inhibitory effect of low pH on V(0) was unaltered by temperature, while for peak power the inhibition was reduced at 30 degrees C (37% versus 18%). The curvature of the force-velocity relationship was temperature sensitive, and showed a higher a/P(0) ratio (less curvature) at 30 degrees C. Importantly, at 30 degrees C low pH significantly depressed the ratio of the slow type I fibre, leading to less force and velocity at peak power. These data demonstrate that the direct effect of low pH on peak power in both slow- and fast-twitch fibres at near-in vivo temperatures (30 degrees C) is greater than would be predicted based on changes in P(0), and that the

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

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Jun Jie Wang

2008-07-01

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

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

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Shayna R. Skokan

2017-07-01

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

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

The chemistry of 3-cyanopyridine-2(1H)-chalcogenones

International Nuclear Information System (INIS)

Litvinov, Victor P

2006-01-01

The data on the methods of synthesis and chemical properties of 3-cyanopyridine-2(1H)-chalcogenones published over the last 20 years are systematised and analysed. Special attention is given to the use of these compounds as building blocks in the synthesis of fused O,N,S-heterocycles.

C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

Energy Technology Data Exchange (ETDEWEB)

Audí-Miró, Carme, E-mail: carmeaudi@ub.edu [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Cretnik, Stefan [Institute of Groundwater Ecology, Helmholtz Zentrum München-National Research Center for Environmental Health, Ingolstädter Landstrasse 1, D-85764 Neuherberg (Germany); Torrentó, Clara; Rosell, Mònica [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Shouakar-Stash, Orfan [Department of Earth & Environmental Sciences, 200 University Ave. W, N2L 3G1 Waterloo, Ontario (Canada); Otero, Neus [Grup de Mineralogia Aplicada i Medi Ambient, Departament de Cristal.lografia, Mineralogia i Dipòsits Minerals, Facultat de Geologia, Universitat de Barcelona (UB), Martí Franquès s/n, 08028, Barcelona (Spain); Palau, Jordi [Université de Neuchâtel, CHYN - Centre d' Hydrogéologie, Rue Emile-Argand 11, CH-2000 Neuchâtel (Switzerland); and others

2015-12-15

Highlights: • {sup 13}C to evaluate natural chlorinated ethenes biodegradation. • {sup 13}C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • {sup 13}C-{sup 37}Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • {sup 13}C-{sup 37}Cl-{sup 2}H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using {sup 13}C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element {sup 13}C-{sup 37}Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using {sup 13}C-{sup 37}Cl-{sup 2}H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the {sup 13}C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element {sup 13}C-{sup 37}Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. {sup 2}H combined with {sup 13}C and {sup 37}Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ{sup 2}H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

C, Cl and H compound-specific isotope analysis to assess natural versus Fe(0) barrier-induced degradation of chlorinated ethenes at a contaminated site

International Nuclear Information System (INIS)

Audí-Miró, Carme; Cretnik, Stefan; Torrentó, Clara; Rosell, Mònica; Shouakar-Stash, Orfan; Otero, Neus; Palau, Jordi

2015-01-01

Highlights: • 13 C to evaluate natural chlorinated ethenes biodegradation. • 13 C to evaluate the efficiency of a zero-valent iron-permeable reactive barrier. • 13 C- 37 Cl to discriminate biotic from abiotic degradation of cis-dichloroethene. • 13 C- 37 Cl- 2 H of cis-DCE and TCE to elucidate different contaminant sources. - Abstract: Compound-specific isotopic analysis of multiple elements (C, Cl, H) was tested to better assess the effect of a zero-valent iron-permeable reactive barrier (ZVI-PRB) installation at a site contaminated with tetrachloroethene (PCE) and trichloroethene (TCE). The focus was on (1) using 13 C to evaluate natural chlorinated ethene biodegradation and the ZVI-PRB efficiency; (2) using dual element 13 C- 37 Cl isotopic analysis to distinguish biotic from abiotic degradation of cis-dichloroethene (cis-DCE); and (3) using 13 C- 37 Cl- 2 H isotopic analysis of cis-DCE and TCE to elucidate different contaminant sources. Both biodegradation and degradation by ZVI-PRB were indicated by the metabolites that were detected and the 13 C data, with a quantitative estimate of the ZVI-PRB efficiency of less than 10% for PCE. Dual element 13 C- 37 Cl isotopic plots confirmed that biodegradation was the main process at the site including the ZVI-PRB area. Based on the carbon isotope data, approximately 45% and 71% of PCE and TCE, respectively, were estimated to be removed by biodegradation. 2 H combined with 13 C and 37 Cl seems to have identified two discrete sources contributing to the contaminant plume, indicating the potential of δ 2 H to discriminate whether a compound is of industrial origin, or whether a compound is formed as a daughter product during degradation.

4-Aminobenzoic acid–1,2-bis(4-pyridylethane (2/1

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Fwu Ming Shen

2010-07-01

Full Text Available In the title compound, C12H12N2·2C7H7NO2, the 4-aminobenzoic acid molecules are linked by O—H...N hydrogen bonds to 1,2-bis(4-pyridylethane, forming linear hydrogen bonded chains parallel to [2overline{1}1]. The structure exhibits a hydrogen-bonding network involving COOH...N(pyridyl and amine and carboxylic N—H... O interactions. In addition, π–π stacking interactions [centroid–centroid distance = 3.8622 (14 Å] are also present.

9-Butyl-9H-carbazole

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2009-03-01

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

(Z-3-(4-Bromoanilino-1-ferrocenylbut-2-en-1-one

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C. Manzur

2010-12-01

Full Text Available In the title compound, [Fe(C5H5(C15H13BrNO], formed from the reaction of ferrocenoylacetone and 4-bromoaniline, the molecular structure is stabilized by an intramolecular N—H...O hydrogen bond between the amine and carbonyl groups.

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.

Browse Title Index

African Journals Online (AJOL)

Issue, Title. Vol 17 (2005), A. C. conduction behaviour in amorphous WO3/CEO2 thin film, Abstract. B Yagoubi, C A Hogarth, A Boukorrt. Vol 16 (2003), A lossless image compression algorithm using variable block size segmentation, Abstract. Z Brahimi, K A Saadi, N Baraka. Vol 15 (2003), Analysis method of wavelet ...

An asymmetric synthesis of (R)-5-(methylamino)-5,6-dihydro-4H-imidazo-[4,5,1-ij]quinolin-2(1H) -one (1) and its [2-14C]-and [6,7-3H2]-labeled forms

International Nuclear Information System (INIS)

Heier, R.F.; Moon, M.W.; Stolle, W.T.; Easter, J.A.; Hsi, R.S.P.

1996-01-01

(R)-5-(Methylamino)-5,6-dihydro-4H-imidazo [4,5,1-ij)quinolin-2(1H)-one (1) is a dopamine agonist which shows selectivity for the D2 receptor subtype, and is of interest as a potential drug for the treatment of Parkinson's disease. An asymmetric epoxidation approach has been used to prepare 1 in eleven steps (15% overall yield) from 8-nitroquinoline. An advanced intermediate in this synthesis, tert-butyl (R)-methyl(8-amino-1,2,3,4-tetrahydro-3-quinolinyl)carbamate, has been reacted with [ 14 C]phosgene to provide a two-step synthesis of 1 labeled with carbon-14 at the C-2 position (236 μCi/mg). Bromination of 1 gave the dibromo analogue which was reduced in the presence of tritium gas to give 1 labeled with tritium at the C-6 and C-7 positions (28.5 Ci/mmol). In addition to providing syntheses for labeled forms of the drug which are useful in drug disposition and receptor binding studies, this approach also provides a convenient synthesis for the unlabeled form of drug. (author)

Microwave assisted synthesis and antimicrobial activity of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones

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Dongamanti Ashok

2015-06-01

Full Text Available A series of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones were design and synthesized by Click reaction followed by Claisen-Schmidt condensation under microwave irradiation and conventional heating methods. The structures of newly synthesized compounds have been established on the basis of elemental analysis, IR, 1H & 13C NMR and mass spectral data. All the compounds were screened for their antimicrobial activity.

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

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Hong-Mian Wu

2008-05-01

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

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

NARCIS (Netherlands)

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

1989-01-01

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

(Acetylacetonato-κ2O,O′carbonyl[tris(naphthalen-1-ylphosphane-κP]rhodium(I acetone hemisolvate

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Hezron Ogutu

2012-04-01

Full Text Available The title compound, [Rh(C5H7O2(C30H21P(CO]·0.5C3H6O, has two different complex molecules in the asymmetric unit, with the RhI atoms in slightly distorted square-planar coordination environments. The molecules are packed as two monomeric molecules with one acetone solvent molecule sitting at the centre.

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

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Mohamed Tebbaa

2012-02-01

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

4,4′-[Thiophene-2,5-diylbis(ethyne-2,1-diyl]dibenzonitrile

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Kari Rissanen

2008-04-01

Full Text Available In the solid state, the title compound, C22H10N2S, forms centrosymmetric dimers by pairs of non-classical C—H...S hydrogen bonds linking approximately coplanar molecules. The benzene ring involved in this interaction makes a dihedral angle of only 7.21 (16° with the thiophene ring, while the other benzene ring is twisted somewhat out of the plane, with a dihedral angle of 39.58 (9°. The hydrogen-bonded dimers stack on top of each other with an interplanar spacing of 3.44 Å. C—H...N hydrogen bonds link together stacks that run in approximately perpendicular directions. Each molecule thus interacts with 12 adjacent molecules, five of them approaching closer than the sum of the van der Waals radii for the relevant atoms. Optimization of the inter-stack contacts contributes to the non-planarity of the molecule.

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

Science.gov (United States)

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

2017-08-01

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

8-[(3-Phenyl-1,2,4-oxadiazol-5-ylmethoxy]quinoline monohydrate

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Shu-Yuan Bai

2013-07-01

Full Text Available In the title compound, C18H13N3O2·H2O, the oxadiazole ring forms dihedral angles 7.21 (10 and 21.25 (11° with the quinoline and benzene rings, respectively. The crystal structure features O—H...N hydrogen bonds and is further consolidated by C—H...O hydrogen-bonding interactions involving the water molecule of hydration.

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

Science.gov (United States)

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

2012-01-01

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

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.

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.

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.

Influence of different organic fertilizers on quality parameters and the delta(15)N, delta(13)C, delta(2)H, delta(34)S, and delta(18)O values of orange fruit (Citrus sinensis L. Osbeck).

Science.gov (United States)

Rapisarda, Paolo; Camin, Federica; Fabroni, Simona; Perini, Matteo; Torrisi, Biagio; Intrigliolo, Francesco

2010-03-24

To investigate the influence of different types of fertilizers on quality parameters, N-containing compounds, and the delta(15)N, delta(13)C, delta(2)H, delta (34)S, and delta(18)O values of citrus fruit, a study was performed on the orange fruit cv. 'Valencia late' (Citrus sinensis L. Osbeck), which was harvested in four plots (three organic and one conventional) located on the same farm. The results demonstrated that different types of organic fertilizers containing the same amount of nitrogen did not effect important changes in orange fruit quality parameters. The levels of total N and N-containing compounds such as synephrine in fruit juice were not statistically different among the different treatments. The delta(15)N values of orange fruit grown under fertilizer derived from animal origin as well as from vegetable compost were statistically higher than those grown with mineral fertilizer. Therefore, delta(15)N values can be used as an indicator of citrus fertilization management (organic or conventional), because even when applied organic fertilizers are of different origins, the natural abundance of (15)N in organic citrus fruit remains higher than in conventional ones. These treatments also did not effect differences in the delta(13)C, delta(2)H, delta(34)S, and delta(18)O values of fruit.

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

Science.gov (United States)

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

2017-01-01

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

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

Science.gov (United States)

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

2008-04-10

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

Synthesis of Donor/Acceptor-Substituted Diazo Compounds in Flow and Their Application in Enantioselective Dirhodium-Catalyzed Cyclopropanation and C-H Functionalization.

Science.gov (United States)

Rackl, Daniel; Yoo, Chun-Jae; Jones, Christopher W; Davies, Huw M L

2017-06-16

A tandem reaction system has been developed for the preparation of donor/acceptor-substituted diazo compounds in continuous flow coupled to dirhodium-catalyzed C-H functionalization or cyclopropanation. Hydrazones were oxidized in flow by solid-supported N-iodo-p-toluenesulfonamide potassium salt (PS-SO 2 NIK) to generate the diazo compounds, which were then purified by passing through a column of molecular sieves/sodium thiosulfate.

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

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Ulrich S. Schubert

2009-05-01

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

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

International Nuclear Information System (INIS)

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

2004-01-01

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

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

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Julio Zukerman-Schpector

2009-07-01

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

1-Methyl-3-(2-methylphenyl-4-phenyl-1H-pyrazolo[3,4-d]pyrimidine

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Mohamed El Hafi

2017-10-01

Full Text Available In the title compound, C19H16N4, the pyrazolopyrimidine unit is slightly twisted. A combination of π-stacking and offset π-stacking interactions forms columns along the b-axis direction.

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

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Kate L. Edler

2010-12-01

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

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

Science.gov (United States)

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

2003-03-24

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

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

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Qiao Yan

2011-12-01

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

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.

Other compounds isolated from Simira glaziovii and the {sup 1}H and {sup 13}C NMR chemical shift assignments of new 1-epi-castanopsol

Energy Technology Data Exchange (ETDEWEB)

Araujo, Marcelo F. de; Vieira, Ivo J. Curcino [Universidade Federal Rural do Rio de Janeiro, Seropedica, RJ (Brazil). Dept. de Quimica; Braz-Filho, Raimundo [Universidade Estadual do Norte Fluminense (UENF), Campos dos Goytacases, RJ (Brazil). Centro de Ciencias Tecnologicas. Lab. de Ciencias Quimicas; Carvalho, Mario G. de, E-mail: mgeraldo@ufrrj.br [Universidade Federal do Rio de Janeiro (NPPN/UFRJ), RJ (Brazil). Centro de Ciencias da Saude. Nucleo de Pesquisa em Produtos Naturais

2012-07-01

A new triterpene, 1-epi-castanopsol, besides eleven known compounds: sitosterol, stigmasterol, campesterol, lupeol, lupenone, simirane B, syringaresinol, scopoletin, isofraxidin, 6,7,8-trimethoxycoumarin and harman, were isolated from the wood of Simira glaziovii. The structures of the known compounds were defined by 1D, 2D {sup 1}H, {sup 13}C NMR spectra data analyses and comparison with literature data. The detailed spectral data analyses allowed the definition of the structure of the new 1-epi isomer of castanopsol and performance of {sup 1}H and {sup 13}C NMR chemical shift assignments. (author)

Ethyl 27-oxo-15-oxa-2,20-diazahexacyclo[18.6.1.01,8.02,6.09,14.021,26]heptacosa-9,11,13,21,23,25-hexaene-7-carboxylate

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Devadasan Velmurugan

2013-01-01

Full Text Available In the title compound, C27H30N2O4, the pyrrolidine ring adopts a twisted conformation. The indoline ring system is almost perpendicular to the mean plane of the pyrrolidine ring, making a dihedral angle of 81.7 (8°. In the crystal, molecules are linked into centrosymmetric dimers with graph-set motif R22(16 via pairs of C—H...O hydrogen bonds. The terminal ethyl group of the ester group is disordered over two sets of sites, with a site-occupancy ratio of 0.587 (11:0.413 (11.

Interaction of stress with the martensitic phase transition in A15 compounds

International Nuclear Information System (INIS)

Welch, D.O.

1981-01-01

Recently there has been a resurgence of interest in the effect of the martensitic phase transition which occurs in many A15 compounds on superconductivity and on elastic and anelastic behavior. Since in many practical applications, A15 compounds are subject to considerable stress and strain, it is of interest to examine the interaction of stress with the martensitic transition; this paper is an examination of the effects of stress predicted by a simple Landau model which successfully describes many features of the transition and the related temperature dependence of the elastic modulus (c 11 -c 12 )/2. The effect of stress on the temperature ranges of stability and metastability of various types of martensitic domain is discussed. The non-linearity of the stress-strain relation in a polycrystalline A15 is studied

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

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

2002-10-01

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

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

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Guo-Liang Zhao

2012-05-01

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

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

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Rajni Kant

2012-04-01

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

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.

Reaction rate and isomer-specific product branching ratios of C2H + C4H8: 1-butene, cis-2-butene, trans-2-butene, and isobutene at 79 K.

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Bouwman, Jordy; Fournier, Martin; Sims, Ian R; Leone, Stephen R; Wilson, Kevin R

2013-06-20

The reactions of C2H radicals with C4H8 isomers 1-butene, cis-2-butene, trans-2-butene, and isobutene are studied by laser photolysis-vacuum ultraviolet mass spectrometry in a Laval nozzle expansion at 79 K. Bimolecular-reaction rate constants are obtained by measuring the formation rate of the reaction product species as a function of the reactant density under pseudo-first-order conditions. The rate constants are (1.9 ± 0.5) × 10(-10), (1.7 ± 0.5) × 10(-10), (2.1 ± 0.7) × 10(-10), and (1.8 ± 0.9) × 10(-10) cm(3) s(-1) for the reaction of C2H with 1-butene, cis-2-butene, trans-2-butene, and isobutene, respectively. Bimolecular rate constants for 1-butene and isobutene compare well to values measured previously at 103 K using C2H chemiluminescence. Photoionization spectra of the reaction products are measured and fitted to ionization spectra of the contributing isomers. In conjunction with absolute-ionization cross sections, these fits provide isomer-resolved product branching fractions. The reaction between C2H and 1-butene yields (65 ± 10)% C4H4 in the form of vinylacetylene and (35 ± 10)% C5H6 in the form of 4-penten-1-yne. The cis-2-butene and trans-2-butene reactions yield solely 3-penten-1-yne, and no discrimination is made between cis- and trans-3-penten-1-yne. Last, the isobutene reaction yields (26 ± 15)% 3-penten-1-yne, (35 ± 15)% 2-methyl-1-buten-3-yne, and (39 ± 15)% 4-methyl-3-penten-1-yne. The branching fractions reported for the C2H and butene reactions indicate that these reactions preferentially proceed via CH3 or C2H3 elimination rather than H-atom elimination. Within the experimental uncertainties, no evidence is found for the formation of cyclic species.

Rats Born to Mothers Treated with Dexamethasone 15 cH Present Changes in Modulation of Inflammatory Process

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Leoni V. Bonamin

2012-01-01

Full Text Available As little information about the effect of ultra high dilutions of glucocorticoid in reproduction is available in the literature, pregnant female Wistar rats (N=12 were blindly subcutaneously treated during all gestational and lactation period with: dexamethasone 4 mg/kg diluted into dexamethasone 15 cH (mixed; or dexamethasone 4 mg/kg diluted in water; or dexamethasone 15 cH, or vehicle. Parental generation had body weight, food and water consumption monitored. The F1 generation was monitored regarding to newborn development. No birth occurred in both groups treated with dexamethasone 4 mg/kg. After 60 days from birth, 12 male F1 rats were randomly selected from each remaining group and inoculated subcutaneously with 1% carrageenan into the footpad, for evaluation of inflammatory performance. Edema and histopathology of the footpad were evaluated, using specific staining methods, immunohistochemistry and digital histomorphometry. Mothers treated with mixed dexamethasone presented reduced water consumption. F1 rats born to dexamethasone 15 cH treated females presented significant increase in mast cell degranulation, decrease in monocyte percentage, increase in CD18+ PMN cells, and early expression of ED2 protein, in relation to control. The results show that the exposure of parental generation to highly diluted dexamethasone interferes in inflammation modulation in the F1 generation.

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

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Ming-Jian Li

2009-09-01

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

Auto-inducing media for uniform isotope labeling of proteins with 15N, 13C and 2H

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Guthertz, Nicolas; Klopp, Julia; Winterhalter, Aurélie; Fernández, César; Gossert, Alvar D.

2015-01-01

Auto-inducing media for protein expression offer many advantages like robust reproducibility, high yields of soluble protein and much reduced workload. Here, an auto-inducing medium for uniform isotope labelling of proteins with 15 N, 13 C and/or 2 H in E. coli is presented. So far, auto-inducing media have not found widespread application in the NMR field, because of the prohibitively high cost of labeled lactose, which is an essential ingredient of such media. Here, we propose using lactose that is only selectively labeled on the glucose moiety. It can be synthesized from inexpensive and readily available substrates: labeled glucose and unlabeled activated galactose. With this approach, uniformly isotope labeled proteins were expressed in unattended auto-inducing cultures with incorporation of 13 C, 15 N of 96.6 % and 2 H, 15 N of 98.8 %. With the present protocol, the NMR community could profit from the many advantages that auto-inducing media offer

catena-Poly[[[trans-diaquabis(pyridine-κNcobalt(II]-μ-(4-{N′-[1-(3-acetyl-4-methyl-1H-pyrazol-5-ylethylidene]hydrazino}benzoato-κ3O:N,N′-[bis(pyridine-κNcobalt(III]-μ-(4-{N′-[1-(3-acetyl-4-methyl-1H-pyrazol-5-ylethylidene]hydrazino}benzoato-κ3N,N′:O]perchlorate 3.66-hydrate

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Igor O. Fritsky

2008-02-01

Full Text Available The title compound, {[Co2(C15H14N4O32(C5H5N4(H2O2]ClO4·3.66H2O}n, is a one-dimensional coordination polymer, with both CoII and CoIII centres in its structure. The ligand environment surrounding CoIII is formed by two N,N-chelating pyrazole-containing ligands and two pyridine molecules in axial positions. The high-spin CoII ions, situated at crystallographic centres of inversion, exhibit a distorted octahedral coordination mode. The ClO4− anion is linked to the polymer chain via hydrogen bonds. The chains are connected by hydrogen bonds to produce a three-dimensional structure.

Different molecular conformations co-exist in each of three 2-aryl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)acetamides: hydrogen bonding in zero, one and two dimensions.

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Narayana, Badiadka; Yathirajan, Hemmige S; Rathore, Ravindranath S; Glidewell, Christopher

2016-09-01

4-Antipyrine [4-amino-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one] and its derivatives exhibit a range of biological activities, including analgesic, antibacterial and anti-inflammatory, and new examples are always of potential interest and value. 2-(4-Chlorophenyl)-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)acetamide, C19H18ClN3O2, (I), crystallizes with Z' = 2 in the space group P\\overline{1}, whereas its positional isomer 2-(2-chlorophenyl)-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)acetamide, (II), crystallizes with Z' = 1 in the space group C2/c; the molecules of (II) are disordered over two sets of atomic sites having occupancies of 0.6020 (18) and 0.3980 (18). The two independent molecules of (I) adopt different molecular conformations, as do the two disorder components in (II), where the 2-chlorophenyl substituents adopt different orientations. The molecules of (I) are linked by a combination of N-H...O and C-H...O hydrogen bonds to form centrosymmetric four-molecule aggregates, while those of (II) are linked by the same types of hydrogen bonds forming sheets. The related compound N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)-2-(3-methoxyphenyl)acetamide, C20H21N3O3, (III), is isomorphous with (I) but not strictly isostructural; again the two independent molecules adopt different molecular conformations, and the molecules are linked by N-H...O and C-H...O hydrogen bonds to form ribbons. Comparisons are made with some related structures, indicating that a hydrogen-bonded R2(2)(10) ring is the common structural motif.