Novel decavanadate cluster complexes [H2V10O28][LH]4·nH2O (L = Imidazole, n = 2 or 2-methylimidazole, n = 0): Preparation, characterization and genotoxic studies

Science.gov (United States)

Siddiqi, Zafar A.; Anjuli; Sharma, Prashant K.; Shahid, M.; Khalid, Mohd.; Siddique, Armeen; Kumar, Sarvendra

2012-12-01

The title complexes were obtained from the reaction of VOSO4 with imidazole or 2-methyl imidazole in presence of adipic acid/iminodiacetic acid. X-ray crystallographic investigations on [H2V10O28](2-MeImzH)4 (2) revealed a strong interaction between decavanadate anion and the protonated ligand moieties as counter cations to stabilize the crystal motif resulting in a high symmetry 2D sheet network. The cyclic voltammetry of (2) suggested formation of a quasi-reversible redox (VV/IV) couple in the solution. The genotoxic studies employing single cell gel electrophoresis (comet assay) confirmed the non-toxic nature of the compounds.

(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.

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

(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.

Diaqua[(1R,2S,4R,8R,9S,11R-2,9-dimethyl-1,4,8,11-tetraazacyclotetradecane]nickel(II dichloride dihydrate

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James Alan Townsend

2012-08-01

Full Text Available The crystal structure of the title complex, [Ni(C12H28N4(H2O2]Cl2·2H2O, displays O—H...Cl and O—H...O hydrogen bonding. The tetraazacyclotetradecane ligand interacts with the NiII atom in the cis V configuration and the final two ligand binding sites are occupied by water.

Crystal structure of 1-[(2S*,4R*-6-fluoro-2-methyl-1,2,3,4-tetrahydroquinolin-4-yl]pyrrolidin-2-one

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P. S. Pradeep

2014-09-01

Full Text Available In the title compound, C14H17FN2O, the 1,2,3,4-tetrahydropyridine ring of the quinoline moiety adopts a half-chair conformation, while the pyrrolidine ring has an envelope conformation with the central methylene C atom as the flap. The pyrrolidine ring lies in the equatorial plane and its mean plane is normal to the mean plane of the quinoline ring system, with a dihedral angle value of 88.37 (9°. The bridging N—C bond distance [1.349 (3 Å] is substantially shorter than the sum of the covalent radii (dcov: C—N = 1.47 Å and C=N = 1.27 Å, which indicates partial double-bond character for this bond, resulting in a certain degree of charge delocalization. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds, forming sheets lying parallel to (10-1. These two-dimensional networks are linked via C—H...F hydrogen bonds and C—H...π interactions, forming a three-dimensional structure.

2-{4-Methyl-N-[(2,3,4,9-tetrahydro-1H-carbazol-3-ylmethyl]benzenesulfonamido}ethyl 4-methylbenzenesulfonate

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Nagihan Çaylak Delibaş

2013-12-01

Full Text Available In the title compound, C29H32N2O5S2, the indole ring system is nearly planar, with a maximum deviation of 0.013 (2 Å, and the cyclohexenone ring has an envelope conformation with the methine C atom as the flap. The two methylbenzene rings are approximately perpendicular to each other, making a dihedral angle of 89.09 (8°. In the crystal, N—H...O hydrogen bonds link the molecules into a chain running along the a-axis direction, and weak C—H...O hydrogen bonds and C—H...π interactions are observed between the chains.

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Phosphinodi(benzylsilane) PhP{(o-C6H4CH2)SiMe2H}2: a versatile "PSi2Hx" pincer-type ligand at ruthenium.

Science.gov (United States)

Montiel-Palma, Virginia; Muñoz-Hernández, Miguel A; Cuevas-Chávez, Cynthia A; Vendier, Laure; Grellier, Mary; Sabo-Etienne, Sylviane

2013-09-03

The synthesis of the new phosphinodi(benzylsilane) compound PhP{(o-C6H4CH2)SiMe2H}2 (1) is achieved in a one-pot reaction from the corresponding phenylbis(o-tolylphosphine). Compound 1 acts as a pincer-type ligand capable of adopting different coordination modes at Ru through different extents of Si-H bond activation as demonstrated by a combination of X-ray diffraction analysis, density functional theory calculations, and multinuclear NMR spectroscopy. Reaction of 1 with RuH2(H2)2(PCy3)2 (2) yields quantitatively [RuH2{[η(2)-(HSiMe2)-CH2-o-C6H4]2PPh}(PCy3)] (3), a complex stabilized by two rare high order ε-agostic Si-H bonds and involved in terminal hydride/η(2)-Si-H exchange processes. A small free energy of reaction (ΔrG298 = +16.9 kJ mol(-1)) was computed for dihydrogen loss from 3 with concomitant formation of the 16-electron species [RuH{[η(2)-(HSiMe2)-CH2-o-C6H4]PPh[CH2-o-C6H4SiMe2]}(PCy3)] (4). Complex 4 features an unprecedented (29)Si NMR decoalescence process. The dehydrogenation process is fully reversible under standard conditions (1 bar, 298 K).

The MgSeO4-UO2SeO4-H2O system at 25 deg C

International Nuclear Information System (INIS)

Serezhkina, L.B.; Serezhkin, V.N.

1984-01-01

The method of isothermal solubility at 25 deg C has been used to study MgSeO 4 -UO 2 SeO 4 -H 2 O system. Formation of the new compound Mg 2 (UO 2 ) 3 (SeO 4 ) 5 X32H 2 O, congruently soluble in water is stated. Thermographic and X-ray diffraction investigations of the prepared magnesium selenato-uranylate and products of its dehydration are conducted

(1R,2R,3R,4R,5S-2,3-Bis[(2S′-2-acetoxy-2-phenylacetoxy]-4-azido-1-[(2,4-dinitrophenylhydrazonomethyl]bicyclo[3.1.0]hexane

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Robert McDonald

2008-02-01

Full Text Available In the title compound, C38H29N7O12, the five-membered ring adopts an envelope conformation in which the `flap' is cis to the cyclopropane group. This conformation is similar to those of other bicyclo[3.1.0]hexane analogues for which crystal structures have been reported. The absolute configuration of the stereogenic centers on the cyclopentane ring, as determined by comparison with the known configurations of the stereogenic centers in the (2S-2-acetoxy-2-phenylacetoxy groups, is 1(R, 2(R, 3(R, 4(R and 5(S. An intramolecular N—H...O hydrogen bond is present.

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

International Nuclear Information System (INIS)

Vaqueiro, Paz

2006-01-01

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

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

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Augusto Rivera

2013-07-01

Full Text Available The title compound, C23H30N2O4, a di-Mannich base derived from 4-methoxyphenol and cis-1,2-diaminecyclohexane, has a perhydrobenzimidazolidine nucleus, in which the cyclohexane ring adopts a chair conformation and the heterocyclic ring has a half-chair conformation with a C—N—C—C torsion angles of −48.14 (15 and −14.57 (16°. The mean plane of the heterocycle makes dihedral angles of 86.29 (6 and 78.92 (6° with the pendant benzene rings. The molecular structure of the title compound shows the presence of two interactions between the N atoms of the imidazolidine ring and the hydroxyl groups through intramolecular O—H...N hydrogen bonds with graph-set motif S(6. The unobserved lone pairs of the N atoms are presumed to be disposed in a syn conformation, being only the second example of an exception to the typical `rabbit-ears' effect in 1,2-diamines.

3β-Acetoxy-lup-20(29-en-28-yl 1H-1,2,4-triazole-1-carboxylate

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R.C. Santos

2010-11-01

Full Text Available The title triterpene, C35H53N3O4, is a C-28 carbamate derivative of 3β-acetoxybetulin prepared in a one-step reaction from the commercially available 1,1′-carbonyl-di(1,2,4-triazole (CDT, crystallized from acetone/n-hexane. All rings are trans fused. The carbamate and acetate substituents are in axial and equatorial positions, respectively. A quantum chemical ab initio Roothaan Hartree–Fock calculation of the equilibrium geometry of the isolated molecule gives values for bond lengths and valency angles in close agreement with experimental values. The calculation also reproduces the observed molecular conformation, with puckering parameters that agree well with those determined from the crystallographic study.

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

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

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Huichun Zhu

2010-01-01

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

2,3,4,6-Tetra-O-acetyl-β-d-galactopyranosyl 2,3,4,6-tetra-O-acetyl-β-d-glucopyranosyl disulfide tetrahydrofuran solvate

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Matías López-Rodríguez

2008-12-01

Full Text Available The asymmetric unit of title compound, C28H38O18S2·C4H8O, comprises one disulfide-bridged sugar molecule and one solvent molecule. No significant differences in structural parameters are found between the present structure and the previously determined unsolvated form [Brito, López-Rodríguez, Bényei & Szilagyi (2006. Carbohydr. Res. 341, 2967–2972]. The compounds are characterized by a compact structure with spatial proximity of the two pyranosyl rings. One of the carbonyl atoms is disordered over two sites [site occupancy = 0.69 (7 for major component] and the displacement parameters for the THF species are unsually large.

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

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Matthew R. Carbone

2014-11-01

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

1-Benzyl-3-(2-furylmethyl-1,2,3,4,5,6-hexahydrospiro[benzo[h]quinazoline-5,1′-cyclohexane]-2,4-dione

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Siranush Gabrielyan

2008-04-01

Full Text Available The title compound, C29H28N2O3, displays antidepressant and anticancer activities. The furan ring is disordered over two orientations [site occupancies 0.690 (12/0.310 (12] related by a rotation of 180°. The ring conformations are chair for the cyclohexane ring, boat for the cyclohexadiene ring and twist for the pyrimidine ring. The crystal packing is determined solely by van der Waals interactions.

Synthesis, structure, optical, photoluminescence and magnetic properties of K2[Co(C2O4)2(H2O)2]·4H2O

Science.gov (United States)

Narsimhulu, M.; Hussain, K. A.

2018-06-01

The synthesis, crystal structure, optical, photoluminescence and magnetic behaviour of potassium bis(oxalato)cobaltate(II)tertrahydrate{K2[Co(C2O4)2(H2O)2]·4H2O} are described. The compound was grown at room temperature from mixture of aqueous solutions by slow evaporation method. The X-ray crystallographic data showed that the compound belongs to the monoclinic crystal system with P21/n space group and Z = 4. The UV-visible diffuse absorbance spectra exhibited bands at 253, 285 and 541 nm in the visible and ultraviolet regions. The optical band gap of the compound was estimated as 3.4 eV. At room temperature, an intense photoluminescence was observed from this material around 392 nm when it excited at 254 nm. The variable temperature dc magnetic susceptibility measurements exposed paramagnetic behaviour at high temperatures and antiferromagnetic ordering at low temperatures.

Synthesis and crystal structure of new uranyl selenite(IV)-selenate(VI) [C5H14N][(UO2)3(SeO4)4(HSeO3)(H2O)](H2SeO3)(HSeO4)

International Nuclear Information System (INIS)

Krivovichev, S.V.; Tananaev, I.G.; Myasoedov, B.F.; Kalenberg, V.

2006-01-01

Crystals of new uranyl selenite(IV)-selenate(VI) [C 5 H 14 N][(UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)](H 2 SeO 3 )(HSeO 4 ) are obtained by the method of evaporation from aqueous solutions. Compound has triclinic lattice, space group P1-bar, a=11.7068(9), b=14.8165(12), c=16.9766(15), α=73.899(6), β=76.221(7), γ=89.361(6) Deg, V=2743.0(4) A 3 , Z=2. Laminated complexes (UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)] 3- are the basis of the structure. [HSe(VI)O 4 ] - , [H 2 Se(IV)O 3 ] complexes and protonated methylbutylamine cations are disposed between layers [ru

Solvent-Dependent Delamination, Restacking, and Ferroelectric Behavior in a New Charge-Separated Layered Compound: [NH4 ][Ag3 (C9 H5 NO4 S)2 (C13 H14 N2 )2 ]⋅8 H2 O.

Science.gov (United States)

Sushrutha, Sringeri Ramesh; Mohana, Shivanna; Pal, Somnath; Natarajan, Srinivasan

2017-01-03

A new anionic coordination polymer, [NH 4 ][Ag 3 (C 9 H 5 NO 4 S) 2 (C 13 H 14 N 2 ) 2 ]⋅8 H 2 O, with a two-dimensional structure, has been synthesized by a reaction between silver nitrate, 8-hydroxyquinoline-5-sulfonic acid (HQS), and 4,4'-trimethylene dipyridine (TMDP). The compound stabilizes in a noncentrosymmetric space group, and the lattice water molecules and the charge-compensating [NH 4 ] + group occupy the inter-lamellar spaces. The lattice water molecules can be fully removed and reinserted, which is accompanied by a crystalline-amorphous-crystalline transformation. This transformation resembles the collapse/delamination and restacking of the layers. To the best of our knowledge, this is the first observation of delamination and restacking in an inorganic coordination polymer that contains silver. The presence of a natural dipole (the anionic framework and cationic ammonium ions) along with the noncentrosymmetric space group gives rise to the room-temperature ferroelectric behavior of the compound. The ferroelectric behavior is also water-dependent and exhibits a ferroelectric-paraelectric transformation. The temperature-dependent dielectric measurements indicate that the ferroelectric/ paraelectric transformation occurs at 320 K. This transformation has also been investigated by using in-situ IR spectroscopy and PXRD studies. The second-harmonic generation (SHG) study indicated values that are comparable to some of the known SHG solids, such as potassium dihydrogen phosphate (KDP) and urea. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Vibrational spectra of Cs2Cu(SO4)2·6H2O and Cs2Cu(SeO4)2·nH2O (n = 4, 6) with a crystal structure determination of the Tutton salt Cs2Cu(SeO4)2·6H2O

Science.gov (United States)

Wildner, M.; Marinova, D.; Stoilova, D.

2016-02-01

The solubility in the three-component systems Cs2SO4-CuSO4-H2O and Cs2SeO4-CuSeO4-H2O have been studied at 25 °C. The experimental results show that double salts, Cs2Cu(SO4)2·6H2O and Cs2Cu(SeO4)2·4H2O, crystallize from the ternary solutions within large concentration ranges. Crystals of Cs2Cu(SeO4)2·6H2O were synthesized at somewhat lower temperatures (7-8 °C). The thermal dehydration of the title compounds was studied by TG, DTA and DSC methods and the respective dehydration schemes are proposed. The calculated enthalpies of dehydration (ΔHdeh) have values of: 434.2 kJ mol-1 (Cs2Cu(SeO4)2·6H2O), 280.9 kJ mol-1 (Cs2Cu(SeO4)2·4H2O), and 420.2 kJ mol-1 (the phase transition of Cs2Cu(SO4)2·6H2O into Cs2Cu(SO4)2·H2O). The crystal structure of Cs2Cu(SeO4)2ṡ6H2O was determined from single crystal X-ray diffraction data. It belongs to the group of Tutton salts, crystallizing isotypic to the respective sulfate in a monoclinic structure which is characterized by isolated Cu(H2O)6 octahedra and SeO4 tetrahedra, interlinked by hydrogen bonds and [9]-coordinated Cs+ cations. Infrared spectra of the cesium copper compounds are presented and discussed with respect to both the normal modes of the tetrahedral ions and the water molecules. The analysis of the infrared spectra of the double compounds reveals that the distortion of the selenate tetrahedra in Cs2Cu(SeO4)2·4H2O is stronger than those in Cs2Cu(SeO4)2·6H2O in agreement with the structural data. Matrix-infrared spectroscopy was applied to confirm this claim - Δν3 for SO4 2 - ions matrix-isolated in Cs2Cu(SeO4)2·6H2O has a value of 35 cm-1 and that of the same ions included in Cs2Cu(SeO4)2·4H2O - 84 cm-1. This spectroscopic finding is due to the formation of strong covalent bands Cu-OSO3 on one hand, and on the other to the stronger deformation of the host SeO4 2 - tetrahedra in Cs2Cu(SeO4)2·4H2O as compared to those in Cs2Cu(SeO4)2·6H2O. The strength of the hydrogen bonds as deduced from the

3-Chloro-4-methyl­quinolin-2(1H)-one

Science.gov (United States)

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

2012-01-01

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

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.

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.

Study of ZrO2-H2SO4-(NH4)2SO4(NH4Cl)-H2O systems

International Nuclear Information System (INIS)

Motov, D.L.; Sozinova, Yu.P.; Rys'kina, M.P.

1988-01-01

Regions of formation, composition and solubility of ammonium sulfatozirconates (ASZ) in ZrO 2 -H 2 SO 4 -(NH 4 ) 2 SO 4 (NH 4 Cl)-H 2 O systems at 25 and 75 deg C are studied by the isothermal method. Five ASZ: (NH 4 ) 2 Zr(OH) 2 (SO 4 ) 2 , NH 4 ZrOH(SO 4 ) 2 xH 2 O, NH 4 ZrO 0.5 (OH) 2 SO 4 x1.5H 2 O, (NH 4 ) 2 Zr(SO 4 ) 3 x2H 2 O, (NH 4 ) 4 Zr(SO 4 ) 4 x4H 2 O are detected, their properties are investigated. Main sulfates are new compounds never described ealier

Disproportionation and thermochemical sulfate reduction reactions in S-H20-Ch4 and S-D2O-CH4 systems from 200 to 340 °C at elevated pressures

Science.gov (United States)

Yuan, Shunda; Chou, I-Ming; Burruss, Robert A.

2013-01-01

Elemental sulfur, as a transient intermediate compound, by-product, or catalyst, plays significant roles in thermochemical sulfate reduction (TSR) reactions. However, the mechanisms of the reactions in S-H2O-hydrocarbons systems are not clear. To improve our understanding of reaction mechanisms, we conducted a series of experiments between 200 and 340 °C for S-H2O-CH4, S-D2O-CH4, and S-CH4-1m ZnBr2 systems in fused silica capillary capsules (FSCC). After a heating period ranging from 24 to 2160 hours (hrs), the quenched samples were analyzed by Raman spectroscopy. Combined with the in situ Raman spectra collected at high temperatures and pressures in the S-H2O and S-H2O-CH4 systems, our results showed that (1) the disproportionation of sulfur in the S-H2O-CH4 system occurred at temperatures above 200 °C and produced H2S, SO42-, and possibly trace amount of HSO4-; (2) sulfate (and bisulfate), in the presence of sulfur, can be reduced by methane between 250 and 340 °C to produce CO2 and H2S, and these TSR temperatures are much closer to those of the natural system (2O-CH4 system may take place simultaneously, with TSR being favored at higher temperatures; and (4) in the system S-D2O-CH4, both TSR and the competitive disproportionation reactions occurred simultaneously at temperatures above 300 °C, but these reactions were very slow at lower temperatures. Our observation of methane reaction at 250 °C in a laboratory time scale suggests that, in a geologic time scale, methane may be destroyed by TSR reactions at temperatures > 200 °C that can be reached by deep drilling for hydrocarbon resources.

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.

(E-2-{[(4-Anilinophenylimino]methyl}-4-bromo-5-fluorophenol

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Sedanur Kalecik

2017-12-01

Full Text Available In the title compound, C19H14BrFN2O, the dihedral angles between the central benzene ring and the pendant trisubstituted ring and phenyl group are 25.7 (2 and 51.7 (2°, respectively. The molecular conformation is influenced by an intramolecular O—H...N hydrogen bond. In the crystal, N—H...O hydrogen bonds link molecules into C(11 chains propagating in [100] and weak aromatic π–π stacking is also observed [centroid–centroid separation = 3.682 (3 Å

Double molybdates in Li2MoO4 - Na2MoO4 - H2O system at 25 grad C

International Nuclear Information System (INIS)

Karov, Z.G.; Mirzoev, R.S.; Makitova, D.D.; Zhilova, S.B.; Podnek, A.G.; Urusova, R.Kh.

1989-01-01

Solubility in Li 2 MoO 4 - Na 2 MoO 4 - H 2 O system at 25 deg C is first stuied. Formation of two Li 2 MoO 4 · Na 2 MoO 4 · 4H 2 O and Li 2 MoO 4 · 3Na 2 MoO 4 · 12H 2 O compounds in a system is ascertained. Density, refractive index, viscosity, surface tension, electric conductivity and pH of saturated solutions are determined. Isothermes of mole volume, equivalent and reduced electric conductivity and seeming mole volume of salts sum in solutions are calculated. All these properties adequtely confirm the character of components interaction in a system determined by solubility method. Crystallhydrates of binary molybdates are separated, indentified and studied

Structural variability in neptunium(V) oxalate compounds: synthesis and structural characterization of Na2NpO2(C2O4)OH.H2O.

Science.gov (United States)

Bean, Amanda C; Garcia, Eduardo; Scott, Brian L; Runde, Wolfgang

2004-10-04

Reaction of a (237)Np(V) stock solution in the presence of oxalic acid, calcium chloride, and sodium hydroxide under hydrothermal conditions produces single crystals of a neptunium(V) oxalate, Na(2)NpO(2)(C(2)O(4))OH.H(2)O. The structure consists of one-dimensional chains running down the a axis and is the first example of a neptunium(V) oxalate compound containing hydroxide anions.

1-O-Acetyl-3,4,6-tri-O-benzyl-2-C-bromomethyl-2-deoxy-α-d-glucopyranose

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Henok H. Kinfe

2013-01-01

Full Text Available In the title compound, C30H33BrO6, the pyranose ring adopts a chair conformation. Two of the O-benzyl phenyl rings lie almost perpendicular to C/C/C/O plane formed by the ring atoms not attached to these O-benzyl phenyl rings, and form dihedral angles of 85.1 (2 and 64.6 (2°, while the third O-benzyl phenyl ring is twisted so that it makes a dihedral angle 34.9 (2° to this C/C/C/O plane. This twist is ascribed to the formation of an S(8 loop stabilized by a weak intramolecular C—H...O hydrogen bond.

[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-[4-(4-Fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-3-yl]-1-methylpyridinium iodide–4-[3-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-4-yl]-1-methylpyridinium iodide (0.6/0.4

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Simona Margutti

2008-01-01

Full Text Available The crystal structure of the title compound, C16H16FN2O2+·I−, was determined as part of a study of the biological activity of isoxazolone derivatives as p38 mitogen-activated protein kinase (MAPK inhibitors. The X-ray crystal structure of 4-[4-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-3-yl]-1-methylpyridinium iodide showed the presence of the regioisomer 4-[3-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-4-yl]-1-methylpyridinium iodide. The synthesis of the former compound was achieved by reacting 4-(4-fluorophenyl-3-(4-pyridylisoxazol-5(2H-one after treatment with Et3N in dimethylformamide, with iodomethane. The unexpected formation of the regioisomer could be explained by a rearrangement occurring via aziridine of the isoxazolone compound. The regioisomers have site occupancies of 0.632 (4/0.368 (4. The two six members rings make a dihedral angle of 66.8 (2°.

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-Dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylato-κ2O4,O5(4-oxido-2-oxo-1,2-dihydropyrimidine-5-carboxylato-κ2O4,O5bis(1,10-phenanthroline-κ2N,N′yttrium(III dihydrate

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Zilu Chen

2008-09-01

Full Text Available In the title compound, [Y(C5H2N2O4(C5H3N2O4(C12H8N22]·2H2O, the YIII ion lies on a twofold rotation axis and exhibits a distorted square-antiprismatic coordination geometry. It is chelated by two 1,10-phenanthroline ligands, a 2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate monoanion and a 4-oxido-2-oxo-1,2-dihydropyrimidine-5-carboxylate dianion. The H atom involved in an N—H...N hydrogen bond between the 1,2-dihydropyrimidine units has half occupancy and is disordered around a twofold rotation axis.

Complexing in the system Rb2SeO4-UO2SeO4-H2O

International Nuclear Information System (INIS)

Kuchumova, N.V.; Shtokova, I.P.; Serezhkina, L.B.; Serezhkin, V.N.

1989-01-01

Method of isothermal solubility at 25 deg C is used to study interaction of rubidium and uranyl selenates in aqueous solution. Formation of congruently soluble Rb 2 UO 2 (SeO 4 ) 2 x2H 2 O and Rb 2 (UO 2 ) 2 x(SeO 4 ) 3 x6H 2 O is stated. For the last compound crystallographic characteristics (a=10.668; b=14.935(9); c=13.891(7) A; β=104.94(1); Z=4, sp.gr. P2 1 /c) are determined. Thermal decomposition of a compound results in formation of Rb 2 U 2 O 7

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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.

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

Science.gov (United States)

Bulatov, Evgeny; Chulkova, Tatiana; Haukka, Matti

2014-01-01

The title compound, C16H12N2O, exists in the crystalline state as the 5-imino-3,4-di­phenyl­-1H-pyrrol-2-one tautomer. The dihedral angles between the pyrrole and phenyl rings are 35.3 (2) and 55.3 (2)°. In the crystal, inversion dimers linked by pairs of N—H⋯N hydrogen bonds generate a graph-set motif of R 2 2(8) via N—H⋯N hydrogen bonds. PMID:24764881

Compound effect of CaCO3 and CaSO4·2H2O on the strength of steel slag: cement binding materials

International Nuclear Information System (INIS)

Qi, Liqian; Liu, Jiaxiang; Liu, Qian

2016-01-01

In this study, we replaced 30% of the cement with steel slag to prepare binding material; additionally, small amounts of CaCO 3 and CaSO 4 ·2H 2 O were added. This was done to study the compound effect of CaCO 3 and CaSO 4 ·2H 2 O on the strength of steel slag-cement binding materials. The hydration degree of the steel slag cementitious material was analyzed by XRD, TG and SEM. The results showed that the optimum proportions of CaCO 3 and CaSO 4 ·2H 2 O were 3% and 2%, respectively. Compared with the steel slag-cement binders without adding CaCO 3 and CaSO 4 ·2H 2 O, the compressive strength increased by 59.9% at 3 days and by 17.8% at 28 days. Acting as the nucleation matrix, CaCO 3 could accelerate the hydration of C 3 S. In addition, CaCO 3 was involved in the hydration reaction, generating a new hydration product, which could stably exist in a slurry. Meanwhile, CaSO 4 ·2H 2 O could increase the number of AFt. The compound effect of CaCO 3 and CaSO 4 ·2H 2 O enhanced the intensity of steel slag-cement binding materials and improved the whole hydration behavior. (author)

(E-3-Hydroxy-13-methyl-16-[4-(methylsulfanylbenzylidene]-7,8,9,11,12,13,15,16-octahydro-6H-cyclopenta[a]phenanthren-17(14H-one

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R. Murugan

2009-01-01

Full Text Available In the title compound, C26H28O2S, the dihedral angles between the mean plane of the five membered ring and the 4-(methylsulfanylbenzylidine ring in the two crystallographically independent molecules are 34.05 (10 and 40.53 (15°. The packing is stabilized by intermolecular O—H...O and C—H...O interactions.

1,4-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.

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.

Hydrazinium lanthanide oxalates: synthesis, structure and thermal reactivity of N_2H_5[Ln_2(C_2O_4)_4(N_2H_5)].4H_2O, Ln = Ce, Nd

International Nuclear Information System (INIS)

De Almeida, Lucie; Grandjean, Stephane; Abraham, Francis; Rivenet, Murielle; Patisson, Fabrice

2014-01-01

New hydrazinium lanthanide oxalates N_2H_5[Ln_2(C_2O_4)_4(N_2H_5)].4H_2O, Ln = Ce (Ce-H_yO_x) and Nd (Nd- H_yO_x), were synthesized by hydrothermal reaction at 150 C between lanthanide nitrate, oxalic acid and hydrazine solutions. The structure of the Nd compound was determined from single-crystal X-ray diffraction data, space group P2_1/c with a = 16.315(4), b = 12.127(3), c = 11.430(2) Angstroms, β = 116.638(4) degrees, V = 2021.4(7) Angstroems"3, Z = 4, and R1 = 0.0313 for 4231 independent reflections. Two distinct neodymium polyhedra are formed, NdO_9 and NdO_8N, an oxygen of one monodentate oxalate in the former being replaced by a nitrogen atom of a coordinated hydrazinium ion in the latter. The infrared absorption band at 1005 cm"-"1 confirms the coordination of N_2H_5"+ to the metal. These polyhedra are connected through μ"2 and μ"3 oxalate ions to form an anionic three-dimensional neodymium-oxalate arrangement. A non-coordinated charge-compensating hydrazinium ion occupies, with water molecules, the resulting tunnels. The N-N stretching frequencies of the infrared spectra demonstrate the existence of the two types of hydrazine ions. Thermal reactivity of these hydrazinium oxalates and of the mixed isotypic Ce/Nd (CeNd-H_yO_x) oxalate were studied by using thermogravimetric and differential thermal analyses coupled with gas analyzers, and high temperature X-ray diffraction. Under air, fine particles of CeO_2 and Ce_0_._5Nd_0_._5O_1_._7_5 are formed at low temperature from Ce-H_yO_x and CeNd-H_yO_x, respectively, thanks to a decomposition/oxidation process. Under argon flow, dioxy-mono-cyanamides Ln_2O_2CN_2 are formed. (authors)

Nd2(SeO3)2(SeO4) . 2H2O - a mixed-valence compound containing selenium in the oxidation states +IV and +VI

International Nuclear Information System (INIS)

Berdonosov, P.S.; Dityat'yev, O.A.; Dolgikh, V.A.; Schmidt, P.; Ruck, Michael; Lightfoot, P.

2004-01-01

Pale pink crystals of Nd 2 (SeO 3 ) 2 (SeO 4 ) . 2H 2 O were synthesized under hydrothermal conditions from H 2 SeO 3 and Nd 2 O 3 at about 200 C. X-ray diffraction on powder and single-crystals revealed that the compound crystallizes with the monoclinic space group C 2/c (a = 12.276(1) A, b = 7.0783(5) A, c = 13.329(1) A, β = 104.276(7) ). The crystal structure of Nd 2 (SeO 3 ) 2 (SeO 4 ) . 2H 2 O is an ordered variant of the corresponding erbium compound. Eight oxygen atoms coordinate the Nd III atom in the shape of a bi-capped trigonal prism. The oxygen atoms are part of pyramidal (Se IV O 3 ) 2- groups, (Se VI O 4 ) 2- tetrahedra and water molecules. The [NdO 8 ] polyhedra share edges to form chains oriented along [010]. The selenate ions link these chains into layers parallel to (001). The layers are interconnected by the selenite ions into a three-dimensional framework. The dehydration of Nd 2 (SeO 3 ) 2 (SeO 4 ) . 2H 2 O starts at 260 C. The thermal decomposition into Nd 2 SeO 5 , SeO 2 and O 2 at 680 C is followed by further loss of SeO 2 leaving cubic Nd 2 O 3 . (Abstract Copyright [2004], Wiley Periodicals, Inc.) [de

Co3(PO4)2·4H2O

Science.gov (United States)

Lee, Young Hoon; Clegg, Jack K.; Lindoy, Leonard F.; Lu, G. Q. Max; Park, Yu-Chul; Kim, Yang

2008-01-01

Single crystals of Co3(PO4)2·4H2O, tricobalt(II) bis­[ortho­phosphate(V)] tetra­hydrate, were obtained under hydro­thermal conditions. The title compound is isotypic with its zinc analogue Zn3(PO4)2·4H2O (mineral name hopeite) and contains two independent Co2+ cations. One Co2+ cation exhibits a slightly distorted tetra­hedral coordination, while the second, located on a mirror plane, has a distorted octa­hedral coordination environment. The tetra­hedrally coordinated Co2+ is bonded to four O atoms of four PO4 3− anions, whereas the six-coordinate Co2+ is cis-bonded to two phosphate groups and to four O atoms of four water mol­ecules (two of which are located on mirror planes), forming a framework structure. In addition, hydrogen bonds of the type O—H⋯O are present throughout the crystal structure. PMID:21200978

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

International Nuclear Information System (INIS)

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

1994-01-01

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

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.

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

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Ravell Bengiat

2016-07-01

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

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.

cyclo-Tetrakis(μ-3-acetyl-4-methyl-1H-pyrazole-5-carboxylato-κ4N2,O3:N1,O5tetrakis[aquacopper(II] tetradecahydrate

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Sergey Malinkin

2011-09-01

Full Text Available The title compound, [Cu4(C7H6N2O34(H2O4]·14H2O, a tetranuclear [2 × 2] grid-type complex with S4 symmetry, contains four CuII atoms which are bridged by four pyrazolecarboxylate ligand anions and are additionally bonded to a water molecule. Each CuII atom is coordinated by two O atoms of the carboxylate and acetyl groups, two pyrazole N atoms of doubly deprotonated 3-acetyl-4-methyl-1H-pyrazole-5-carboxylic acid and one O atom of a water molecule. The geometry at each CuII atom is distorted square-pyramidal, with the two N and two O atoms in the equatorial plane and O atoms in the axial positions. O—H...O hydrogen-bonding interactions additionally stabilize the structure. One of the uncoordinated water molecules shows half-occupancy.

4-Fluoro-N-methyl-N-(1,2,3,4-tetrahydrocarbazol-3-ylbenzenesulfonamide

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Kaspar Gothardt Rasmussen

2009-04-01

Full Text Available In the title compound, C19H19FN2O2S, the hydrogenated six-membered ring of the carbazole unit adopts a half-chair conformation and the plane of the fluorophenyl ring forms a dihedral angle of 41.5 (1° with respect to the carbazole mean plane. The crystal structure is segregated into layers containing the carbazole units and fluorophenyl rings in alternate (200 planes. The carbazole units form centrosymmetric face-to-face interactions [interplanar separation = 4.06 (1 Å] and edge-to-face interactions in which the N—H group is directed towards an adjacent carbazole face, with a shortest H...C contact of 2.53 Å. The fluorophenyl rings form face-to-face contacts with an approximate interplanar separation of 3.75 Å and a centroid–centroid distance of 4.73 (1 Å.

Preparation, Characterization, and Structure of Two Layered Molybdenum(VI) Phosphates: KMo(H 2O)O 2PO 4 and NH 4Mo(H 2O)O 2PO 4

Science.gov (United States)

Millini, Roberto; Carati, Angela

1995-08-01

New layered Mo(VI) compounds, KMo(H 2O)O 2PO 4 (I) and NH 4Mo(H 2O)O 2PO 4 (II), were synthesized hydrothermally and their structures were determined from single-crystal X-ray analysis. Compounds (I) and (II) are isostructural and crystallize in the monoclinic P2 1/ n space group with a = 12.353(3), b = 8.623(2), c = 5.841(1) Å, β = 102.78(1)°, V = 606.8(2) Å 3, Z = 4, and R = 0.027 ( Rw = 0.030) for compound (I) and a = 12.435(3), b = 8.761(2), c = 6.015(1), β = 103.45(1)°, V = 637.3(2) Å 3, Z = 4, and R = 0.040 ( Rw = 0.041) for compound (II). The structure consists of layers built up of eight- and four-membered rings resulting from the alternation of corner-sharing [MoO 6] octahedra and [PO 4] tetrahedra. The layers stack along the (1¯01) direction by intercalating K and NH 4 ions.

Design and syntheses of hybrid metal-organic materials based on K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] metallotectons

Science.gov (United States)

Sun, Yayong; Zong, Yingxia; Ma, Haoran; Zhang, Ao; Liu, Kang; Wang, Debao; Wang, Wenqiang; Wang, Lei

2016-05-01

By using K3[M(C2O4)3]·3H2O [M(III)=Fe, Al, Cr] (C2O42-=oxalate) metallotectons as the starting material, we have synthesized eight novel complexes with formulas [{Fe(C2O4)2(H2O)2}2]·(H-L1)2·H2O 1, [Fe(C2O4)Cl2]·(H2-L2)0.5·(L2)0.5·H2O 2, [{Fe(C2O4)1.5Cl2}2]·(H-L3)43, [Fe2(C2O4)Cl8]·(H2-L4)2·2H2O 4, K[Al(C2O4)3]·(H2-L5)·2H2O 5, K[Al(C2O4)3]·(H-L6)2·2H2O 6, K[Cr(C2O4)3]·2H2O 7, Na[Fe(C2O4)3]·(H-L6)2·2H2O 8 (with L1=4-dimethylaminopyridine, L2=2,3,5,6-tetramethylpyrazine, L3=2-aminobenzimidazole, L4=1,4-bis-(1H-imidazol-1-yl)benzene, L5=1,4-bis((2-methylimidazol-1-yl)methyl)benzene, L6=2-methylbenzimidazole). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra and thermogravimetric analyses. Compound 3 is a 2D H-bonded supramolecular architecture. Others are 3D supramolecular structures. Compound 1 shows a [Fe(C2O4)2(H2O)2]- unit and 3D antionic H-bonded framework. Compound 2 features a [Fe(C2O4)Cl2]- anion and 1D iron-oxalate-iron chain. Compound 3 features a [Fe2(C2O4)3Cl4]4- unit. Compound 4 features distinct [Fe2(C2O4)Cl8]4- units, which are mutual linked by water molecules to generated a 2D H-bonded network. Compound 5 features infinite ladder-like chains constructed by [Al(C2O4)3]3- units and K+ cations. The 1D chains are further extended into 3D antionic H-bonded framework through O-H···O H-bonds. Compounds 6-8 show 2D [KAl(C2O4)3]2- layer, [KCr(C2O4)3]2- layer and [NaFe(C2O4)3]2- layer, respectively.

2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate

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Guoquan Zhou

2012-04-01

Full Text Available The title compound, C6H7O2S3+·BF4−, consists of a planar 2-thioxo-1,3-dithiol-4,5-yl unit [maximum deviation from the ring plane = 0.020 (3 Å], with an ethylenedioxy group fused at the 4,5-positions; the ethylenedioxy C atoms are disordered over two positions with site-occupancy factors of 0.5. The 1,4-dioxine ring has a twist-chair conformation. Weak cation–anion S...F interactions [3.022 (4–3.095 (4 Å] and an S...O [3.247 (4 Å] interaction are present.

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.

3,5-Bis[1-acetyl-5-(4-chlorophenyl-4,5-dihydro-1H-pyrazol-3-yl]-2,6-dimethylpyridine tetrahydrofuran solvate

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Qun Qian

2008-07-01

Full Text Available In the title compound, C29H27Cl2N5O2·C4H8O, the polycyclic system is composed of three parts: one central pyridine ring substituted by two functionalized pyrazoline rings. The dihedral angles between the central pyridine plane and pyrazoline planes are 5.11 (1 and 13.99 (1°, whereas the dihedral angles between each chlorophenyl plane and the attached pyrazoline planes are 88.65 (1 and 83.87 (1°. Molecules are linked by intermolecular C—H...O hydrogen bonds, forming a three-dimensional network.

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

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Suman Sinha

2011-12-01

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

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.

Hydrothermal synthesis and crystal structure of a new molybdenum oxide compound with manganese-o-phen subunit: [Mn(o-phen)(H2O)MoO4]·H2O (o-phen=o-phenanthroline)

International Nuclear Information System (INIS)

Zhang Quanzheng; Lu Canzhong; Yang Wenbin; Chen Shumei; Yu Yaqin; He Xiang; Yan Ying; Liu Jiuhui; Xu Xinjiang; Xia Changkun; Wu Xiaoyuan; Chen Lijuan

2004-01-01

A new one-dimensional molybdenum oxide compound with manganese-o-phen subunit: [Mn(o-phen)(H 2 O)MoO 4 ]·H 2 O (1) (o-phen=o-phenanthroline) was synthesized by the hydrothermal reaction of Na 2 MoO 4 ·2H 2 O, MnSO 4 ·H 2 O, oxalic acid, o-phenanthroline (o-phen) and water. Its structure was determined by elemental analyses, ESR spectrum, TG analysis, IR spectrum and single-crystal X-ray diffraction. Compound 1 crystallizes in triclinic system, space group P-1 with a=7.0401(2) A, b=10.4498(2) A, c=10.5720(2) A, α=73.26(7) deg., β=83.34(8) deg., γ=77.33(9) deg., V=725.5089(0) A 3 , Z=2, and R 1 =0.0322 for 2337 observed reflections. Compound 1 exhibits one-dimensional chain structure. The chains are linked up via hydrogen bonding to 2D layers, which are further assembled through π-π stacking interactions to a 3D supermolecular structure

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

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Yan Jiang

2012-02-01

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

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.

Production of 34S-labeled gypsum (Ca34SO4.2H2O Produção de gesso (Ca34SO4.2H2O, marcado com 34S

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Alexssandra Luiza Rodrigues Molina Rossete

2006-08-01

Full Text Available Agricultural gypsum (CaSO4.2H2O stands out as an effective source of calcium and sulfur, and to control aluminum saturation in the soil. Labeled as 34S it can elucidate important aspects of the sulfur cycle. Ca34SO4.2H2O was obtained by chemical reaction between Ca(OH2 and H2(34SO4, performed under slow agitation. The acid was produced by ion exchange chromatography using the Dowex 50WX8 cation exchange resin and a Na2(34SO4 eluting solution. After precipitation, the precipitate was separated and dried in a ventilated oven at 60ºC. From 2.2 L H2SO4 0.2 mol L-1 and 33.6 g Ca(OH2, 73.7 ± 0.6 g Ca34SO4.2H2O were produced on average in the tests, representing a mean yield of 94.6 ± 0.8%, with 98% purity. The 34SO2 gas was obtained from Ca34SO4.2H2O in the presence of NaPO3 in a high vacuum line and was used for the isotopic determination of S in an ATLAS-MAT model CH-4 mass spectrometer.O gesso agrícola (CaSO4.2H2O destaca-se como fonte eficiente de cálcio e enxofre e na redução da saturação de alumínio no solo. O 34S como traçador isotópico pode elucidar aspectos importantes no ciclo do enxofre. Para tanto o Ca34SO4.2H2O foi obtido por reação química entre o Ca(OH2 e solução de H2(34SO4, realizada sob agitação lenta. O ácido foi produzido por cromatografia de troca iônica, utilizando resina catiônica Dowex 50WX8 e solução eluente de Na2(34SO4. Após a precipitação foi separado o precipitado e realizada a secagem em estufa ventilada à temperatura de 60ºC. Nos testes, a partir de 2,2 L de H2SO4 0,2 mol L-1 e 33,6 g de Ca(OH2, foram produzidos em média 73,7 ± 0,6 g de Ca34SO4.2H2O representando um rendimento médio de 94,6 ± 0,8%, com pureza de 98%. A partir do Ca34SO4.2H2O na presença de NaPO3, em linha de alto vácuo, obteve-se o gás 34SO2 utilizado para a determinação isotópica do S no espectrômetro de massas ATLAS-MAT modelo CH-4.

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

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Bianca Barreto Martins

2017-07-01

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

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.

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.

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

OpenAIRE

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

2008-01-01

In the title compound, C26H28O2S, the dihedral angles between the mean plane of the five membered ring and the 4-(methylsulfanyl)benzylidine ring in the two crystallographically independent molecules are 34.05 (10) and 40.53 (15)°. The packing is stabilized by intermolecular O—H...O and C—H...O interactions.

Electrodeposition mechanism of quaternary compounds Cu2ZnSnS4: Effect of the additives

Science.gov (United States)

Tang, Aiyue; Li, Zhilin; Wang, Feng; Dou, Meiling; Liu, Jingjun; Ji, Jing; Song, Ye

2018-01-01

The electrodeposition mechanism of pure phase Cu2ZnSnS4 (CZTS) thin film with subsequent annealing was investigated in detail. An electrolyte design principle of quaternary compounds was proposed. The complex ions of Cu(H2C6H5O7)+, Cu2(C6H5O7)+, Zn(C4H5O6)+, Sn(H2C6H5O7)+ and Sn2(C6H5O7)+, which influenced the reduction process and played important roles in co-deposition, were identified by UV spectra. Electrochemical studies indicated that trisodium citrate and tartaric acid could narrow the co-deposition potential range of the four elements to -0.8 V to -1.2 V (vs. SCE). The cause was the synergetic effect that trisodium citrate inhibited the reduction of Cu2+ and Sn2+ and tartaric acid promoted the reduction of Zn2+. The reduction of S2O32- was mainly attributed to the induction effect of the metallic ions, and the H+ dissociated from tartaric acid could also promote the cathode process of S2O32-. The reaction mechanism could be summarized as the following steps: (I) Cu(H2C6H5O7)+, Cu2(C6H5O7)+ → Cu, Sn(H2C6H5O7)+, Sn2(C6H5O7)+ → Sn, Zn(C4H5O6)+ → Zn; (II) the desorption of (H2C6H5O7)- and (C6H5O7)-, and the reduction of S2O32- induced by metallic ions and H+. The mechanism studies provided a path of electrolyte design for multicomponent compounds.

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.

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.

Crystal structure of 2-amino-N-(2-fluorophenyl-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide

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K. Chandra Kumar

2015-11-01

Full Text Available In the title compound, C15H15FN2OS, the dihedral angle between the planes of the benzothiophene ring system and the fluorobenzene ring is 3.74 (14°. The six-membered ring of the benzothiophene moiety adopts a half-chair conformation. The molecular conformation is consolidated by intramolecular N—H...F and N—H...O hydrogen bonds. In the crystal, molecules are linked by N—H...O hydrogen bonds, generating C(6 [001] chains.

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

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Salima Thabti

2013-04-01

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

(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.

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.

Hydrazinium lanthanide oxalates: synthesis, structure and thermal reactivity of N2H5[Ln2(C2O4)4(N2H5)]·4H2O, Ln = Ce, Nd.

Science.gov (United States)

De Almeida, Lucie; Grandjean, Stéphane; Rivenet, Murielle; Patisson, Fabrice; Abraham, Francis

2014-03-28

New hydrazinium lanthanide oxalates N2H5[Ln2(C2O4)4(N2H5)]·4H2O, Ln = Ce (Ce-HyOx) and Nd (Nd-HyOx), were synthesized by hydrothermal reaction at 150 °C between lanthanide nitrate, oxalic acid and hydrazine solutions. The structure of the Nd compound was determined from single-crystal X-ray diffraction data, space group P2₁/c with a = 16.315(4), b = 12.127(3), c = 11.430(2) Å, β = 116.638(4)°, V = 2021.4(7) Å(3), Z = 4, and R1 = 0.0313 for 4231 independent reflections. Two distinct neodymium polyhedra are formed, NdO9 and NdO8N, an oxygen of one monodentate oxalate in the former being replaced by a nitrogen atom of a coordinated hydrazinium ion in the latter. The infrared absorption band at 1005 cm(-1) confirms the coordination of N2H5(+) to the metal. These polyhedra are connected through μ2 and μ3 oxalate ions to form an anionic three-dimensional neodymium-oxalate arrangement. A non-coordinated charge-compensating hydrazinium ion occupies, with water molecules, the resulting tunnels. The N-N stretching frequencies of the infrared spectra demonstrate the existence of the two types of hydrazine ions. Thermal reactivity of these hydrazinium oxalates and of the mixed isotypic Ce/Nd (CeNd-HyOx) oxalate were studied by using thermogravimetric and differential thermal analyses coupled with gas analyzers, and high temperature X-ray diffraction. Under air, fine particles of CeO2 and Ce(0.5)Nd(0.5)O(1.75) are formed at low temperature from Ce-HyOx and CeNd-HyOx, respectively, thanks to a decomposition/oxidation process. Under argon flow, dioxymonocyanamides Ln2O2CN2 are formed.

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

OpenAIRE

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

2017-01-01

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

2-(4-Fluorobenzylidenepropanedinitrile: monoclinic polymorph

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Ahmed M. El-Agrody

2013-04-01

Full Text Available The title compound, C10H5FN2, is a monoclinic (P21/c polymorph of the previously reported triclinic (P-1 form [Antipin et al. (2003. J. Mol. Struct. 650, 1–20]. The 13 non-H atoms in the title polymorph are almost coplanar (r.m.s. deviation = 0.020 Å; a small twist between the fluorobenzene and dinitrile groups [C—C—C—C torsion angle = 175.49 (16°] is evident in the triclinic polymorph. In the crystal, C—H...N interactions lead to supramolecular layers parallel to (-101; these are connected by C—F...π interactions.

Synthesis, crystal structure, thermal analysis and dielectric properties of Rb4(SO4)(HSO4)2(H3AsO4) compound

Science.gov (United States)

Belhaj Salah, M.; Nouiri, N.; Jaouadi, K.; Mhiri, T.; Zouari, N.

2018-01-01

A new inorganic Rb4(SO4)(HSO4)2(H3AsO4) compound was prepared. It was found to crystallize in the monoclinic system (P21 space group) with the following lattice parameters: a = 5868 (1) Å, b = 13,579(2) Å, c = 11,809 (3) Å and β = 94,737 (1)°. The structure is characterized by SO42-, HSO4- and H3AsO4 tetrahedra connected by hydrogen bridge to form two types of dimmer (H(8)S(2)O4- … S(1)O42- and H(12)S(2)O4- … H3AsO4). These dimmers are interconnected by both hydrogen bonds O(14)sbnd H(14)· · ·O(4) and O(15)sbnd H(15)· · ·O(2). They are also linked by the hydrogen bridge assured by the hydrogen atoms H(2), H(3) and H(4) of the H3AsO4 group to build the chain S(1)O4⋯H3AsO4 which are parallel to the ''a'',direction. The rubidium cations are coordinated by eight oxygen atoms with Rbsbnd O distance ranging from 2893(8) to 3.415(6) Å. The existence of Osbnd H and (S/As)sbnd O bonds in the structure at room temperature has been confirmed by IR and Raman spectroscopy in the frequency ranges 4000-400 cm-1and 1200 - 50 cm-1, respectively. Thermal analysis of Rb4(HSO4)(HSO4)2(H3AsO4) showed that the transformation to high temperature phase occurs at 407 K by one-step process. Thermal decomposition of the product takes place at much higher temperatures, with an onset of approximately 522 K. The first transition detected by differential scanning calorimetry (DSC) was also analyzed by dielectric and conductivity measurements using the impedance spectroscopy techniques. The conductivity in the high temperature phase at 428 K is 1.04 × 10-3 Ω-1 cm-1, and the activation energy for the proton transport is 0.36 eV. The conductivity relaxation parameters associated with the high disorder protonic conduction have been examined from analysis of the M"/M"max spectrum measured in a wide temperature range. Transport properties of this material appear to be due to the proton hopping mechanism. The obtained results show that this transition is protonic by nature.

Triaqua(1,10-phenanthroline-2,9-dicarboxylatocobalt(II dihydrate

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Zi-Fa Shi

2010-04-01

Full Text Available The title compound, [Co(C14H6N2O4(H2O3]·2H2O, has twofold crystallographic symmetry. The CoII atom is in a distorted pentagonal-bipyramidal coordination environment with two N atoms and two O atoms from a tetradentate 1,10-phenanthroline-2,9-dicarboxylate ligand and one O atom from a water molecule forming the pentagonal plane, and two O atoms from two water molecules occupying axial positions. In the crystal, adjacent molecules are linked by O—H...O hydrogen bonds, forming a three-dimensional network.

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

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Sibi Narayanan

2012-12-01

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

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

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Narsimha Reddy Penthala

2009-08-01

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

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

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Eser Ihan

2008-10-01

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

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

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S. Sriman Narayanan

2008-09-01

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

(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].

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.

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

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Chi-Xiao Zhang

2013-02-01

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

(2RS-2-(2,4-Difluorophenyl-1-[(4-iodobenzyl(methylamino]-3-(1H-1,2,4-triazol-1-ylpropan-2-ol

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Hui-Ping Xiong

2012-08-01

Full Text Available In the title compound (common name: iodiconazole, C19H19F2IN4O, there is an intramolecular O—H...N hydrogen bond and molecules are linked by weak interactions only, namely C—H...N, C—H...O and C—H...F hydrogen bonds, and π-electron ring–π-electron ring interactions between the triazole rings with centroid–centroid distances of 3.725 (3 Å.

6-(4-Bromophenyl-2-(4-fluorobenzylimidazo[2,1-b][1,3,4]thiadiazole

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Afshan Banu

2011-04-01

Full Text Available In the title compound, C17H11BrFN3S, the imidazothiadiazole and bromophenyl rings are individually almost planar, with maximum deviations of 0.0215 (4 and 0.0044 (4 Å, respectively, and are inclined at an angle of 27.34 (3° with respect to each other. The dihedral angle between the mean planes of the fluorobenzyl and imidazothiadiazole rings is 79.54 (3°. The crystal structure is stabilized by intermolecular C—H...N interactions resulting in chains of molecules along the b axis.

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

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Nada Kheira Sebbar

2016-06-01

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

Uniaxially oriented polycrystalline thin films and air-stable n-type transistors based on donor-acceptor semiconductor (diC8BTBT)(FnTCNQ) [n = 0, 2, 4

Science.gov (United States)

Shibata, Yosei; Tsutsumi, Jun'ya; Matsuoka, Satoshi; Matsubara, Koji; Yoshida, Yuji; Chikamatsu, Masayuki; Hasegawa, Tatsuo

2015-04-01

We report the fabrication of high quality thin films for semiconducting organic donor-acceptor charge-transfer (CT) compounds, (diC8BTBT)(FnTCNQ) (diC8BTBT = 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene and FnTCNQ [n = 0,2,4] = fluorinated derivatives of 7,7,8,8,-tetracyanoquinodimethane), which have a high degree of layered crystallinity. Single-phase and uniaxially oriented polycrystalline thin films of the compounds were obtained by co-evaporation of the component donor and acceptor molecules. Organic thin-film transistors (OTFTs) fabricated with the compound films exhibited n-type field-effect characteristics, showing a mobility of 6.9 × 10-2 cm2/V s, an on/off ratio of 106, a sub-threshold swing of 0.8 V/dec, and an excellent stability in air. We discuss the suitability of strong intermolecular donor-acceptor interaction and the narrow CT gap nature in compounds for stable n-type OTFT operation.

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.

2,2,6-Trimethyl-5-[2-(4-methylphenylethynyl]-4H-1,3-dioxin-4-one

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Ignez Caracelli

2009-11-01

Full Text Available The 1,3-dioxin-4-one ring in the title compound, C16H16O3, is in a half-boat conformation with the quaternary O—C(CH32—O atom lying 0.546 (1 Å out of the plane defined by the remaining five atoms. The crystal structure is consolidated by C—H...O contacts that lead to supramolecular layers.

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.

[Disulfanediylbis(ferrocenylthiophosphinato-κ2O,O]titanocene tetrahydrofuran trisolvate

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Mehmet Karakus

2012-04-01

Full Text Available The title compound, [Fe2Ti(C5H54(C10H8O2P2S4]·3C4H8O, contains a central seven-membered TiO2P2S2 ring with a very similar geometry compared to the derivative showing anisyl instead of ferrocenyl substituents, the Ti—O distance being marginally longer for the anisyl derivative. Two tetrahydrofuran solvent molecules are each disordered on a twofold axis.

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

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Ning-Juan Zheng

2012-04-01

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

Crystal structure of (E-2-benzylidene-4-[(3-phenyl-4,5-dihydroisoxazol-5-ylmethyl]-2H-benzo[b][1,4]thiazin-3(4H-one

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Nada Kheira Sebbar

2015-06-01

Full Text Available In the title compound, C25H20N2O2S, the dihydroisoxazole ring exhibits an envelope conformation with the methine atom being the flap, while the 1,4-thiazine ring displays a screw-boat conformation. The six-membered ring fused to the 1,4-thiazine ring makes dihedral angles of 63.04 (2 and 54.7 (2° with the mean planes through the five-membered heterocycle and the attached phenyl ring, respectively. The phenyl group connected to the 1,4-thiazine ring is disordered over two sites [major component = 0.57 (2]. The most prominent interactions in the crystal structure are C—H...O hydrogen bonds that link molecules, forming inversion dimers, and C—H...N hydrogen bonds that link the dimers into columns parallel to the b axis.

Synthesis, crystal structure, and spectroscopic characterization of trans-bis[(mu-1,3-bis(4-pyridyl)propane)(mu-(3-thiopheneacetate-O))(3-thiopheneacetate-O)]dicopper(II), [[Cu2(O2CCH2C4H3S)4mu-(BPP)2

Science.gov (United States)

Marinho, Maria Vanda; Yoshida, Maria Irene; Guedes, Kassilio J; Krambrock, Klaus; Bortoluzzi, Adailton J; Hörner, Manfredo; Machado, Flávia C; Teles, Wagner M

2004-02-23

From the reaction between a dinuclear paddle-wheel carboxylate, namely [Cu2mu-(O2CCH2C4H3S)4] (1), and the flexible ligand 1,3-bis(4-pyridyl)propane (BPP) a neutral 2-D coordination polymer [[Cu2(O2CCH2C4H3S)4mu-(BPP)2

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

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Rajamani Raja

2015-09-01

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

Compound effect of CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O on the strength of steel slag: cement binding materials

Energy Technology Data Exchange (ETDEWEB)

Qi, Liqian; Liu, Jiaxiang; Liu, Qian, E-mail: ljxpost@263.net [Beijing Key Laboratory of Electrochemical Process and Technology for Materials, The State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing (China)

2016-03-15

In this study, we replaced 30% of the cement with steel slag to prepare binding material; additionally, small amounts of CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O were added. This was done to study the compound effect of CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O on the strength of steel slag-cement binding materials. The hydration degree of the steel slag cementitious material was analyzed by XRD, TG and SEM. The results showed that the optimum proportions of CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O were 3% and 2%, respectively. Compared with the steel slag-cement binders without adding CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O, the compressive strength increased by 59.9% at 3 days and by 17.8% at 28 days. Acting as the nucleation matrix, CaCO{sub 3} could accelerate the hydration of C{sub 3}S. In addition, CaCO{sub 3} was involved in the hydration reaction, generating a new hydration product, which could stably exist in a slurry. Meanwhile, CaSO{sub 4}·2H{sub 2}O could increase the number of AFt. The compound effect of CaCO{sub 3} and CaSO{sub 4}·2H{sub 2}O enhanced the intensity of steel slag-cement binding materials and improved the whole hydration behavior. (author)

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

International Nuclear Information System (INIS)

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

2014-01-01

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

1-(4a,8-Dimethyl-1,2,3,4,4a,5,6,8a-octahydronaphthalen-2-yl-3-(4-methylphenylprop-2-en-1-one

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Mohamed Tebbaa

2011-06-01

Full Text Available The title compound, C22H28O, was isolated from the aerial part of Inula viscosa (L Aiton [or Dittrichia viscosa (L Greuter]. The cyclohexene ring has a half-chair conformation, whereas the cyclohexane ring displays a chair conformation being substituted at position 2 by a 3-(4-methylphenylprop-2-enoyl group. In the crystal, weak intermolecular C—H...O hydrogen bonds link molecules into chains in the [010] direction.

1-[3-(2-Benzyloxy-6-hydroxy-4-methylphenyl-5-[3,5-bis(trifluoromethylphenyl]-4,5-dihydro-1H-pyrazol-1-yl]propane-1-one

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U. H. Patel

2013-06-01

Full Text Available In the title compound, C28H24F6N2O3, the mean plane of the central pyrazoline ring forms dihedral angles of 2.08 (9 and 69.02 (16° with the 2-benzyloxy-6-hydroxy-4-methylphenyl and 3,5-bis(trifluoromethylphenyl rings, respectively. The dihedral angle between the mean planes of the pyrazoline and 3,5-bis(trifluoromethylphenyl rings is 68.97 (9°. An intramolecular O—H...N hydrogen bond is observed, which forms an S(6 graph-set motif. In the crystal, pairs of weak C—H...F halogen interactions link the molecules into inversion dimers while molecular chains along [100] are formed by C—H...O contacts.

Poly[[aqua(μ2-4,4′-bipyridine-κ2N:N′[μ3-3-bromo-2-(carboxylatomethylbenzoato-κ3O1:O1′:O2]cadmium] monohydrate

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Yangmei Liu

2012-08-01

Full Text Available In the title compound, {[Cd(C9H5BrO4(C10H8N2(H2O]·H2O}n, the CdII atom has a distorted octahedral coordination geometry. Two N atoms from two 4,4′-bipyridine (bipy ligands occupy the axial positions, while the equatorial positions are furnished by three carboxylate O atoms from three 3-bromo-2-(carboxylatomethylbenzoate (bcb ligands and one O atom from a water molecule. The bipy and bcb ligands link the CdII atoms into a three-dimensional network. O—H...O hydrogen bonds and π–π interactions between the pyridine and benzene rings [centroid–centroid distance = 3.736 (4 Å] are present in the crystal.

N,N′-Bis(2-hydroxy-3-ethoxybenzylidenebutane-1,4-diamine

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Hoong-Kun Fun

2009-04-01

Full Text Available The title Schiff base compound, C22H28N2O4, lies across a crystallographic inversion centre and adopts an E configuration with respect to the C=N bond. Pairs of weak intermolecular C—H...O interactions link neighbouring molecules into dimers with an R22(28 ring motif. The crystal structure is stabilized by intermolecular C—H...π interactions. An intramolecular O—H...N hydrogen bond occurs.

Structures and electron affinities of the di-arsenic fluorides As2Fn/As2Fn- (n=1-8).

Science.gov (United States)

Kasalová, Veronika; Schaefer, Henry F

2005-04-15

Developments in the preparation of new materials for microelectronics are focusing new attention on molecular systems incorporating several arsenic atoms. A systematic investigation of the As2Fn/As2Fn- systems was carried out using Density Functional Theory methods and a DZP++ quality basis set. Global and low-lying local geometric minima and relative energies are discussed and compared. The three types of neutral-anion separations reported in this work are: the adiabatic electron affinity (EAad), the vertical electron affinity (EAvert), and the vertical detachment energy (VDE). Harmonic vibrational frequencies pertaining to the global minimum for each compound are reported. From the first four studied species (As2Fn, n=1-4), all neutral molecules and their anions are shown to be stable with respect to As-As bond breaking. The neutral As2F molecule and its anion are predicted to have Cs symmetry. We find the trans F-As-As-F isomer of C2h symmetry and a pyramidalized vinylidene-like As-As-F2- isomer of Cs symmetry to be the global minima for the As2F2 and As2F2- species, respectively. The lowest lying minima of As2F3 and As2F3- are vinyl radical-like structures F-As-As-F2 of Cs symmetry. The neutral As2F4 global minimum is a trans-bent (like Si2H4) F2-As-As-F2 isomer of C2 symmetry, while its anion is predicted to have an unusual fluorine-bridged (C(1)) structure. The global minima of the neutral As2Fn species, n=5-8, are weakly bound complexes, held together by dipole-dipole interactions. All such structures have the AsFm-AsFn form, where (m,n) is (2,3) for As2F5, (3,3) for As2F6, (4,3) for As2F7), and (5,3) for As2F8. For As2F8 the beautiful pentavalent F4As-AsF4 structure (analogous to the stable AsF5 molecule) lies about 30 kcal/mol above the AsF3 . . . AsF5 complex. The stability of AsF(5) depends crucially on the strong As-F bonds, and replacing one of these with an As-As bond (in F4As-AsF4) has a very negative impact on the molecule's stability. The anions As

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

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Hoong-Kun Fun

2009-01-01

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

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

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Seik Weng Ng

2013-03-01

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

(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.

cis-Bis[N′-(4-bromobenzoyl-N,N-dimethylthioureato-κ2O,S]copper(II

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Gün Binzet

2011-05-01

Full Text Available The asymmetric unit of the title compound, [Cu(C10H10BrN2OS2], contains two independent complex molecules with almost identical conformations. Two S and two O atoms form the coordination environment of the Cu atom, resulting in a slightly distorted square-planar coordination. The S atoms are in a cis configuration. The crystal structure is stabilized by weak intermolecular C—H...Br hydrogen-bonding interactions.

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

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Goverdhan Mehta

2012-12-01

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

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.

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.

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-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.

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.

[(Z-O-Ethyl N-(4-nitrophenylthiocarbamato-κS](triethylphosphine-κPgold(I

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Soo Yei Ho

2009-11-01

Full Text Available In the title compound, [Au(C9H9N2O3S(C6H15P], two virtually identical molecules comprise the asymmetric unit. These are connected by Au...Au [3.6796 (4 Å] and Au...S [3.6325 (18 and 3.5471 (18 Å] contacts, forming a dimeric aggregate. The presence of intramolecular Au...O contacts [2.993 (5 and 2.957 (5 Å] is responsible for the slight deviations from the ideal linear coordination environments about the AuI ions. The conformation about the central C=N double bond is Z. Supramolecular chains sustained by π–π [3.573 (4 Å] and C—H...π interactions are evident in the crystal structure. These are connected into layers via weak intermolecular C—H...O interactions involving the nitro-group O atoms.

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

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Khusnutdin M. Shakhidoyatov

2010-03-01

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

Coordination polymers of scandium sulfate. Crystal structures of (H2Bipy)[Sc(H2O)(SO4)2]2·2H2O and (H2Bipy)[HSO4]2

International Nuclear Information System (INIS)

Petrosyants, S.P.; Ilyukhin, A.B.

2005-01-01

Compounds with general formula Cat x [Sc(H 2 O) z (SO 4 ) y ]·nH 2 O (Cat=NH 4 , H 2 Bipy (Bipy - 4,4'-bipyridine), HEdp (Edp - ethylene dipyridine)) identified on element analysis data and IR spectra are synthesized. X-ray diffraction analysis of (H 2 Bipy)[Sc(H 2 O)(SO 4 ) 2 ] 2 ·2H 2 O shows that in structure of the compound chains of ScO 6 octahedron and SO 4 tetrahedrons are joined in bands by tridentate coordination of sulfate ions. Bands form skeleton in endless emptiness of which there are H 2 Bipy 2+ cations [ru

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

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Hoong-Kun Fun

2009-11-01

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

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

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Vahan Martirosyan

2008-03-01

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

Co3(PO42·4H2O

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Yang Kim

2008-10-01

Full Text Available Single crystals of Co3(PO42·4H2O, tricobalt(II bis[orthophosphate(V] tetrahydrate, were obtained under hydrothermal conditions. The title compound is isotypic with its zinc analogue Zn3(PO42·4H2O (mineral name hopeite and contains two independent Co2+ cations. One Co2+ cation exhibits a slightly distorted tetrahedral coordination, while the second, located on a mirror plane, has a distorted octahedral coordination environment. The tetrahedrally coordinated Co2+ is bonded to four O atoms of four PO43− anions, whereas the six-coordinate Co2+ is cis-bonded to two phosphate groups and to four O atoms of four water molecules (two of which are located on mirror planes, forming a framework structure. In addition, hydrogen bonds of the type O—H...O are present throughout the crystal structure.

2,4-Dichloro-N-p-tolylbenzamide

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Aamer Saeed

2009-10-01

Full Text Available In the title compound, C14H11Cl2NO, the C—N—C(=O—C amide unit is almost planar (r.m.s. deviation = 0.0317 Å and subtends dihedral angles of 65.93 (6 and 29.45 (7°, respectively, to the dichlorobenzene and tolyl rings. The two aromatic rings are inclined at 37.92 (6° to one another. In the crystal structure, N—H...O hydrogen bonds link the molecules into chains along b. Additional weak C—H...Cl and C—H...O hydrogen bonds combine with C—H...π and very weak π–π contacts [Cg...Cg distance = 4.0217 (12 Å] to stack the molecules down b.

N-{(2S-3-Hydroxy-4-[(5-methyl-1,3,4-thiadiazol-2-ylsulfanyl]-1-phenyl-2-butyl}-4-methylbenzenesulfonamide

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Claudia R. B. Gomes

2011-09-01

Full Text Available The thiadiazoyl and sulfonyl-benzene rings in the title compound, C20H23N3O3S3, are aligned to the same side of the molecule, forming a twisted `U' shape [dihedral angle = 77.6 (5°]. The benzyl-benzene ring is orientated in the opposite direction from the molecule but projects approximately along the same axis as the other rings [dihedral angle between benzene rings = 28.2 (5°] so that, overall, the molecule has a flattened shape. The hydroxy and amine groups are almost syn which enables the formation of intermolecular hydroxy-OH...N(thiadiazoyl and amine-H...O(sulfonyl hydrogen bonds leading to a supramolecular chain aligned along the a axis.

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

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Kai Yang

2009-05-01

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

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

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Garima Sharma

2012-09-01

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

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

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Michael J. Ferguson

2008-10-01

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

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

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Vladimir P. Zaytsev

2014-12-01

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

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

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Wolfgang Holzer

2010-09-01

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

(μ-2,3-Dihydroxybutane-1,4-dithiolatobis[triphenyltin(IV

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Cuiping Li

2010-02-01

Full Text Available In the title compound, [Sn2(C6H56(C4H8O2S2], the geometry around the Sn atoms is distorted tetrahedral. The hydroxy groups are involved in O—H...O hydrogen bonding, which connects molecules into centrosymmetric dimers.

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

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Jing Xu

2009-08-01

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

Near interface traps in SiO{sub 2}/4H-SiC metal-oxide-semiconductor field effect transistors monitored by temperature dependent gate current transient measurements

Energy Technology Data Exchange (ETDEWEB)

Fiorenza, Patrick; La Magna, Antonino; Vivona, Marilena; Roccaforte, Fabrizio [Consiglio Nazionale delle Ricerche-Istituto per la Microelettronica e Microsistemi (CNR-IMM), Strada VIII 5, Zona Industriale 95121 Catania (Italy)

2016-07-04

This letter reports on the impact of gate oxide trapping states on the conduction mechanisms in SiO{sub 2}/4H-SiC metal-oxide-semiconductor field effect transistors (MOSFETs). The phenomena were studied by gate current transient measurements, performed on n-channel MOSFETs operated in “gate-controlled-diode” configuration. The measurements revealed an anomalous non-steady conduction under negative bias (V{sub G} > |20 V|) through the SiO{sub 2}/4H-SiC interface. The phenomenon was explained by the coexistence of a electron variable range hopping and a hole Fowler-Nordheim (FN) tunnelling. A semi-empirical modified FN model with a time-depended electric field is used to estimate the near interface traps in the gate oxide (N{sub trap} ∼ 2 × 10{sup 11} cm{sup −2}).

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

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Guang-Yin Wang

2011-09-01

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

[H3N(CH2)4NH3]2[Al4(C2O4)(H2PO4)2(PO4)4].4[H2O]: A new layered aluminum phosphate-oxalate

International Nuclear Information System (INIS)

Peng Li; Li Jiyang; Yu Jihong; Li Guanghua; Fang Qianrong; Xu Ruren

2005-01-01

A new layered inorganic-organic hybrid aluminum phosphate-oxalate [H 3 N(CH 2 ) 4 NH 3 ] 2 [Al 4 (C 2 O 4 )(H 2 PO 4 ) 2 (PO 4 ) 4 ].4[H 2 O](AlPO-CJ25) has been synthesized hydrothermally, by using 1,4-diaminobutane (DAB) as structure-directing agent. The structure has been solved by single-crystal X-ray diffraction analysis and further characterized by IR, 31 P MAS NMR, TG-DTA as well as compositional analyses. Crystal data: the triclinic space group P-1, a=8.0484(7) A, b=8.8608(8) A, c=13.2224(11) A, α=80.830(6) deg. , β=74.965(5) deg. , γ=78.782(6) deg. , Z=2, R 1[ I >2 σ ( I )] =0.0511 and wR 2(alldata) =0.1423. The alternation of AlO 4 tetrahedra and PO 4 tetrahedra gives rise to the four-membered corner-sharing chains, which are interconnected through AlO 6 octahedra to form the layered structure with 4,6-net sheet. Interestingly, oxalate ions are bis-bidentately bonded by participating in the coordination of AlO 6 , and bridging the adjacent AlO 6 octahedra. The layers are held with each other through strong H-bondings between the terminal oxygens. The organic ammonium cations and water molecules are located in the large cavities between the interlayer regions. -- Graphical abstract: The alternation of AlO 4 tetrahedra and PO 4 tetrahedra gives rise to the four-membered corner-sharing chains, which are interconnected through AlO 6 octahedra to form the layered structure with 4,6-net sheet. Oxalate ions are bis-bidentately boned by participating in the coordination of AlO 6 , and bridging the adjacent AlO 6 octahedra

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

Energy Technology Data Exchange (ETDEWEB)

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

1994-02-01

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

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.

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

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Mu-Sen Lin

2012-07-01

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

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

African Journals Online (AJOL)

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

1-[2-(4-Bromobenzyloxy-2-phenylethyl]-1H-1,2,4-triazole

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Tuncer Hökelek

2008-10-01

Full Text Available In the molecule of the title compound, C17H16BrN3O, the triazole ring is oriented at dihedral angles of 6.14 (9° and 82.08 (9°, respectively, with respect to the phenyl and bromobenzene rings. The dihedral angle between the bromobenzene and phenyl rings is 87.28 (7°. The intramolecular C—H...O hydrogen bond results in the formation of a planar five-membered ring, which is oriented at a dihedral angle of 0.13 (6° with respect to the bromobenzene ring. There is an intermolecular C—H...π contact between a methylene group and the bromobenzene ring.

Sequence Variations in the Flagellar Antigen Genes fliC H25 and fliC H28 of Escherichia coli and Their Use in Identification and Characterization of Enterohemorrhagic E. coli (EHEC) O145:H25 and O145:H28

Science.gov (United States)

Beutin, Lothar; Delannoy, Sabine; Fach, Patrick

2015-01-01

Enterohemorrhagic E. coli (EHEC) serogroup O145 is regarded as one of the major EHEC serogroups involved in severe infections in humans. EHEC O145 encompasses motile and non-motile strains of serotypes O145:H25 and O145:H28. Sequencing the fliC-genes associated with the flagellar antigens H25 and H28 revealed the genetic diversity of the fliC H25 and fliC H28 gene sequences in E. coli. Based on allele discrimination of these fliC-genes real-time PCR tests were designed for identification of EHEC O145:H25 and O145:H28. The fliC H25 genes present in O145:H25 were found to be very similar to those present in E. coli serogroups O2, O100, O165, O172 and O177 pointing to their common evolution but were different from fliC H25 genes of a multiple number of other E. coli serotypes. In a similar way, EHEC O145:H28 harbor a characteristic fliC H28 allele which, apart from EHEC O145:H28, was only found in enteropathogenic (EPEC) O28:H28 strains that shared some common traits with EHEC O145:H28. The real time PCR-assays targeting these fliC H25[O145] and fliC H28[O145] alleles allow better characterization of EHEC O145:H25 and EHEC O145:H28. Evaluation of these PCR assays in spiked ready-to eat salad samples resulted in specific detection of both types of EHEC O145 strains even when low spiking levels of 1–10 cfu/g were used. Furthermore these PCR assays allowed identification of non-motile E. coli strains which are serologically not typable for their H-antigens. The combined use of O-antigen genotyping (O145wzy) and detection of the respective fliC H25[O145] and fliC H28[O145] allele types contributes to improve identification and molecular serotyping of E. coli O145 isolates. PMID:26000885

2,2'-(Carbono-thio-yldisulfanedi-yl)bis-(2-methyl-propanoic acid).

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Moreno-Fuquen, Rodolfo; Grande, Carlos; Advincula, Rigoberto C; Tenorio, Juan C; Ellena, Javier

2013-05-01

The mol-ecular structure of the title compound, C9H14O4S3, exhibits intra-molecular C-H⋯S hydrogen bonds. In the crystal, pairs of O-H⋯O hydrogen bonds lead to the formation of centrosymmetric dimers, which are in turn connected by weak C-H⋯O inter-actions. The combination of these inter-actions generates edge-fused R 2 (2)(8) and R 2 (2)(20) rings running along [211].

Octa-akis(4-amino-pyridine)-1κN,2κN-aqua-2κO-μ-carbonato-1:2κO,O':O''-dinickel(II) dichloride penta-hydrate.

Science.gov (United States)

Fun, Hoong-Kun; Sinthiya, A; Jebas, Samuel Robinson; Ravindran Durai Nayagam, B; Alfred Cecil Raj, S

2008-10-18

In the title compound, [Ni(2)(CO(3))(C(5)H(6)N(2))(8)(H(2)O)]Cl(2)·5H(2)O, one of the the Ni(II) ions is six-coordinated in a distorted octa-hedral geometry, with the equatorial plane defined by four pyridine N atoms from four amino-pyridine ligands, the axial positions being occupied by one water O and a carbonate O atom. The other Ni(II) ion is also six-coordinated, by four other pyridine N atoms from four other amino-pyridine ligands and two carbonate O atoms to complete a distorted octa-hedral geometry. In the crystal structure, mol-ecules are linked into an infinite three-dimensional network by O-H⋯O, N-H⋯Cl, N-H⋯O, O-H⋯N, C-H⋯O, C-H⋯N and C/N-H⋯π inter-actions involving the pyridine rings.

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

International Nuclear Information System (INIS)

Mandal, Sukhendu; Natarajan, Srinivasan

2005-01-01

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

Design and syntheses of hybrid metal–organic materials based on K{sub 3}[M(C{sub 2}O{sub 4}){sub 3}]·3H{sub 2}O [M(III)=Fe, Al, Cr] metallotectons

Energy Technology Data Exchange (ETDEWEB)

Sun, Yayong; Zong, Yingxia; Ma, Haoran; Zhang, Ao; Liu, Kang; Wang, Debao, E-mail: dbwang@qust.edu.cn; Wang, Wenqiang; Wang, Lei, E-mail: inorchemwl@126.com

2016-05-15

By using K{sub 3}[M(C{sub 2}O{sub 4}){sub 3}]·3H{sub 2}O [M(III)=Fe, Al, Cr] (C{sub 2}O{sub 4}{sup 2−}=oxalate) metallotectons as the starting material, we have synthesized eight novel complexes with formulas [{Fe(C_2O_4)_2(H_2O)_2}{sub 2}]·(H–L{sub 1}){sub 2}·H{sub 2}O 1, [Fe(C{sub 2}O{sub 4})Cl{sub 2}]·(H{sub 2}–L{sub 2}){sub 0.5}·(L{sub 2}){sub 0.5}·H{sub 2}O 2, [{Fe(C_2O_4)_1_._5Cl_2}{sub 2}]·(H–L{sub 3}){sub 4}3, [Fe{sub 2}(C{sub 2}O{sub 4})Cl{sub 8}]·(H{sub 2}–L{sub 4}){sub 2}·2H{sub 2}O 4, K[Al(C{sub 2}O{sub 4}){sub 3}]·(H{sub 2}–L{sub 5})·2H{sub 2}O 5, K[Al(C{sub 2}O{sub 4}){sub 3}]·(H–L{sub 6}){sub 2}·2H{sub 2}O 6, K[Cr(C{sub 2}O{sub 4}){sub 3}]·2H{sub 2}O 7, Na[Fe(C{sub 2}O{sub 4}){sub 3}]·(H–L{sub 6}){sub 2}·2H{sub 2}O 8 (with L{sub 1}=4-dimethylaminopyridine, L{sub 2}=2,3,5,6-tetramethylpyrazine, L{sub 3}=2-aminobenzimidazole, L{sub 4}=1,4-bis-(1H-imidazol-1-yl)benzene, L{sub 5}=1,4-bis((2-methylimidazol-1-yl)methyl)benzene, L{sub 6}=2-methylbenzimidazole). Their structures have been determined by single-crystal X-ray diffraction analyses, elemental analyses, IR spectra and thermogravimetric analyses. Compound 3 is a 2D H-bonded supramolecular architecture. Others are 3D supramolecular structures. Compound 1 shows a [Fe(C{sub 2}O{sub 4}){sub 2}(H{sub 2}O){sub 2}]{sup −} unit and 3D antionic H-bonded framework. Compound 2 features a [Fe(C{sub 2}O{sub 4})Cl{sub 2}]{sup -} anion and 1D iron-oxalate-iron chain. Compound 3 features a [Fe{sub 2}(C{sub 2}O{sub 4}){sub 3}Cl{sub 4}]{sup 4−} unit. Compound 4 features distinct [Fe{sub 2}(C{sub 2}O{sub 4})Cl{sub 8}]{sup 4−} units, which are mutual linked by water molecules to generated a 2D H-bonded network. Compound 5 features infinite ladder-like chains constructed by [Al(C{sub 2}O{sub 4}){sub 3}]{sup 3−} units and K{sup +} cations. The 1D chains are further extended into 3D antionic H-bonded framework through O–H···O H-bonds. Compounds 6–8 show 2D [KAl(C{sub 2}O

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

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Andya Nemati

2008-10-01

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

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....

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

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M. S. Begum

2015-12-01

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

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

Science.gov (United States)

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

2016-04-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-12-15

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

Crystal structures of ZnCl2·2.5H2O, ZnCl2·3H2O and ZnCl2·4.5H2O

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Erik Hennings

2014-12-01

Full Text Available The formation of different complexes in aqueous solutions is an important step in understanding the behavior of zinc chloride in water. The structure of concentrated ZnCl2 solutions is governed by coordination competition of Cl− and H2O around Zn2+. According to the solid–liquid phase diagram, the title compounds were crystallized below room temperature. The structure of ZnCl2·2.5H2O contains Zn2+ both in a tetrahedral coordination with Cl− and in an octahedral environment defined by five water molecules and one Cl− shared with the [ZnCl4]2− unit. Thus, these two different types of Zn2+ cations form isolated units with composition [Zn2Cl4(H2O5] (pentaaqua-μ-chlorido-trichloridodizinc. The trihydrate {hexaaquazinc tetrachloridozinc, [Zn(H2O6][ZnCl4]}, consists of three different Zn2+ cations, one of which is tetrahedrally coordinated by four Cl− anions. The two other Zn2+ cations are each located on an inversion centre and are octahedrally surrounded by water molecules. The [ZnCl4] tetrahedra and [Zn(H2O6] octahedra are arranged in alternating rows parallel to [001]. The structure of the 4.5-hydrate {hexaaquazinc tetrachloridozinc trihydrate, [Zn(H2O6][ZnCl4]·3H2O}, consists of isolated octahedral [Zn(H2O6] and tetrahedral [ZnCl4] units, as well as additional lattice water molecules. O—H...O hydrogen bonds between the water molecules as donor and ZnCl4 tetrahedra and water molecules as acceptor groups leads to the formation of a three-dimensional network in each of the three structures.

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

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Julio Zukerman-Schpector

2018-03-01

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

(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.

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

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Xiulan Zhang

2013-09-01

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

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.

Diaquabis[2,6-bis(4H-1,2,4-triazol-4-ylpyridine-κN2]bis(selenocyanato-κNcobalt(II

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Yuan-Yuan Liu

2012-08-01

Full Text Available In the title compound, [Co(NCSe2(C9H7N72(H2O2], the Co2+ cation is coordinated by two selenocyanate anions, two 2,6-bis(4H-1,2,4-triazol-4-ylpyridine ligands and two water molecules within a slightly distorted N4O2 octahedron. The asymmetric unit consists of one Co2+ cation, which is located on a center of inversion, as well as one selenocyanate anion, one 2,6-bis(4H-1,2,4-triazol-4-ylpyridine ligand and one water molecule in general positions. Intermolecular O—H...N hydrogen bonds join the complex molecules into layers parallel to the bc plane. The layers are linked by C—H...N and C—H...Se hydrogen bonds into a three-dimensional supramolecular architecture.

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

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S. Dahmani

2010-04-01

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

catena-Poly[[[triaqua[3-(4-carboxyphenoxyphthalato-κO2]manganese(II]-μ-4,4′-bipyridine-κ2N:N′] 4,4′-bipyridine monosolvate dihydrate

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Wei Sun

2013-02-01

Full Text Available In the title compound, {[Mn(C15H8O7(C10H8N2(H2O3]·C10H8N2·2H2O}n, the bridging mode of the coordinating 4,4′-bipyridine ligands leads to the formation of polymeric zigzag chains parallel to [0-11]. The chains are separated by 4,4′-bipyridine and water solvent molecules. Within a chain, the MnII atom is six-coordinated by two N atoms of the bridging 4,4′-bipyridine ligands, three water O atoms and one carboxylate O atom of a single deprotonated 3-(4-carboxyphenoxyphthalic acid ligand. Both coordinating and solvent 4,4′-bipyridine molecules are situated on centres of inversion. An intricate network of O—H...O and O—H...N hydrogen bonds involving the carboxy group, the coordinating water molecules and the two types of solvent molecules leads to the formation of a three-dimensional network.

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

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Jian-Feng Zheng

2008-07-01

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

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

Science.gov (United States)

Kuchár, Juraj; Cernák, Juraj

2009-07-01

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

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

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Hualing Zhu

2011-07-01

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

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.

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

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Flavien A. A. Toze

2011-11-01

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

(2RS)-2-(2,4-Difluoro-phen-yl)-1-[(4-iodo-benz-yl)(meth-yl)amino]-3-(1H-1,2,4-tri-azol-1-yl)propan-2-ol.

Science.gov (United States)

Xiong, Hui-Ping; Gao, Shou-Hong; Li, Chun-Tong; Wu, Zhi-Jun

2012-08-01

IN THE TITLE COMPOUND (COMMON NAME: iodiconazole), C(19)H(19)F(2)IN(4)O, there is an intra-molecular O-H⋯N hydrogen bond and mol-ecules are linked by weak inter-actions only, namely C-H⋯N, C-H⋯O and C-H⋯F hydrogen bonds, and π-electron ring-π-electron ring inter-actions between the triazole rings with centroid-centroid distances of 3.725 (3) Å.

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

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Aliou H. Barry

2003-12-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

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.

Experimental and semi-empirical and DFT calculational studies on (e)-2-(1-(2-(4-methylphenylsulfonamido) ethyliminio) ethyl) phenolate

International Nuclear Information System (INIS)

Alpaslan, G.; Agar, E.; Ersahin, F.; Isik, S.; Erdoenmez, A.

2010-01-01

The molecular and crystal structure of the title compound, C 1 7H 2 0N 2 O 3 S, has been determined by X-ray single crystal diffraction technique. The compound crystallizes in the monoclinic, space group P2 1 /n with unit cell dimensions a=11.4472(6), b=11.1176(4), c=13.4873(7)A 0 , M r =332.41, V=1639.36(13)A 03 , Z=4, R 1 =0.034 and wR 2 =0.097. The molecule adopts a zwitterionic form, stabilized by an intramolecular N + -H 2 O - type ionic weak hydrogen bond. The molecule pack via intermolecular N-H 2 O hydrogen bonds which, together with an intramolecular N + -H 2 O - bond, form an S(6)R 2 4 (4)S(6) motif. Calculational studies were performed by using AM1, PM3 semi-empirical and DFT methods. Geometry optimizations of compound have been carried out by using three semi-empirical methods and DFT method and bond lengths, bond and torsion angles of title compound have been determined. Atomic charge distribution have been obtained from AM1, PM3 and DFT. In order to determine conformational flexibility on the molecule, molecular energy profile of the title compound was obtained with respect to the selected torsion angle T(N1-C9-C10-N2), which is varied from -180 degrees to +180 degrees in every 10 via PM3 semi-empirical method.

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

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Mustafa Göçmentürk

2014-01-01

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

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

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Xu-Feng Liu

2011-11-01

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

5,11,17,23-Tetra-tert-butyl-25,26,27,28-tetrapropynyloxy-2,8,14,20-tetrathiacalix[4]arene

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Xiang-Gao Meng

2009-12-01

Full Text Available The title compound [systematic name: 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrapropynyloxy-2,8,14,20-tetrathiacalix[4]arene], C52H56O4S4, is an alkylated product bearing four propyne groups at the lower rim of a 5,11,17,23-tetra-tert-butyl-tetrathiacalix[4]arene. The molecule is located on a crystallographic twofold rotation axis, running through two S atoms and perpendicular to the long axis of the molecule. The four propyne groups, located in an alternate fashion above and below the mean plane of the four S atoms, are almost parallel to the calixarene long axis. The dihedral angle between the two crystallographically independent benzene rings is 86.77 (14°. Two tert-butyl groups are disordered over two positions with site occupancies of 0.59 (2 and 0.41 (2.

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

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Naki Çolak

2013-07-01

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

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.

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