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

Directory of Open Access Journals (Sweden)

Islam Ullah Khan

2012-07-01

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

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

Directory of Open Access Journals (Sweden)

Moha Berraho

2010-12-01

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

Diffusion of Lithium Ions in Amorphous and Crystalline Poly(ethylene oxide)_3:LiCF_3SO_3 Polymer Electrolytes

International Nuclear Information System (INIS)

Xue, Sha; Liu, Yingdi; Li, Yaping; Teeters, Dale; Crunkleton, Daniel W.; Wang, Sanwu

2017-01-01

The PEO_3:LiCF_3SO_3 polymer electrolyte has attracted significant research due to high conductivity and enhanced stability in lithium polymer batteries. Most experimental studies have shown that amorphous PEO lithium salt electrolytes have higher conductivity than the crystalline ones. Other studies, however, have shown that crystalline PEO salt complexes can conduct ions. As a result, further theoretical investigations are warranted to help clarify the issue. In this work, we use density functional theory with the climbing image nudged elastic band method to investigate the atomic-scale mechanism of lithium ion transport in the polymer electrolytes. We also use density functional theory and ab initio molecular dynamics simulations to obtain the amorphous structure of PEO_3:LiCF_3SO_3. The diffusion pathways and activation energies of lithium ions in both crystalline and amorphous PEO_3:LiCF_3SO_3 are determined. In crystalline PEO_3:LiCF_3SO_3, the activation energy for the low-barrier diffusion pathway is approximately 1.0 eV. In the amorphous phase, the value is 0.6 eV. This result would support the experimental observation that amorphous PEO_3:LiCF_3SO_3 has higher ionic conductivity than the crystalline phase.

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

Directory of Open Access Journals (Sweden)

Lorenzo C. Visentin

2011-01-01

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

The Effects of Lithium Triflate (LiCF3SO3) on the PMMA-based Solid Polymer Electrolytes

International Nuclear Information System (INIS)

Chew, K. W.; Chen, S. S.; Pang, W. L.; Tan, C. G.; Osman, Z.

2010-01-01

The effects of Lithium triflate salt (LiCF 3 SO 3 ), on the poly (methyl methacrylate)(PMMA)-based solid polymer electrolytes plasticized with propylene carbonate (PC) solvated in Tetrahydrofuran (THF) have been studied through a.c impedance spectroscopy and infrared spectroscopy. Lithium triflate was incorporated into the predetermined PMMA/PC system that has the highest value of ionic conductivity. In current investigations, four combination systems: Pure PMMA, (PMMA+PC) systems, (PMMA+LiCF 3 SO 3 ) and (PMMA+PC+LiCF 3 SO 3 ) systems were prepared using the solution cast method. Solutions were stirred for numerous hours to obtain a homogenous solution before it is poured into the petri dishes under ambient temperature to form the solid electrolyte thin film. The films were then removed from petri discs and transferred into the dessicator for further drying prior to the different tests. From the characterization done through the a.c impedance spectroscopy, the highest room temperature ionic conductivity in the pure PMMA sample, (PMMA+PC) system and (PMMA+LiCF 3 SO 3 ) system is 2.83x10 -12 Scm -1 , 4.39x10 -11 Scm -1 and 3.93x10 -6 Scm -1 respectively. The conductivity for (PMMA+PC+LiCF 3 SO 3 ) system was obtained with the 30 wt% of lithium triflate, which is 2.48x10 -5 Scm -1 . Infrared spectroscopy shows that complexation occurred between the polymer and the plasticizer, and the polymer and plasticizer and salt. The interactions have been studied in the C=O band, C-O-C band and the O-CH 3 band.

(E-3-Propoxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one monohydrate

Directory of Open Access Journals (Sweden)

Burkhon Zh Elmuradov

2010-05-01

Full Text Available The title compound, C15H16N2O2·H2O, was synthesized via the alkylation of 3-hydroxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one with n-propyl iodide in the presence of sodium hydroxide. The organic molecule and the water molecule both lie on a crystallographic mirror plane. In the crystal structure, intermolecular O—H...O and O—H...N hydrogen bonds link the components into extended chains along [100].

AGC-3 Graphite Preirradiation Data Analysis Report

Energy Technology Data Exchange (ETDEWEB)

William Windes; David Swank; David Rohrbaugh; Joseph Lord

2013-09-01

This report describes the specimen loading order and documents all pre-irradiation examination material property measurement data for the graphite specimens contained within the third Advanced Graphite Capsule (AGC-3) irradiation capsule. The AGC-3 capsule is third in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens allowing quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades to be generated which will ascertain the in-service behavior of the graphite for pebble bed and prismatic Very High Temperature Reactor (VHTR) designs. The general design of AGC-3 test capsule is similar to the AGC-2 test capsule, material property tests were conducted on graphite specimens prior to loading into the AGC-3 irradiation assembly. However the 6 major nuclear graphite grades in AGC-2 were modified; two previous graphite grades (IG-430 and H-451) were eliminated and one was added (Mersen’s 2114 was added). Specimen testing from three graphite grades (PCEA, 2114, and NBG-17) was conducted at Idaho National Laboratory (INL) and specimen testing for two grades (IG-110 and NBG-18) were conducted at Oak Ridge National Laboratory (ORNL) from May 2011 to July 2013. This report also details the specimen loading methodology for the graphite specimens inside the AGC-3 irradiation capsule. The AGC-3 capsule design requires "matched pair" creep specimens that have similar dose levels above and below the neutron flux profile mid-plane to provide similar specimens with and without an applied load. This document utilized the neutron flux profile calculated for the AGC-3 capsule design, the capsule dimensions, and the size (length) of the selected graphite and silicon carbide samples to create a stacking order that can produce "matched pairs" of graphite samples above and below the AGC-3 capsule elevation mid-point to

A crystallographically isolated dimeric hydrolyzed chlorophosphazene dianion

Directory of Open Access Journals (Sweden)

Matthew J. Panzner

2009-01-01

Full Text Available Single crystals of the title compound bis[bis(1-ethyl-3-methyl-imidazol-2-ylidenesilver(I] 1,5,5,7,11,11-hexachloro-2,8-dioxa-4,6,10,12,13,14-hexaaza-1λ5,3,5λ5,7λ5,9,11λ5-hexaphosphatricyclo[7.3.1.13,7]tetradeca-1(13,4,7(14,10-tetraene-6,12-diide 3,9-dioxide, [Ag(C6H10N22](Cl6N6O4P60.5, were isolated from the reaction of the silver N-heteocyclic carbene complex [Ag(C6H10N22]Cl and hexachlorocyclotriphosphazene [NPCl2]3 in the presence of water. The asymmetric unit contains one silver carbene cation with the carbene ligands bound to the Ag(I in an almost linear arrangement and one half of a hydrolyzed phosphazene dianion. The second cation and additional half of the anion are generated by an inversion center.

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

Directory of Open Access Journals (Sweden)

Tuncer Hökelek

2009-07-01

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

Transport property of novel sono-catalysed LiCF sub 3 SO sub 3 doped SiO sub 2 -PEG ormolyte

CERN Document Server

Jung, H Y; Wi, C J; Whang, C M

2003-01-01

Transport property of a novel sono-catalysed LiCF sub 3 SO sub 3 doped SiO sub 2 -10 wt% PEG ormolyte is reported. The ormolyte was synthesized by sol-gel method by varying the LiCF sub 3 SO sub 3 concentration [Li/O] from 0 to 0.1 in mole. The composition with [Li/O] = 0.05 exhibited the highest conductivity (sigma sub 2 sub 5 sub d eg sub C = 2.4x10 sup - sup 4 S cm sup - sup 1) with an enhancement of 10 sup 3 from that of the host matrix: SiO sub 2 -10 wt% PEG sono gel and has been referred to as 'optimum conducting composition (OCC)'. The direct determination of Li sup + ion mobility (mu)/mobile ion concentration (n) indicated that the enhancement was due to the increase in mu and n both. The temperature dependence of sigma, mu and n were carried out for the OCC samples in order to evaluate the respective energies involved in different thermally activated processes and to understand the ion transport mechanism. The ion transference number (t sub i sub o sub n) measurement inferred the ions as the sole cha...

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

Directory of Open Access Journals (Sweden)

Garima Sharma

2012-09-01

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

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

Directory of Open Access Journals (Sweden)

Ahmed Benzalim

2016-05-01

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

Atmospheric chemistry of CF3CFHCF2OCF3 and CF3CFHCF2OCF2H: Reaction with Cl atoms and OH radicals, degradation mechanism, and global warming potentials

DEFF Research Database (Denmark)

Wallington, TJ; Hurley, MD; Nielsen, OJ

2004-01-01

Fourier transform infrared (FTIR) smog chamber techniques were used to measure k(Cl + CF3CFHCF2OCF3) = (4.09 +/- 0.42) x 10(-17), k(OH + CF3CFHCF2OCF3) = (1.43 +/- 0.28) x 10(-15), k(Cl + CF3CFHCF2OCF2H) = (6.89 +/- 1.29) x 10(-17), and k(OH + CF3CFHCF2OCF2H) = (1.79 +/- 0.34) x 10(-15) cm(3) mol...... respectively. The 100-year time horizon global warming potentials of CF3CFHCF2OCF3 and CF3CFHCF2OCF2H relative to CO2 are 4530 and 4340. Results are discussed with respect to the atmospheric chemistry of hydrofluoroethers....

Electrochemical, spectroscopic, and DFT study of C60(CF3)n frontier orbitals (n = 2-18): the link between double bonds in pentagons and reduction potentials.

Science.gov (United States)

Popov, Alexey A; Kareev, Ivan E; Shustova, Natalia B; Stukalin, Evgeny B; Lebedkin, Sergey F; Seppelt, Konrad; Strauss, Steven H; Boltalina, Olga V; Dunsch, Lothar

2007-09-19

The frontier orbitals of 22 isolated and characterized C(60)(CF(3))(n) derivatives, including seven reported here for the first time, have been investigated by electronic spectroscopy (n = 2 [1], 4 [1], 6 [2], 8 [5], 10 [6], 12 [3]; the number of isomers for each composition is shown in square brackets) fluorescence spectroscopy (n = 10 [4]), cyclic voltammetry under air-free conditions (all compounds with n mV s(-1) up to 5.0 V s(-1), respectively. The 18 experimental 0/- E(1/2) values (vs C(60)(0/-)) are a linear function of the DFT-predicted LUMO energies (average E1/2 deviation from the least-squares line is 0.02 V). This linear relationship was used to predict the 0/- E(1/2) values for the n = 16 and 18 derivatives, and none of the predicted values is more positive than the 0/- E(1/2) value for one of the isomers of C(60)(CF(3))(10). In general, reduction potentials for the 0/- couple are shifted anodically relative to the C(60)(0/-) couple. However, the 0/- E(1/2) values for a given composition are strongly dependent on the addition pattern of the CF3 groups. In addition, LUMO energies for isomers of C(60)(X)(n) (n = 2, 4, 6, 8, 10, and 12) that are structurally related to many of the CF(3) derivatives were calculated and compared for X = CH(3), H, Ph, NH(2), CH(2)F, CHF(2), F, NO(2), and CN. The experimental and computational results for the C(60)(CF(3))(n) compounds and the computational results for more than 50 additional C(60)(X)(n) compounds provide new insights about the frontier orbitals of C(60)(X)(n) derivatives. For a given substituent, X, the addition pattern is as important, if not more important in many cases, than the number of substituents, n, in determining E(1/2) values. Those addition patterns with double bonds in pentagons having two C(sp(2)) nearest neighbors result in the strongest electron acceptors.

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.

Preparation and Characterization of cis- and trans-[Ir(tn)2Cl2]CF3SO3 and of [Ir(tn)3]Cl3 (tn=propane-1,3-diamine)

DEFF Research Database (Denmark)

Brorson, Michael; Galsbøl, Frode; Simonsen, Kim

1998-01-01

for the preparation of [Rh(tn)3]Cl3 in quantitative yield from Rh(thtp)3Cl3 is also given. The complexes were characterized by 1H and 13C NMR and by UV/VIS spectroscopy. The conformation of the six-membered chelate rings of [Ir(tn)3]3+ in the solid state was determined by single-crystal X-ray diffraction of [Ir(tn)3......Procedures are given for the preparation and isolation of cis- and trans-[Ir(tn)2Cl2]CF3SO3 and of [Ir(tn)3]Cl3, (tn=propane-1,3-diamine). The compounds were prepared by the use of Ir(thtp)3Cl3 (thtp=tetrahydrothiophene) as starting material, using either DMSO or neat tn as solvent. A procedure......] [Co(CN)6] x 5H2O. The three chelate rings all adopt the energetically favoured chair conformation; however, the overall idealized symmetry is C1. A comparative ligand field analysis, based on Gaussian resolution of the solution UV/VIS spectra for a number of homoleptic [M(N6)]3+ (M=CoIII, RhIII, Ir...

Betaine-induced assembly of neutral infinite columns and chains of linked silver(I) polyhedra with embedded acetylenediide.

Science.gov (United States)

Zhao, Xiao-Li; Wang, Quan-Ming; Mak, Thomas C W

2005-03-18

Ten polymeric silver(I) double salts containing embedded acetylenediide: [(Ag2C2)2(AgCF3CO2)9(L1)3] (1), [(Ag2C2)2(AgCF3CO2)10(L2)3]H2O (2), [(Ag2C2)(AgCF3CO2)4(L3)(H2O)]0.75 H2O (3), [(Ag2C2)(1.5)(AgCF3CO2)7(L4)2] (4), [(Ag2C2)(AgCF3CO2)7(L5)2(H2O)] (5), [(Ag2C2) (AgC2F5CO2)7(L1)3(H2O)] (6), [(Ag2C2)(AgCF3CO2)7(L1)3(H2O)]2 H2O (7), [(Ag2C2)(AgC2F5CO2)6(L3)2] (8), [(Ag2C2)2(AgC2F5CO2)12(L4)2(H2O)4]H2O (9), and [(Ag2C2)(AgCF3CO2)6(L3)2(H2O)]H2O (10) have been isolated by varying the types of betaines, the perfluorocarboxylate ligands employed, and the reaction conditions. Single-crystal X-ray analysis has shown that 1-4 all have a columnar structure composed of fused silver(I) double cages, with C2(2-) species embedded in its stem and an exterior coat comprising anionic and zwitterionic carboxylates. For 5 and 6, single silver(I) cages are linked into a beaded chain through both types of carboxylate ligands. In 7, two different coordination modes of L1 connect the silver(I) polyhedra into a chain. For 8, the mu(2)-O,O' coordination mode of L3 connects the silver(I) double cages into a chain. Compound 9 exhibits a two-dimensional architecture generated from the cross-linkage of double cages by C2F5CO2-, L4, and [Ag2(C2F5CO2)2] units. Similar to 9, 10 is also a two-dimensional structure, which is formed by connecting the chains of linked double cages through [Ag2(CF3CO2)2] bridging.

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-07-15

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

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

Science.gov (United States)

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

2011-01-08

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

catena-Poly[[[aquasilver(I]-μ-1,1′-(butane-1,4-diyldi-1H-imidazole-κ2N3:N3′] hemi(biphenyl-4,4′-dicarboxylate dihydrate

Directory of Open Access Journals (Sweden)

Zheyu Zhang

2009-12-01

Full Text Available In the title compound, {[Ag(C10H14N4(H2O](C14H8O40.5·2H2O}n, the AgI ion is three-coordinated by two N atoms from two independent 1,1′-(butane-1,4-diyldi-1H-imidazole (BBI ligands and one water O atom in a distorted T-shaped coordination geometry. The biphenyl-4,4′-dicarboxylate (BPDC dianions do not coordinate to AgI ions but act as counter-ions. The AgI ions are linked by BBI ligands, forming a zigzag chain. These chains are linked into a two-dimensional supramolecular architecture by O—H...O hydrogen-bonding interactions between water molecules and carboxylate O atoms of the BPDC dianions.

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

Directory of Open Access Journals (Sweden)

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.

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

Directory of Open Access Journals (Sweden)

Vijayan Viswanathan

2017-05-01

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

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

Directory of Open Access Journals (Sweden)

Bing-Yuan Su

2008-11-01

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

Atmospheric chemistry of CF3O radicals: Reaction with H2O

DEFF Research Database (Denmark)

Wallington, T.J.; Hurley, M.D.; Schneider, W.F.

1993-01-01

Evidence is presented that CF3O radicals react with H2O in the gas phase at 296 K to give CF3OH and OH radicals. This reaction is calculated to be exothermic by 1.7 kcal mol-I implying a surprisingly strong CF3O-H bond energy of 120 +/- 3 kcal mol-1. Results from a relative rate experimental study...... suggest that the rate constant for the reaction of CF3O radicals with H2O lies in the range (0.2-4.0) X 10(-17) cm3 molecule-1 s-1. Implications for the atmospheric chemistry of CF3O radicals are discussed....

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

Directory of Open Access Journals (Sweden)

R. A. Nagalakshmi

2015-01-01

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

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

Directory of Open Access Journals (Sweden)

S. Sriman Narayanan

2008-09-01

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

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

Directory of Open Access Journals (Sweden)

Peter G. Jones

2010-01-01

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

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

Directory of Open Access Journals (Sweden)

Wolfgang Frey

2008-03-01

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

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

Directory of Open Access Journals (Sweden)

B. Narayana

2013-01-01

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

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

Directory of Open Access Journals (Sweden)

Zukhra Ch. Kadirova

2009-07-01

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

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

Directory of Open Access Journals (Sweden)

Abdellah N'ait Ousidi

2016-03-01

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

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

Directory of Open Access Journals (Sweden)

Hadi Kargar

2012-07-01

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

Bis(1,10-phenanthroline-κ2N,N′(sulfato-κ2O,O′cobalt(II propane-1,3-diol solvate

Directory of Open Access Journals (Sweden)

Kai-Long Zhong

2010-03-01

Full Text Available The title compound, [Co(SO4(C12H8N22]·C3H8O2, was obtained unexpectedly as a by-product during an attempt to synthesize a mixed-ligand complex of CoII with 1,10-phenanthroline (phen and melamine via a solvothermal reaction. The CoII metal ions are in a distorted octahedral coordination environment formed by four N atoms from two chelating phen ligands and two O atoms from a bidentate sulfate ligand. The two chelating N2C2 groups are almost perpendicular to each other [dihedral angle = 80.06 (8°]. A twofold rotation axis passes through the Co and S atoms, and also through the central C atom of the propane-1,3-diol solvent molecule. Intermolecular O—H...O hydrogen bonds help to stabilize the structure.

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

Directory of Open Access Journals (Sweden)

Shu-Shen Zhang

2011-10-01

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

Gold(I) Complexes with N-Donor Ligands. 2.(1) Reactions of Ammonium Salts with [Au(acac-kappaC(2))(PR(3))] To Give [Au(NH(3))L](+), [(AuL)(2)(&mgr;(2)-NH(2))](+), [(AuL)(4)(&mgr;(4)-N)](+), or [(AuL)(3)(&mgr;(3)-O)](+). A New and Facile Synthesis of [Au(NH(3))(2)](+) Salts. Crystal Structure of [{AuP(C(6)H(4)OMe-4)(3)}(3)(&mgr;(3)-O)]CF(3)SO(3).

Science.gov (United States)

Vicente, José; Chicote, María-Teresa; Guerrero, Rita; Jones, Peter G.; Ramírez De Arellano, M. Carmen

1997-09-24

The complexes [Au(acac-kappaC(2))(PR(3))] (acac = acetylacetonate, R = Ph, C(6)H(4)OMe-4) react with (NH(4))ClO(4) to give amminegold(I), [Au(NH(3))(PR(3))]ClO(4), amidogold(I), [(AuPR(3))(2)(&mgr;(2)-NH(2))]ClO(4), or nitridogold(I), [(AuPR(3))(4)(&mgr;(4)-N)]ClO(4), complexes, depending on the reaction conditions. Similarly, [Au(acac-kappaC(2))(PPh(3))] reacts with (NH(3)R')OTf (OTf = CF(3)SO(3)) (1:1) or with [H(3)N(CH(2))(2)NH(2)]OTf (1:1) to give (amine)gold(I) complexes [Au(NH(2)R')(PPh(3))]OTf (R' = Me, C(6)H(4)NO(2)-4) or [(AuPPh(3))(2){&mgr;(2)-H(2)N(CH(2))(2)NH(2)}](OTf)(2), respectively. The ammonium salts (NH(2)R'(2))OTf (R' = Et, Ph) react with [Au(acac-kappaC(2))(PR(3))] (R = Ph, C(6)H(4)OMe-4) (1:2) to give, after hydrolysis, the oxonium salts [(AuPR(3))(3)(&mgr;(3)-O)]OTf (R = Ph, C(6)H(4)OMe-4). When NH(3) is bubbled through a solution of [AuCl(tht)] (tht = tetrahydrothiophene), the complex [Au(NH(3))(2)]Cl precipitates. Addition of [Au(NH(3))(2)]Cl to a solution of AgClO(4) or TlOTf leads to the isolation of [Au(NH(3))(2)]ClO(4) or [Au(NH(3))(2)]OTf, respectively. The crystal structure of [(AuPR(3))(3)(&mgr;(3)-O)]OTf.Me(2)CO (R = C(6)H(4)OMe-4) has been determined: triclinic, space group P&onemacr;, a = 14.884(3) Å, b = 15.828(3) Å, c = 16.061(3) Å, alpha = 83.39(3) degrees, beta = 86.28(3) degrees, gamma = 65.54(3) degrees, R1 (wR2) = 0.0370 (0.0788). The [(AuPR(3))(3)(&mgr;(3)-O)](+) cation shows an essentially trigonal pyramidal array of three gold atoms and one oxygen atom with O-Au-P bond angles of ca. 175 degrees and Au.Au contacts in the range 2.9585(7)-3.0505(14) Å. These cations are linked into centrosymmetric dimers through two short Au.Au [2.9585(7), 3.0919(9) Å] contacts. The gold atoms of the dimer form a six-membered ring with a chair conformation.

Dielectric and conduction mechanism studies of PEMA/ENR-50 blend with LiCF3SO3 salt

Science.gov (United States)

Sukri, N.; Mohamed, N. S.; Subban, R. H. Y.

2017-09-01

Solid polymer electrolytes (SPEs) composed of a blend of Poly(ethyl methacrylate) (PEMA) and Epoxidized Natural Rubber-50 (ENR-50) and Lithium triflate (LiCF3SO3) were prepared by solution casting technique. The conductivity was measured by using electrical impedance spectroscopy (EIS). Measurement of conductivity was carried out as a function of frequency at various concentrations of salt. The SPE exhibit high conductivity of ˜10-5 S/cm at ambient temperature when 40 wt% of LiCF3SO3 was added. Increase in conductivity is attributed to increasing number of charge carriers due to dissociation of salt when the concentration of salt increased. Dielectric properties and ac conductivity of the samples were analyzed. The values of dielectric constant were found to increase with increasing conductivity of the samples. The electrical modulus shows the formation of dispersion peaks. Relaxation time of ionic charge carriers were extracted from the maximum peak of loss tangent at various concentrations of LiCF3SO3 salt. The temperature dependence of the power law exponent s is explained by the overlapping large polaron-tunnelling (OLPT) model.

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

Directory of Open Access Journals (Sweden)

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.

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

Directory of Open Access Journals (Sweden)

Sarah Maloney

2013-02-01

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

Investigation on dielectric relaxation of PMMA-grafted natural rubber incorporated with LiCF3SO3

International Nuclear Information System (INIS)

Yap, K.S.; Teo, L.P.; Sim, L.N.; Majid, S.R.; Arof, A.K.

2012-01-01

Natural rubber (NR) grafted with 30 wt% poly (methyl methacrylate) (PMMA) and designated as MG30 has been added with varying amounts of LiCF 3 SO 3 . X-ray diffraction (XRD) shows the samples to be amorphous. Fourier transform infrared (FTIR) spectroscopy indicates complexation between the cation of the salt and the oxygen atom of the C=O and -COO- groups of MG30. From electrochemical impedance spectroscopy (EIS), MG30 with 30 wt% LiCF 3 SO 3 salt exhibits the highest ambient conductivity of 1.69×10 -6 S cm -1 and lowest activation energy of 0.24 eV. The dielectric behavior has been analyzed using dielectric permittivity (ε′), dissipation factor (tan δ) and dielectric modulus (M ⁎ ) of the samples. The dielectric constant of pure MG30 has been estimated to be ∼1.86.

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

Directory of Open Access Journals (Sweden)

Palanikumar Maniam

2011-06-01

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

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

Directory of Open Access Journals (Sweden)

Eyad Mallah

2015-01-01

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

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

Atmospheric chemistry of CF3CH2CH2OH

DEFF Research Database (Denmark)

Hurley, Michael D.; Misner, Jessica A.; Ball, James C.

2005-01-01

Relative rate techniques were used to study the kinetics of the reactions of Cl atoms and OH radicals with CF3CH2C(O)H and CF3CH2CH2OH in 700 Torr of N-2 or air diluent at 296 2 K. The rate constants determined were k(Cl+CF3CH2C(O)H) = (1.81 +/- 0.27) x 10(-11), k(OH+CF3CH2C(O)H) = (2.57 +/- 0.44...

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

Science.gov (United States)

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

2009-04-01

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

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

Directory of Open Access Journals (Sweden)

Qiu-qi Ye

2012-09-01

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

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

Directory of Open Access Journals (Sweden)

Krzysztof Lyczko

2013-01-01

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

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

Directory of Open Access Journals (Sweden)

Norihiro Tokitoh

2008-02-01

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

cis-Tetrachloridobis(1H-imidazole-κN3platinum(IV

Directory of Open Access Journals (Sweden)

Vadim Yu. Kukushkin

2012-05-01

Full Text Available In the title complex, cis-[PtCl4(C3H4N22], the PtIV ion lies on a twofold rotation axis and is coordinated in a slightly distorted octahedral geometry. The dihedral angle between the imidazole rings is 69.9 (2°. In the crystal, molecules are linked by N—H...Cl hydrogen bonds, forming a three-dimensional network.

Simple introduction of anion trapping site to polymer electrolytes through dehydrocoupling or hydroboration reaction using 9-borabicyclo[3.3.1]nonane

International Nuclear Information System (INIS)

Mizumo, Tomonobu; Sakamoto, Kenji; Matsumi, Noriyoshi; Ohno, Hiroyuki

2005-01-01

Organoboron-based anion trapping polymer electrolytes were synthesized through hydroboration or dehydrocoupling reaction between poly(propylene oxide) (PPO) oligomer (M n =400, 1200, 2000 and 4000) and 9-borabicyclo[3.3.1]nonane (9-BBN). Obtained oligomers were added various lithium salts (LiN(CF 3 SO 2 ) 2 , LiSO 3 CF 3 , LiCO 2 CF 3 or LiBr) to analyze the ionic conductivity and lithium ion transference number (t Li + ). The ionic conductivity of the oligomer in the presence of LiN(CF 3 SO 2 ) 2 showed higher ionic conductivity than other systems, however, the t Li + was less than 0.3. When LiSO 3 CF 3 or LiCO 2 CF 3 , was added high t Li + over 0.6 was obtained. Such difference in t Li + can be explained by HSAB principle. Since boron is a hard acid, soft (CF 3 SO 2 ) 2 N - anion can not be trapped effectively. High ionic conductivity of 1.3x10 -6 Scm -1 and high t Li + of 0.73 was obtained when PPO chain length was 2000. These values of facilely prepared polymer electrolytes are comparable to those of the PPOs having covalently bonded salt moieties on the chain ends

Crystal structure of tris(1,10-phenanthroline-κ2N,N′iron(II bis[bis(trifluoromethylsulfonylimide] monohydrate

Directory of Open Access Journals (Sweden)

Kazunori Teramoto

2015-01-01

Full Text Available The crystal structure of the title complex, [Fe(C12H8N23][(CF3SO22N]2·H2O, is constructed by one octahedral [Fe(phen3]2+ (phen = 1,10-phenanthroline cation (point group symmetry 2, two Tf2N− [bis(trifluoromethylsulfonylimide] anions, and one water molecule of crystallization (point group 2. The Fe—N bond lengths are indicative of a d6 low-spin state for the FeII ion in the complex. The dihedral angle between the phen ligands in the cation is 87.64 (6°. The Tf2N− counter-anion is non-coordinating, with the –CF3 groups arranged in a trans fashion with respect to each other, leading to an anti,anti conformation of the –CF3 groups and –SO2N– moieties relative to the S—C bonds. The water molecule of crystallization connects two O atoms of the Tf2N− anions through weak hydrogen bonds. C—H...O hydrogen-bonding interactions are also observed, consolidating the packing of the molecules into a three-dimensional network structure.

Crystal structures of N2,N3,N5,N6-tetrakis(pyridin-2-ylmethylpyrazine-2,3,5,6-tetracarboxamide and N2,N3,N5,N6-tetrakis(pyridin-4-ylmethylpyrazine-2,3,5,6-tetracarboxamide

Directory of Open Access Journals (Sweden)

Dilovan S. Cati

2017-02-01

Full Text Available The title compounds, C32H28N10O4· unknown solvent, (I, and C32H28N10O4, (II, are pyrazine-2,3,5,6-tetracarboxamide derivatives. In (I, the substituents are (pyridin-2-ylmethylcarboxamide, while in (II, the substituents are (pyridin-4-ylmethylcarboxamide. Both compounds crystallize in the monoclinic space group P21/n, with Z′ = 1 for (I, and Z′ = 0.5 for (II. The whole molecule of (II is generated by inversion symmetry, the pyrazine ring being situated about a center of inversion. In (I, the four pyridine rings are inclined to the pyrazine ring by 83.9 (2, 82.16 (18, 82.73 (19 and 17.65 (19°. This last dihedral angle involves a pyridine ring that is linked to the adjacent carboxamide O atom by an intramolecular C—H...O hydrogen bond. In compound (II, the unique pyridine rings are inclined to the pyrazine ring by 33.3 (3 and 81.71 (10°. There are two symmetrical intramolecular C—H...O hydrogen bonds present in (II. In the crystal of (I, molecules are linked by N—H...O and N—H...N hydrogen bonds, forming layers parallel to (10-1. The layers are linked by C—H...O and C—H...N hydrogen bonds, forming a three-dimensional framework. In the crystal of (II, molecules are linked by N—H...N hydrogen bonds, forming chains propagating along the [010] direction. The chains are linked by a weaker N—H...N hydrogen bond, forming layers parallel to the (101 plane, which are in turn linked by C—H...O hydrogen bonds, forming a three-dimensional structure. In the crystal of compound (I, a region of disordered electron density was treated with the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18]. Their contribution was not taken into account during refinement. In compound (II, one of the pyridine rings is positionally disordered, and the refined occupancy ratio for the disordered Car—Car—Npy atoms is 0.58 (3:0.42 (3.

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

Directory of Open Access Journals (Sweden)

Shoaib Anwar

2012-08-01

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

Haloacyl complexes of boron, [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I).

Science.gov (United States)

Finze, Maik; Bernhardt, Eduard; Willner, Helge; Lehmann, Christian W

2005-11-04

The haloacyltris(trifluoromethyl)borate anions [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I) have been synthesized by reacting (CF3)3BCO with either MHal (M=K, Cs; Hal=F) in SO2 or MHal (M=[nBu4N]+, [Et4N]+, [Ph4P]+; Hal=Cl, Br, I) in dichloromethane. Metathesis reactions of the fluoroacyl complex with Me3SiHal (Hal=Cl, Br, I) led to the formation of its higher homologues. The thermal stabilities of the haloacyltris(trifluoromethyl)borates decrease from the fluorine to the iodine derivative. The chemical reactivities decrease in the same order as demonstrated by a series of selected reactions. The new [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br) salts are used as starting materials in the syntheses of novel compounds that contain the (CF3)3B-C fragment. All borate anions [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I) have been characterized by multinuclear NMR spectroscopy (11B, 13C, 17O, 19F) and vibrational spectroscopy. [PPh4][(CF3)3BC(O)Br] crystallizes in the monoclinic space group P2/c (no. 13) and the bond parameters are compared with those of (CF3)3BCO and K[(CF3)3BC(O)F]. The interpretation of the spectroscopic and structural data are supported by DFT calculations [B3LYP/6-311+G(d)].

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

Directory of Open Access Journals (Sweden)

Mehmet Akkurt

2014-06-01

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

Structural, magnetic and transport properties of Mn3.1Sn0.9 and Mn3.1Sn0.9N compounds

International Nuclear Information System (INIS)

Feng, W.J.; Li, D.; Ren, W.J.; Li, Y.B.; Li, W.F.; Li, J.; Zhang, Y.Q.; Zhang, Z.D.

2007-01-01

The cubic anti-perovskite Mn 3.1 Sn 0.9 N compound is prepared via nitrogenation of the hexagonal Mn 3.1 Sn 0.9 compound. A magnetic phase diagram of Mn 3.1 Sn 0.9 compound is constructed by analysis of data of its magnetic properties. For Mn 3.1 Sn 0.9 N compound, parasitic ferromagnetism exists in the temperature range of 5-370 K, besides a spin-reorientation at about 280 K. Mn 3.1 Sn 0.9 compound exhibits a metallic conducting behavior, while Mn 3.1 Sn 0.9 N displays a metal-nonmetal transition due to the electron localization caused by the static disorder. The differences of the physical properties between the both compounds, are discussed, in terms of the correlation of the hexagonal DO 19 and the cubic anti-perovskite structures, the reduction of the distances between Mn atoms, and the spin-pairing or charge transfer effect due to the electron donation by N 2p to Mn 3d states after introduction of N atoms into the interstitial sites of Mn 3.1 Sn 0.9 compound

Preparation and characterization of novel thermoset polyimide and polyimide-peo doped with LiCF3SO3

Directory of Open Access Journals (Sweden)

M. H. Ugur

2014-02-01

Full Text Available This paper deals with the synthesis and characterization of a new type of anhydrous ionic conducting lithium doped membranes consist of polyimide (PI, poly (ethylene oxide (PEO and lithium trifluoromethanesulfonate (LiCF3SO3 for solid polymer electrolyte (SPE. For this purpose, different molar ratios of lithium salt (Li-salt solution are added into poly (amic acid (PAA intermediate prepared from the reaction of 3,3',4,4'-benzophenon tetracarboxylic dianhydride (BTDA and 4,4'-oxydianiline (ODA. PEO is incorporated into PAA since it forms more stable complexes and possess high ionic conductivities. Then, Li-salt containing PAA solutions are imidized by thermal process. The effect of interaction between host polymer and Li-salt is characterized by FT-IR (Fourier Transform Infrared spectroscopy and SEM (scanning electron micrsocopy. The conductivities of Li-salt and PEO containing PI composite membranes are in the range of 10–7–10–5 S•cm–1. The conductivity increases with incorporation of PEO. Thermogravimetric analysis results reveal that the PI/PEO/LiCF3SO3 composite polymer electrolyte membranes are thermally stable up to 500°C.

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

Directory of Open Access Journals (Sweden)

Gene-Hsiang Lee

2006-03-01

Full Text Available The title compound 6-amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]-triazin-8(7H-one (4, molecular formula C11H10N6OS, was obtained by the reaction of3-amino-2-benzyl-6-hydrazino-1,2,4-triazin-5(2H-one (3 with carbon disulfide in awater/pyridine mixture. Compound 4 can also be synthesized by reacting6-amino-3(2Hmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (7 with benzylbromide in methanolic ammonia water. The compound crystallizes in the monoclinicspace group P21/c with a = 7.2926(15, b = 14.456(2, c = 11.436(2 å, β = 105.30(2°, V= 1162.9(4 å3 and Z = 4, resulting in a density Dcalc of 1.567 g/cm3. Molecules of 4 arelinked by extensive intermolecular N-H···N and N-H···O hydrogen bonding [graph set R22 (9]. The structure is further stabilized by π-π stacking interactions. 2

Synthesis of some glycoside analogs and related compounds from 9-amino-6-(methylthio)-9H-purine.

Science.gov (United States)

Temple, C; Kussner, C L; Montgomery, J A

1975-12-01

Additional information on the anticancer activity of 9-amino-9H-purine-6(1H)-thione and its derivatives was sought by the synthesis of some 9-(substituted amino)-6-(methylthio)-9H-purines in which the 9-substituent contained functional groups capable of either reversible or irreversible binding with an enzymatic site. Condensation of 9-amino-6-(methylthio)-9H-purine (1) with some carbonyl compounds followed by hydride reduction of the azomethine linkage in the intermediates leads to the 2-pyrrolylmethyl (8), 2,3,4-trihydroxybutyl (10), and the 1,5-dihydroxy-2- and 3-pentyl (11 and 12) compounds. A 4-hydroxybutyl derivative (13) was obtained by alkylation of 18, the 9-acetyl derivative of 1, with 4-chlorobutyl acetate followed by saponification. The cyclization of 13 and 11 with a sulfonyl chloride gave the 9-pyrrolidin-1-yl (27) and the 9-[2-(tosyloxymethyl)pyrrolidin-1-yl] (28), respectively. Acylation of 1 with ethyl L-2-pyrrolidine-5-carboxylate and ethyl 1-methyl-5-pyrrolidone-3-carboxylate, respectively, in Me2SO containing NaH gave the corresponding amides 15 and 17. Alkylation of 18 with 1-bromo-2-chloroethane and epichlorohydrin gave the N-(2-chloroethyl) and N-(1,2-epoxy-3-propyl) derivatives 19 and 20. The chloro group of the chlorobutyl derivative of 18 was displaced with KSCN and NaN3, respectively, to give the thiocyanate and azido derivatives 23 and 24. Hydrogenation of the latter gave the amine (25), which was acylated with ethyl chloroformate to give the (ethoxycarbonyl)amino compound 26. None of these compounds showed activity against L1210 leukemia cells implanted ip in mice on a single-dose schedule, suggesting that the activity observed in the simpler 9-aminopurines resulted from cleavage of the hydrazino linkage to give pH-purine-6(1H)-thione.

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

Directory of Open Access Journals (Sweden)

Feng-Ling Yang

2008-12-01

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

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

Science.gov (United States)

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

2014-04-07

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

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

Directory of Open Access Journals (Sweden)

2009-03-01

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

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

Directory of Open Access Journals (Sweden)

Miao Ou-Yang

2008-11-01

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

Bis(1,10-phenanthroline-κ2N,N′(sulfato-κ2O,O′cobalt(II butane-2,3-diol monosolvate

Directory of Open Access Journals (Sweden)

Shi-Juan Wang

2011-04-01

Full Text Available In the title compound, [Co(SO4(C12H8N22]·C4H10O2, the Co2+ ion has a distorted octahedral coordination environment composed of four N atoms from two chelating 1,10-phenanthroline ligands and two O atoms from an O,O′-bidentate sulfate anion. The dihedral angle between the two chelating N2C2 groups is 83.48 (1°. The Co2+ ion, the S atom and the mid-point of the central C—C bond of the butane-2,3-diol solvent molecule are situated on twofold rotation axes. The molecules of the complex and the solvent molecules are held together by pairs of symmetry-related O—H...O hydrogen bonds with the uncoordinated O atoms of the sulfate ions as acceptors. The solvent molecule is disordered over two sets of sites with site occupancies of 0.40 and 0.60.

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

Directory of Open Access Journals (Sweden)

Rachid Bouhfid

2014-03-01

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

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

Directory of Open Access Journals (Sweden)

Li-Cheng Sun

2012-03-01

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

Simple formation of products of exo-nido→closo-regrouping during substitution of PPh3-ligands by bis(diphenyl phosphino)alkanes in three-bridging ruthena carborane 5,6,10-[RuCl(PPh3)2]-5,6,10-(μ-H)3-10-H-exo-nido-7,8-C2B9H8

International Nuclear Information System (INIS)

Cheredilin, D.N.; Balagurova, E.V.; Godovikov, I.A.; Solodovnikov, S.P.; Chizhevskij, I.T.

2005-01-01

It is established that the substitution of PPh 3 -ligands by diphosphines [Ph 2 P(CH 2 ) n PPh] (n=3, 4) in three-bridging exo-nido-ruthena carborane 5,6,10-[RuCl(PPh 3 ) 2 ]-5,6,10-(μ-H) 3 -10-H-exo-nido-7,8-C 2 B 9 H 8 (1) decreases temperature of exo-nido→closo-regrouping (22 Deg C). It is demonstrated that the exo-nido-ruthena carborane complex (1) is well suited and available as reagent for preparation of closo-ruthena carboranes with different chelate diphosphines. Formation of closo-products follows through the stage of exo-nido→closo-regrouping of diphosphine complexes with exo-nido-structure [ru

Methanesulfonates of high-valent metals. Syntheses and structural features of MoO{sub 2}(CH{sub 3}SO{sub 3}){sub 2}, UO{sub 2}(CH{sub 3}SO{sub 3}){sub 2}, ReO{sub 3}(CH{sub 3}SO{sub 3}), VO(CH{sub 3}SO{sub 3}){sub 2}, and V{sub 2}O{sub 3}(CH{sub 3}SO{sub 3}){sub 4} and their thermal decomposition under N{sub 2} and O{sub 2} atmosphere

Energy Technology Data Exchange (ETDEWEB)

Betke, Ulf; Neuschulz, Kai; Wickleder, Mathias S. [Carl von Ossietzky University of Oldenburg, Institute of Pure and Applied Chemistry (Germany)

2011-11-04

Oxide methanesulfonates of Mo, U, Re, and V have been prepared by reaction of MoO{sub 3}, UO{sub 2}(CH{sub 3}COO){sub 2}.2 H{sub 2}O, Re{sub 2}O{sub 7}(H{sub 2}O){sub 2}, and V{sub 2}O{sub 5} with CH{sub 3}SO{sub 3}H or mixtures thereof with its anhydride. These compounds are the first examples of solvent-free oxide methanesulfonates of these elements. MoO{sub 2}(CH{sub 3}SO{sub 3}){sub 2} (Pbca, a=1487.05(4), b=752.55(2), c=1549.61(5) pm, V=1.73414(9) nm{sup 3}, Z=8) contains [MoO{sub 2}] moieties connected by [CH{sub 3}SO{sub 3}] ions to form layers parallel to (100). UO{sub 2}(CH{sub 3}SO{sub 3}){sub 2} (P2{sub 1}/c, a=1320.4(1), b=1014.41(6), c=1533.7(1) pm, β=112.80(1) {sup circle}, V=1.8937(3) nm{sup 3}, Z=8) consists of linear UO{sub 2}{sup 2+} ions coordinated by five [CH{sub 3}SO{sub 3}] ions, forming a layer structure. VO(CH{sub 3}SO{sub 3}){sub 2} (P2{sub 1}/c, a=1136.5(1), b=869.87(7), c=915.5(1) pm, β=113.66(1) {sup circle}, V=0.8290(2) nm{sup 3}, Z=4) contains [VO] units connected by methanesulfonate anions to form corrugated layers parallel to (100). In ReO{sub 3}(CH{sub 3}SO{sub 3}) (P anti 1, a=574.0(1), b=1279.6(3), c=1641.9(3) pm, α=102.08(2), β=96.11(2), γ=99.04(2) {sup circle}, V=1.1523(4) nm{sup 3}, Z=8) a chain structure exhibiting infinite O-[ReO{sub 2}]-O-[ReO{sub 2}]-O chains is formed. Each [ReO{sub 2}]-O-[ReO{sub 2}] unit is coordinated by two bidentate [CH{sub 3}SO{sub 3}] ions. V{sub 2}O{sub 3}(CH{sub 3}SO{sub 3}){sub 4} (I2/a, a=1645.2(3), b=583.1(1), c=1670.2(3) pm, β=102.58(3), V=1.5637(5) pm{sup 3}, Z=4) adopts a chain structure, too, but contains discrete [VO]-O-[VO] moieties, each coordinated by two bidentate [CH{sub 3}SO{sub 3}] ligands. Additional methanesulfonate ions connect the [V{sub 2}O{sub 3}] groups along [001]. Thermal decomposition of the compounds was monitored under N{sub 2} and O{sub 2} atmosphere by thermogravimetric/differential thermal analysis and XRD measurements. Under N{sub 2} the decomposition proceeds

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

Directory of Open Access Journals (Sweden)

2009-03-01

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

Investigation on dielectric relaxation of PMMA-grafted natural rubber incorporated with LiCF{sub 3}SO{sub 3}

Energy Technology Data Exchange (ETDEWEB)

Yap, K.S.; Teo, L.P.; Sim, L.N.; Majid, S.R. [Centre for Ionics University of Malaya, Physics Department, University of Malaya, 50603 Kuala Lumpur (Malaysia); Arof, A.K., E-mail: akarof@um.edu.my [Centre for Ionics University of Malaya, Physics Department, University of Malaya, 50603 Kuala Lumpur (Malaysia)

2012-07-01

Natural rubber (NR) grafted with 30 wt% poly (methyl methacrylate) (PMMA) and designated as MG30 has been added with varying amounts of LiCF{sub 3}SO{sub 3}. X-ray diffraction (XRD) shows the samples to be amorphous. Fourier transform infrared (FTIR) spectroscopy indicates complexation between the cation of the salt and the oxygen atom of the C=O and -COO- groups of MG30. From electrochemical impedance spectroscopy (EIS), MG30 with 30 wt% LiCF{sub 3}SO{sub 3} salt exhibits the highest ambient conductivity of 1.69 Multiplication-Sign 10{sup -6} S cm{sup -1} and lowest activation energy of 0.24 eV. The dielectric behavior has been analyzed using dielectric permittivity ({epsilon} Prime), dissipation factor (tan {delta}) and dielectric modulus (M{sup Low-Asterisk }) of the samples. The dielectric constant of pure MG30 has been estimated to be {approx}1.86.

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

Directory of Open Access Journals (Sweden)

Dai Jing

2009-06-01

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

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

Directory of Open Access Journals (Sweden)

Moayad Hossaini Sadr

2011-12-01

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

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

Directory of Open Access Journals (Sweden)

Evgeny Bulatov

2014-02-01

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

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

Directory of Open Access Journals (Sweden)

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.

Isotypic crystal structures of 1-benzyl-4-(4-bromophenyl-2-imino-1,2,5,6,7,8,9,10-octahydrocycloocta[b]pyridine-3-carbonitrile and 1-benzyl-4-(4-fluorophenyl-2-imino-1,2,5,6,7,8,9,10-octahydrocycloocta[b]pyridine-3-carbonitrile

Directory of Open Access Journals (Sweden)

R. A. Nagalakshmi

2014-11-01

Full Text Available The molecules of the two isotypic title compounds, C25H24BrN3, (I, and C25H24FN3, (II, comprise a 2-iminopyridine ring fused with a cyclooctane ring. In (I, the cyclooctane ring adopts a twisted chair–chair conformation, while in (II, this ring adopts a twisted boat–chair conformation. The dihedral angles between the planes of the pyridine ring and the bromobenzene and phenyl rings are 80.14 (12 and 71.72 (13°, respectively, in (I. The equivalent angles in (II are 75.25 (8 and 68.34 (9°, respectively. In both crystals, inversion dimers linked by pairs of C—H...N interactions generate R22(14 loops, which are further connected by weak C—H...π interactions, generating (110 sheets.

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

Science.gov (United States)

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

2007-07-23

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

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

Directory of Open Access Journals (Sweden)

Alain Igau

2013-12-01

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

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

Directory of Open Access Journals (Sweden)

Tara Shahani

2010-06-01

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

Toxicity of fatty acid 18:5n3 from Gymnodinium cf. mikimotoi: II. Intracellular pH and K+ uptake in isolated trout hepatocytes.

Science.gov (United States)

Fossat, B; Porthé-Nibelle, J; Sola, F; Masoni, A; Gentien, P; Bodennec, G

1999-01-01

Effects of octadecapentaenoic acid 18:5n3 and other related polyunsaturated fatty acids present in gymnodinium cf. mikimotoi were tested in isolated trout hepatocytes. These exotoxins decreased intracellular pH followed by a slow recovery to initial value and alkalinization of acidic compartments, suggesting an inhibition of vacuolar H(+)-ATPases. Moreover, addition of 18:5n3 to the extracellular medium induced a decrease of K+ uptake into hepatocytes as a result of Na,K-ATPase inhibition. However, high concentrations (10(-5)-10(-3) M) are necessary to induce these effects.

N-Heterocyclic Carbene Coinage Metal Complexes of the Germanium-Rich Metalloid Clusters [Ge9R3]− and [Ge9RI2]2− with R = Si(iPr3 and RI = Si(TMS3

Directory of Open Access Journals (Sweden)

Felix S. Geitner

2017-07-01

Full Text Available We report on the synthesis of novel coinage metal NHC (N-heterocyclic carbene compounds of the germanium-rich metalloid clusters [Ge9R3]− and [Ge9RI2]2− with R = Si(iPr3 and RI = Si(TMS3. NHCDippCu{η3Ge9R3} with R = Si(iPr3 (1 represents a less bulky silyl group-substituted derivative of the known analogous compounds with R = Si(iBu3 or Si(TMS3. The coordination of the [NHCDippCu]+ moiety to the cluster unit occurs via one triangular face of the tri-capped trigonal prismatic [Ge9] cluster. Furthermore, a series of novel Zintl cluster coinage metal NHC compounds of the type (NHCM2{η3Ge9RI2} (RI = Si(TMS3 M = Cu, Ag and Au; NHC = NHCDipp or NHCMes is presented. These novel compounds represent a new class of neutral dinuclear Zintl cluster coinage metal NHC compounds, which are obtained either by the stepwise reaction of a suspension of K12Ge17 with Si(TMS3Cl and the coinage metal carbene complexes NHCMCl (M = Cu, Ag, Au, or via a homogenous reaction using the preformed bis-silylated cluster K2[Ge9(Si(TMS32] and the corresponding NHCMCl (M = Cu, Ag, Au complex. The molecular structures of NHCDippCu{η3Ge9(Si(iPr33} (1 and (NHCDippCu2{η3-Ge9(Si(TMS32} (2 were determined by single crystal X-ray diffraction methods. In 2, the coordination of the [NHCDippCu]+ moieties to the cluster unit takes place via both open triangular faces of the [Ge9] entity. Furthermore, all compounds were characterized by means of NMR spectroscopy (1H, 13C, 29Si and ESI-MS.

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

Directory of Open Access Journals (Sweden)

Assem Barakat

2016-09-01

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

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

Science.gov (United States)

Yıldırım, İlkay; Karabulut, Bünyamin

2011-03-01

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

AGC-3 Experiment Irradiation Monitoring Data Qualification Final Report

Energy Technology Data Exchange (ETDEWEB)

Laurence Hull

2014-10-01

The Graphite Technology Development Program will run a series of six experiments to quantify the effects of irradiation on nuclear grade graphite. The third experiment, Advanced Graphite Creep 3 (AGC 3), began with Advanced Test Reactor (ATR) Cycle 152B on November 27, 2012, and ended with ATR Cycle 155B on April 23, 2014. This report documents qualification of AGC 3 experiment irradiation monitoring data for use by the Very High Temperature Reactor (VHTR) Technology Development Office (TDO) Program for research and development activities required to design and license the first VHTR nuclear plant. Qualified data meet the requirements for data collection and use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements. Trend data may not meet the requirements, but may still provide some useable information. All thermocouples (TCs) functioned throughout the AGC 3 experiment. There was one interval between December 18, 2012, and December 20, 2012, where 10 NULL values were reported for various TCs. These NULL values were deleted from the Nuclear Data Management and Analysis System database. All temperature data are Qualified for use by the VHTR TDO Program. Argon, helium, and total gas flow data were within expected ranges and are Qualified for use by the VHTR TDO Program. Total gas flow was approximately 50 sccm through the AGC 3 experiment capsule. Helium gas flow was briefly increased to 100 sccm during ATR shutdowns. At the start of the AGC 3 experiment, moisture in the outflow gas line was stuck at a constant value of 335.6174 ppmv for the first cycle (Cycle 152B). When the AGC 3 experiment capsule was reinstalled in ATR for Cycle 154B, a new moisture filter was installed. Moisture data from Cycle 152B are Failed. All moisture data from the final three cycles (Cycles 154B, 155A, and 155B) are Qualified for use by the VHTR TDO Program.

Poly[[(μ4-benzene-1,3,5-tricarboxylato-κ4O1:O1′:O2:O3bis(2,2-bipyridine-κ2N,N′(μ2-hydroxidodicopper(II] trihydrate

Directory of Open Access Journals (Sweden)

Mohamed N. El-kaheli

2014-07-01

Full Text Available In the title two-dimensional coordination polymer, {[Cu2(C9H3O6(OH(C10H8N22]·3H2O}n, each of the two independent CuII atoms is coordinated by a bridging OH group, two O atoms from two benzene-1,3,5-tricarboxylate (L ligands and two N atoms from a 2,2- bipyridine (bipy ligand in a distorted square-pyramidal geometry. Each L ligand coordinates four CuII atoms, thus forming a polymeric layer parallel to the bc plane with bipy molecules protruding up and down. The lattice water molecules involved in O—H...· O hydrogen bonding are situated in the inner part of each layer. The crystal packing is consolidated by π–π interactions between the aromatic rings of bipy ligands from neigbouring layers [intercentroid distance = 3.762 (3 Å].

Disordered crystal structure of 20H-AlON, Al10O3N8

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Science.gov (United States)

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

2009-07-06

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

Bis[tris(propane-1,3-diamine-κ2N,N′nickel(II] diaquabis(propane-1,3-diamine-κ2N,N′nickel(II hexabromide dihydrate

Directory of Open Access Journals (Sweden)

Aymen Yangui

2014-06-01

Full Text Available In the title compound, [Ni(C3H10N23]2[Ni(C3H10N22(H2O2]Br6·2H2O, one Ni2+ cation, located on an inversion centre, is coordinated by four N atoms from two ligands and by two water O atoms. The other Ni2+ cation, located in a general position, is coordinated by six N atoms from three ligands. In both cases, the Ni2+ cation has an octahedral coordination environment. The overall structural cohesion is ensured by three types of hydrogen bonds, N—H...Br, O—H...Br and O—H...O, which connect the two types of complex cations, the bromide counter-anions and the lattice water molecules into a three-dimensional network.

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

Directory of Open Access Journals (Sweden)

Muhammad Hafeez

2013-12-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Directory of Open Access Journals (Sweden)

Ankur Trigunait

2010-08-01

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

(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

Directory of Open Access Journals (Sweden)

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.

Bis[(E-N-(pyridin-3-ylmethylidenehydroxylamine-κN1]silver(I perchlorate

Directory of Open Access Journals (Sweden)

Jing Xu

2012-06-01

Full Text Available Each of the ions in the title salt, [Ag(C6H6N2O2]ClO4, is completed by the application of crystallographic twofold symmetry. The AgI atom is coordinated by two pyridine N atoms in an almost linear fashion [N—Ag—N = 170.0 (2°], with the T-shaped coordination geometry being completed by a weakly associated perchlorate-O atom. Supramolecular zigzag chains along [100] mediated by O—H...N hydrogen bonds [as parts of R22(6 loops] feature in the crystal packing. The perchlorate O atoms are disordered over two sets of sites in a statistical ratio.

Bis[μ-1,2-bis(1H-imidazol-1-ylmethylbenzene-κ2N3:N3′]disilver(I 3-carboxylato-4-hydroxybenzenesulfonate methanol solvate trihydrate

Directory of Open Access Journals (Sweden)

Hong-Mei Sun

2009-09-01

Full Text Available In the title compound, [Ag2(C14H14N42](C7H4O6S·CH3OH·3H2O, the complex dication has a binuclear structure in which each AgI ion is two-coordinated in a slightly distorted linear coordination geometry. The two AgI atoms are bridged by two 1,2-bis[(1H-imidazol-1-ylmethyl]benzene (IBI ligands, forming a 22-membered ring. In the dication, π–π interactions are observed between the imidazole rings with centroid–centroid distances of 3.472 (3 and 3.636 (3 Å. In the crystal, the uncoordinated water molecules, anions and methanol solvent molecules are linked into chains along the b axis by O—H...O hydrogen bonds. In addition, π–π interactions are observed between the benzene rings of the IBI ligands, with a centroid–centroid distance of 3.776 (2 Å. The sulfonate group is disordered over two orientations with occupancies of 0.676 (12 and 0.324 (12.

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

Directory of Open Access Journals (Sweden)

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.

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

Directory of Open Access Journals (Sweden)

Khaled Boukebbous

2016-10-01

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

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

Directory of Open Access Journals (Sweden)

Hakima Chicha

2014-06-01

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

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

Directory of Open Access Journals (Sweden)

Ahmed Benharref

2015-08-01

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

Atmospheric chemistry of (CF3)2CFOCH3

DEFF Research Database (Denmark)

Andersen, Lene Løffler; Østerstrøm, Freja From; Nielsen, Ole John

2014-01-01

FTIR smog chamber techniques were used to measure k(Cl + (CF 3)2CFOCH3) = (1.80 ± 0.42) × 10-13, k(Cl + (CF3)2CFOCHO) = (1.47 ± 0.56) × 10-14, and k(OH + (CF3) 2CFOCH3) = (1.55 ± 0.24) × 10-14 cm3 molecule-1 s-1. The chlorine-atom initiated oxidation of (CF3)2CFOCH3 in air in the absence of NOX r...

Atmospheric chemistry of CF3CF═CH2 and (Z)-CF3CF═CHF: Cl and NO3 rate coefficients, Cl reaction product yields, and thermochemical calculations.

Science.gov (United States)

Papadimitriou, Vassileios C; Lazarou, Yannis G; Talukdar, Ranajit K; Burkholder, James B

2011-01-20

Rate coefficients, k, for the gas-phase reactions of Cl atoms and NO(3) radicals with 2,3,3,3-tetrafluoropropene, CF(3)CF═CH(2) (HFO-1234yf), and 1,2,3,3,3-pentafluoropropene, (Z)-CF(3)CF═CHF (HFO-1225ye), are reported. Cl-atom rate coefficients were measured in the fall-off region as a function of temperature (220-380 K) and pressure (50-630 Torr; N(2), O(2), and synthetic air) using a relative rate method. The measured rate coefficients are well represented by the fall-off parameters k(0)(T) = 6.5 × 10(-28) (T/300)(-6.9) cm(6) molecule(-2) s(-1) and k(∞)(T) = 7.7 × 10(-11) (T/300)(-0.65) cm(3) molecule(-1) s(-1) for CF(3)CF═CH(2) and k(0)(T) = 3 × 10(-27) (T/300)(-6.5) cm(6) molecule(-2) s(-1) and k(∞)(T) = 4.15 × 10(-11) (T/300)(-0.5) cm(3) molecule(-1) s(-1) for (Z)-CF(3)C═CHF with F(c) = 0.6. Reaction product yields were measured in the presence of O(2) to be (98 ± 7)% for CF(3)C(O)F and (61 ± 4)% for HC(O)Cl in the CF(3)CF═CH(2) reaction and (108 ± 8)% for CF(3)C(O)F and (112 ± 8)% for HC(O)F in the (Z)-CF(3)CF═CHF reaction, where the quoted uncertainties are 2σ (95% confidence level) and include estimated systematic errors. NO(3) reaction rate coefficients were determined using absolute and relative rate methods. Absolute measurements yielded upper limits for both reactions between 233 and 353 K, while the relative rate measurements yielded k(3)(295 K) = (2.6 ± 0.25) × 10(-17) cm(3) molecule(-1) s(-1) and k(4)(295 K) = (4.2 ± 0.5) × 10(-18) cm(3) molecule(-1) s(-1) for CF(3)CF═CH(2) and (Z)-CF(3)CF═CHF, respectively. The Cl-atom reaction with CF(3)CF═CH(2) and (Z)-CF(3)CF═CHF leads to decreases in their atmospheric lifetimes and global warming potentials and formation of a chlorine-containing product, HC(O)Cl, for CF(3)CF═CH(2). The NO(3) reaction has been shown to have a negligible impact on the atmospheric lifetimes of CF(3)CF═CH(2) and (Z)-CF(3)CF═CHF. The energetics for the reaction of Cl, NO(3), and OH with CF

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

Directory of Open Access Journals (Sweden)

2009-03-01

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

Synthesis, modelling, and mu-opioid receptor affinity of N-3(9)-arylpropenyl-N-9(3)-propionyl-3,9-diazabicycl.

Science.gov (United States)

Pinna, G A; Murineddu, G; Curzu, M M; Villa, S; Vianello, P; Borea, P A; Gessi, S; Toma, L; Colombo, D; Cignarella, G

2000-08-01

A series of N-3-arylpropenyl-N-9-propionyl-3,9-diazabicyclo[3.3.1]nonanes (1a-g) and of reverted N-3-propionyl-N-9-arylpropenyl isomers (2a-g), as homologues of the previously reported analgesic 3,8-diazabicyclo[3.2.1]octanes (I-II), were synthesized and evaluated for the binding affinity towards opioid receptor subtypes mu, delta and kappa. Compounds 1a-g and 2a-g exhibited a strong selective mu-affinity with Ki values in the nanomolar range, which favourably compared with those of I and II. In addition, contrary to the trend observed for DBO-I, II, the mu-affinity of series 2 is markedly higher than that of the isomeric series 1. This aspect was discussed on the basis of the conformational studies performed on DBN which allowed hypotheses on the mode of interaction of these compounds with the mu receptor.

cis-Tetra­chloridobis(1H-imidazole-κN 3)platinum(IV)

Science.gov (United States)

Bokach, Nadezhda A.; Kukushkin, Vadim Yu.; Izotova, Yulia A.; Usenko, Natalia I.; Haukka, Matti

2012-01-01

In the title complex, cis-[PtCl4(C3H4N2)2], the PtIV ion lies on a twofold rotation axis and is coordinated in a slightly distorted octa­hedral geometry. The dihedral angle between the imidazole rings is 69.9 (2)°. In the crystal, mol­ecules are linked by N—H⋯Cl hydrogen bonds, forming a three-dimensional network. PMID:22590070

Structure of Sr3V10O28.22H2O

International Nuclear Information System (INIS)

Nieto, J.M.; Salagre, P.; Medina, F.; Sueiras, J.E.; Solans, X.

1993-01-01

The crystal structure of hydrated strontium decavanadate, Sr 3 V 10 O 28 .22H 2 O, has been determined. It contains two types of strontium ions: the first is coordinated to seven water molecules which define a pentagonal bipyramid; the second bonds to five molecules of water and three O atoms of different decavanadate ions, thereby bridging between decavanadate ions to produce layers of formula [Sr 2 V 10 O 38 H 20 ] n on the crystallographic plane (100). The heptacoordinated Sr and the five molecules of water associated with it are located between the different layers. (orig.)

Nd(NH2SO3)(SO4) . 1.5 H2O: a non-centrosymmetric amidosulfate-sulfate of neodymium

International Nuclear Information System (INIS)

Wickleder, M.S.

2005-01-01

The thermal decomposition of Nd(NH 2 SO 3 ) 3 . 2 H 2 O in a closed tube leads to violet single crystals of Nd(NH 2 SO 3 )(SO 4 ) . 1.5 H 2 O. The compound crystallizes with the space group P1 (Z = 2, a = 689.2, b = 691.4, c = 962.0 pm, α = 109.64, β = 97.00, γ = 109.62 ). The triclinic unit cell can be transformed into the respective bodycentered setting I1 (Z = 2, a = 977.9, b = 795.6, c = 1113.0 pm, α = 90.69, β = 115.06, γ = 88.98 ) leading to a nearly monoclinic unit cell for the compound. In the crystal structure of Nd(NH 2 SO 3 )(SO 4 ) . 1.5 H 2 O two Nd 3+ ions are present. Nd(1) 3+ is coordinated by four NH 2 SO 3 - and two SO 4 2- ions, and one H 2 O molecule. Owing to the chelating attack of the sulfate groups, the CN is nine. Nd(2) 3+ is surrounded by four monodentate SO 4 2- and two NH 2 SO 3 - groups. Two H 2 O ligands fill up the coordination sphere and lead to a CN of eight. The linkage of the polyhedra leads to a three-dimensional network. (orig.)

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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

Directory of Open Access Journals (Sweden)

Ya-Wen Zhang

2009-08-01

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

Synthesis, crystal structure and biological activity of a novel 1,2,3-thidiazole compound

International Nuclear Information System (INIS)

Ke, W.

2013-01-01

A new 1,2,3-thiadiazole compound was synthesized and characterized by 1H NMR, MS and HRMS. The crystal structure of the title compound (C/sub 12/H/sub 11/ClN/sub 2/O/sub 4/S/sub 2/, Mr = 346.80) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 with a = 8.4425(17) A, b = 8.9801(18) A, c = 9.859(2) A, alpha = 84.36(3) degree, beta = 86.71(3)degree, lambda = 83.25(3) degree, V = 737.9(3)A3, Z 2, F(000) = 356, Dc = 1.561 g/cm/sup 3/, mu = 0.557 mm-1, the final R1 0.0380 and wR2 = 0.0982 for 2160 observed reflections with I > 2sigma(I). A total of 12585 reflections were collected, of which 2601 were independent (Rint 0.0364). The herbicidal activity of title compound was determined, the results showed the title compound displayed excellent herbicidal activity against Brassica campestris. (author)

Chemical consequences of radioactive decay. 1. Study of 249Cf ingrowth into crystalline 249BkBr3: a new crystalline phase of CfBr3

International Nuclear Information System (INIS)

Young, J.P.; Haire, R.G.; Peterson, J.R.; Ensor, D.D.; Fellows, R.L.

1980-01-01

Spectrophotometric and x-ray powder diffraction methods have been applied to a study of the ingrowth of californium-249 by β - decay of berkelium-249 in crystalline 249 BkBr 3 . It was found that the Cf daughter grows in with the same oxidation state and crystal structure as the parent. Thus, six-coordinate BkBr 3 (AlCl 3 -type monoclinic structure) generates six-coordinate CfBr 3 , and eight-coordinate BkBr 3 (PuBr 3 -type orthorhombic structure) generates eight-coordinate CfBr 3 , a previously unknown form of CfBr 3 . It was also found that the daughter Cf(III) in the BkBr 3 parent compound can be reduced to Cf(II) by treatment with H 2 , as it can in pure CfBr 3 . 5 figures

Diaqua?bis?(1,10-phenanthroline-?2 N,N?)manganese(II) sulfate hexa?hydrate

OpenAIRE

Zhang, Chun; Zhu, Hong-lin

2010-01-01

In the title compound, [Mn(C12H8N2)2(H2O)2]SO4·6H2O, the complex cations assemble into positively charged sheets parallel to (010) via intermolecular π–π stacking interactions with a mean interplanar distance of 3.410 (6) along [100] and 3.465 (5) Å along [001]. The sulfate anions and uncoordinated water molecules are interconnected between these layers by hydrogen bonds, forming negatively charged layers which are li...

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

Directory of Open Access Journals (Sweden)

Mohamed Mokhtar Mohamed Abdelahi

2017-05-01

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

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

International Nuclear Information System (INIS)

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

1993-01-01

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

[2,9-Bis(3,5-dimethyl-1H-pyrazol-1-yl-κN2-1,10-phenanthroline-κ2N,N′]bis(thiocyanato-κNcadmium(II

Directory of Open Access Journals (Sweden)

Yan Hui Chi

2011-01-01

Full Text Available In the title complex, [Cd(NCS2(C22H20N6], the CdII ion is in a CdN6 coordination geometry which is intermediate between octahedral and trigonal–prismatic. The dihedral angles formed between the mean planes of the pyrazole rings and the phenanthroline system are 15.74 (15 and 16.30 (13°. In the crystal, there is a π–π stacking interaction involving two symmetry-related pyrazole rings, with a centroid–centroid distance of 3.664 (3 Å. In addition, there is a relatively short intermolecular contact between C atoms [C...C = 3.399 (6 Å] involving symmetry-related pyridine rings along the a axis.

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

Directory of Open Access Journals (Sweden)

Fortune Ezemobi

2014-12-01

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

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

International Nuclear Information System (INIS)

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

1996-01-01

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

Silver(I) complexes of the weakly coordinating solvents SO(2) and CH(2)Cl(2): crystal structures, bonding, and energetics of [Ag(OSO)][Al{OC(CF(3))(3)}(4)], [Ag(OSO)(2/2)][SbF(6)], and [Ag(CH(2)Cl(2))(2)][SbF(6)].

Science.gov (United States)

Decken, Andreas; Knapp, Carsten; Nikiforov, Grigori B; Passmore, Jack; Rautiainen, J Mikko; Wang, Xinping; Zeng, Xiaoqing

2009-06-22

Pushing the limits of coordination chemistry: The most weakly coordinated silver complexes of the very weakly coordinating solvents dichloromethane and liquid sulfur dioxide were prepared. Special techniques at low temperatures and the use of weakly coordinating anions allowed structural characterization of [Ag(OSO)][Al{OC(CF(3))(3)}(4)], [Ag(OSO)(2/2)][SbF(6)], and [Ag(Cl(2)CH(2))(2)][SbF(6)] (see figure). An investigation of the bonding shows that these complexes are mainly stabilized by electrostatic monopole-dipole interactions.The synthetically useful solvent-free silver(I) salt Ag[Al(pftb)(4)] (pftb=--OC(CF(3))(3)) was prepared by metathesis reaction of Li[Al(pftb)(4)] with Ag[SbF(6)] in liquid SO(2). The solvated complexes [Ag(OSO)][Al(pftb)(4)], [Ag(OSO)(2/2)][SbF(6)], and [Ag(CH(2)Cl(2))(2)][SbF(6)] were prepared and isolated by special techniques at low temperatures and structurally characterized by single-crystal X-ray diffraction. The SO(2) complexes provide the first examples of coordination of the very weak Lewis base SO(2) to silver(I). The SO(2) molecule in [Ag(OSO)][Al(pftb)(4)] is eta(1)-O coordinated to Ag(+), while the SO(2) ligands in [Ag(OSO)(2/2)][SbF(6)] bridge two Ag(+) ions in an eta(2)-O,O' (trans,trans) manner. [Ag(CH(2)Cl(2))(2)][SbF(6)] contains [Ag(CH(2)Cl(2))(2)](+) ions linked through [SbF(6)](-) ions to give a polymeric structure. The solid-state silver(I) ion affinities (SIA) of SO(2) and CH(2)Cl(2), based on bond lengths and corresponding valence units in the corresponding complexes and tensimetric titrations of Ag[Al(pftb)(4)] and Ag[SbF(6)] with SO(2) vapor, show that SO(2) is a weaker ligand to Ag(+) than the commonly used weakly coordinating solvent CH(2)Cl(2) and indicated that binding strength of SO(2) to silver(I) in the silver(I) salts increases with increasing size of the corresponding counteranion ([Al(pftb)(4)](-)>[SbF(6)](-)). The experimental findings are in good agreement with theoretical gas-phase ligand

Crystal structure of bis(μ-3-nitrobenzoato-κ3O,O′:O;κ3O:O,O′-bis[bis(3-cyanopyridine-κN1(3-nitrobenzoato-κ2O,O′cadmium

Directory of Open Access Journals (Sweden)

Tuncer Hökelek

2017-03-01

Full Text Available The asymmetric unit of the title compound, [Cd2(C7H4NO44(C6H4N24], contains one CdII atom, two 3-nitrobenzoate (NB anions and two 3-cyanopyridine (CPy ligands. The two CPy ligands act as monodentate N(pyridine-bonding ligands, while the two NB anions act as bidentate ligands through the carboxylate O atoms. The centrosymmetric dinuclear complex is generated by application of inversion symmetry, whereby the CdII atoms are bridged by the carboxylate O atoms of two symmetry-related NB anions, thus completing the distorted N2O5 pentagonal–bipyramidal coordination sphere of each CdII atom. The benzene and pyridine rings are oriented at dihedral angles of 10.02 (7 and 5.76 (9°, respectively. In the crystal, C—H...N hydrogen bonds link the molecules, enclosing R22(26 ring motifs, in which they are further linked via C—H...O hydrogen bonds, resulting in a three-dimensional network. In addition, π–π stacking interactions between parallel benzene rings and between parallel pyridine rings of adjacent molecules [shortest centroid-to-centroid distances = 3.885 (1 and 3.712 (1 Å, respectively], as well as a weak C—H...π interaction, may further stabilize the crystal structure.

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)

In silico probing and biological evaluation of SETDB1/ESET-targeted novel compounds that reduce tri-methylated histone H3K9 (H3K9me3) level

Science.gov (United States)

Park, Insun; Hwang, Yu Jin; Kim, TaeHun; Viswanath, Ambily Nath Indu; Londhe, Ashwini M.; Jung, Seo Yun; Sim, Kyoung Mi; Min, Sun-Joon; Lee, Ji Eun; Seong, Jihye; Kim, Yun Kyung; No, Kyoung Tai; Ryu, Hoon; Pae, Ae Nim

2017-10-01

ERG-associated protein with the SET domain (ESET/SET domain bifurcated 1/SETDB1/KMT1E) is a histone lysine methyltransferase (HKMT) and it preferentially tri-methylates lysine 9 of histone H3 (H3K9me3). SETDB1/ESET leads to heterochromatin condensation and epigenetic gene silencing. These functional changes are reported to correlate with Huntington's disease (HD) progression and mood-related disorders which make SETDB1/ESET a viable drug target. In this context, the present investigation was performed to identify novel peptide-competitive small molecule inhibitors of the SETDB1/ESET by a combined in silico-in vitro approach. A ligand-based pharmacophore model was built and employed for the virtual screening of ChemDiv and Asinex database. Also, a human SETDB1/ESET homology model was constructed to supplement the data further. Biological evaluation of the selected 21 candidates singled out 5 compounds exhibiting a notable reduction of the H3K9me3 level via inhibitory potential of SETDB1/ESET activity in SETDB1/ESET-inducible cell line and HD striatal cells. Later on, we identified two compounds as final hits that appear to have neuronal effects without cytotoxicity based on the result from MTT assay. These compounds hold the calibre to become the future lead compounds and can provide structural insights into more SETDB1/ESET-focused drug discovery research. Moreover, these SETDB1/ESET inhibitors may be applicable for the preclinical study to ameliorate neurodegenerative disorders via epigenetic regulation.

In silico probing and biological evaluation of SETDB1/ESET-targeted novel compounds that reduce tri-methylated histone H3K9 (H3K9me3) level.

Science.gov (United States)

Park, Insun; Hwang, Yu Jin; Kim, TaeHun; Viswanath, Ambily Nath Indu; Londhe, Ashwini M; Jung, Seo Yun; Sim, Kyoung Mi; Min, Sun-Joon; Lee, Ji Eun; Seong, Jihye; Kim, Yun Kyung; No, Kyoung Tai; Ryu, Hoon; Pae, Ae Nim

2017-10-01

ERG-associated protein with the SET domain (ESET/SET domain bifurcated 1/SETDB1/KMT1E) is a histone lysine methyltransferase (HKMT) and it preferentially tri-methylates lysine 9 of histone H3 (H3K9me3). SETDB1/ESET leads to heterochromatin condensation and epigenetic gene silencing. These functional changes are reported to correlate with Huntington's disease (HD) progression and mood-related disorders which make SETDB1/ESET a viable drug target. In this context, the present investigation was performed to identify novel peptide-competitive small molecule inhibitors of the SETDB1/ESET by a combined in silico-in vitro approach. A ligand-based pharmacophore model was built and employed for the virtual screening of ChemDiv and Asinex database. Also, a human SETDB1/ESET homology model was constructed to supplement the data further. Biological evaluation of the selected 21 candidates singled out 5 compounds exhibiting a notable reduction of the H3K9me3 level via inhibitory potential of SETDB1/ESET activity in SETDB1/ESET-inducible cell line and HD striatal cells. Later on, we identified two compounds as final hits that appear to have neuronal effects without cytotoxicity based on the result from MTT assay. These compounds hold the calibre to become the future lead compounds and can provide structural insights into more SETDB1/ESET-focused drug discovery research. Moreover, these SETDB1/ESET inhibitors may be applicable for the preclinical study to ameliorate neurodegenerative disorders via epigenetic regulation.

AGC-3 Experiment Irradiation Monitoring Data Qualification Final Report

Energy Technology Data Exchange (ETDEWEB)

Hull, Laurence C. [Idaho National Lab. (INL), Idaho Falls, ID (United States). VHTR Technology Development Office

2014-08-01

The Graphite Technology Development Program will run a series of six experiments to quantify the effects of irradiation on nuclear-grade graphite. The third experiment, Advanced Graphite Creep 3 (AGC-3), began with Advanced Test Reactor (ATR) Cycle 152B on November 27, 2012, and ended with ATR Cycle 155B on April 23, 2014. This report documents qualification of AGC-3 experiment irradiation monitoring data for use by the Very High Temperature Reactor (VHTR) Technology Development Office (TDO) Program for research and development activities required to design and license the first VHTR nuclear plant. Qualified data meet the requirements for data collection and use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements. Trend data may not meet the requirements, but may still provide some useable information. The report documents qualification of AGC-3 experiment irradiation monitoring data following MCP-2691. This report also documents whether AGC-3 experiment irradiation monitoring data meet the requirements for data collection as specified in technical and functional requirements documents and quality assurance (QA) plans. Data handling is described showing how data are passed from the data collection experiment to the Nuclear Data Management and Analysis System (NDMAS) team. The data structure is described, including data batches, components, attributes, and response variables. The description of the approach to data qualification includes the steps taken to qualify the data and the specific tests used to verify that the data meet requirements. Finally, the current status of the data received by NDMAS from the AGC-3 experiment is presented with summarized information on test results and resolutions. This report addresses all of the irradiation monitoring data collected during the AGC-3 experiment.

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.

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

Directory of Open Access Journals (Sweden)

Hoong-Kun Fun

2012-08-01

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

New family of lanthanide-based inorganic-organic hybrid frameworks: Ln2(OH)4[O3S(CH2)nSO3]·2H2O (Ln = La, Ce, Pr, Nd, Sm; n = 3, 4) and their derivatives.

Science.gov (United States)

Liang, Jianbo; Ma, Renzhi; Ebina, Yasuo; Geng, Fengxia; Sasaki, Takayoshi

2013-02-18

We report the synthesis and structure characterization of a new family of lanthanide-based inorganic-organic hybrid frameworks, Ln(2)(OH)(4)[O(3)S(CH(2))(n)SO(3)]·2H(2)O (Ln = La, Ce, Pr, Nd, Sm; n = 3, 4), and their oxide derivatives. Highly crystallized samples were synthesized by homogeneous precipitation of Ln(3+) ions from a solution containing α,ω-organodisulfonate salts promoted by slow hydrolysis of hexamethylenetetramine. The crystal structure solved from powder X-ray diffraction data revealed that this material comprises two-dimensional cationic lanthanide hydroxide {[Ln(OH)(2)(H(2)O)](+)}(∞) layers, which are cross-linked by α,ω-organodisulfonate ligands into a three-dimensional pillared framework. This hybrid framework can be regarded as a derivative of UCl(3)-type Ln(OH)(3) involving penetration of organic chains into two {LnO(9)} polyhedra. Substitutional modification of the lanthanide coordination promotes a 2D arrangement of the {LnO(9)} polyhedra. A new hybrid oxide, Ln(2)O(2)[O(3)S(CH(2))(n)SO(3)], which is supposed to consist of alternating {[Ln(2)O(2)](2+)}(∞) layers and α,ω-organodisulfonate ligands, can be derived from the hydroxide form upon dehydration/dehydroxylation. These hybrid frameworks provide new opportunities to engineer the interlayer chemistry of layered structures and achieve advanced functionalities coupled with the advantages of lanthanide elements.

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

Directory of Open Access Journals (Sweden)

Makuteswaran Sridharan

2008-11-01

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

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

Directory of Open Access Journals (Sweden)

Natsumi Ohira

2016-05-01

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

Crystal structures of 2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-ethoxyprop-2-en-1-ide and bis(2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-(dicyanomethylenepropane-1,3-diide

Directory of Open Access Journals (Sweden)

Zouaoui Setifi

2015-05-01

Full Text Available In 2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-ethoxyprop-2-en-1-ide, C10H9N2+·C9H5N4O−, (I, the ethyl group in the anion is disordered over two sets of atomic sites with occupancies 0.634 (9 and 0.366 (9, and the dihedral angle between the ring planes in the cation is 2.11 (7°. The two independent C(CN2 groups in the anion make dihedral angles of 10.60 (6 and 12.44 (4° with the central propenide unit, and the bond distances in the anion provide evidence for extensive electronic delocalization. In bis(2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-(dicyanomethylenepropane-1,3-diide [alternative name bis(2,2′-bipyridin-1-ium tris(dicyanomethylenemethanediide], 2C10H9N2+·C10N62− (II, the dihedral angles between the ring planes in the two independent cations are 7.7 (2 and 10.92 (17°. The anion exhibits approximate C3 symmetry, consistent with extensive electronic delocalization, and the three independent C(CN2 groups make dihedral angles of 23.8 (2, 27.0 (3 and 27.4 (2° with the central plane. The ions in (I are linked by an N—H...N hydrogen bond and the resulting ion pairs are linked by two independent C—H...N hydrogen bonds, forming a ribbon containing alternating R44(18 and R44(26 rings, where both ring types are centrosymmetric. The ions in (II are linked by two independent N—H...N hydrogen bonds and the resulting ion triplets are linked by a C—H...N hydrogen bond, forming a C21(7 chain containing anions and only one type of cation, with the other cation linked to the chain by a further C—H...N hydrogen bond.

Synthesis, characterization and thermal decomposition of [Pd2 (C2-dmba (µ-SO4 (SO22

Directory of Open Access Journals (Sweden)

Caires Antonio Carlos Fávero

1998-01-01

Full Text Available The bridged sulphate complex [Pd2 (C²,dmba (µ-SO4 (SO22] has been obtained by reacting a saturated solution of SO2 in methanol and the cyclometallated compound [Pd(C²,N-dmba(µ-N3] 2; (dmba = N,N-dimethylbenzylamine, at room temperature for 24 h. Reaction product was characterized by elemental analysis, NMR comprising 13C{¹H} and ¹H nuclei and I.R. spectrum's measurements. Thermal behavior has been investigated and residual products identified by X-ray powder diffraction.

CO2 Capture and Separation Properties in the Ionic Liquid 1-n-Butyl-3-Methylimidazolium Nonafluorobutylsulfonate

Directory of Open Access Journals (Sweden)

Lingyun Zhou

2014-05-01

Full Text Available Recently, the use of ionic liquids (ILs for carbon capture and separation processes has gained great interest by many researchers due to the high solubility of CO2 in ILs. In the present work, solubility measurements of CO2 in the novel IL 1-n-butyl-3-methylimidazolium nonafluorobutylsulfonate [C4mim][CF3CF2CF2CF2SO3] were performed with a high-pressure view-cell technique in the temperature range from 293.15 to 343.15 K and pressures up to about 4.2 MPa. For comparison, solubilities of H2, N2, and O2 in the IL were also measured at 323.15 K via the same procedure. The Krichevsky-Kasarnovsky equation was employed to correlate the measured solubility data. Henry’s law constants, enthalpies, and entropies of absorption for CO2 in the IL were also determined and presented. The CO2 solubility in this IL was compared with other ILs sharing the same cation. It was shown that the solubility of CO2 in these ILs follows the sequence: [C4mim][CF3CF2CF2CF2SO3] ≈ [C4mim][Tf2N] > [C4mim][CF3CF2CF2COO] > [C4mim][BF4], and the solubility selectivity of CO2 relative to O2, N2, and H2 in [C4mim][CF3CF2CF2CF2SO3] was 8, 16, and 22, respectively. Furthermore, this IL is regenerable and exhibits good stability. Therefore, the IL reported here would be a promising sorbent for CO2.

1,4,9,12-Tetramethoxy-14-octyl-5,8-dihydrodiindolo[3,2-b;2′,3′-h]carbazole with an unknown solvent

Directory of Open Access Journals (Sweden)

Norma Wrobel

2017-03-01

Full Text Available The title compound, 2C36H39N3O4·H2O, is a linear π-conjugated ladder oligomer with an alkyl chain on the central nitrogen atom. This diindolocarbazole, prepared via a twofold Cadogan reaction, adopts a sligthly convex shape, anti to the disordered octyl group. The unit cell contains nine molecules of the title compound and half a water molecule per main molecule. The water molecule forms hydrogen bridges, connecting the carbazole-NH and methoxy groups of different molecules. The crystal contains solvent molecules which are located in a channel parallel to the c axis. It was not possible to determine the position and nature of the solvent (a mixure of choroform, n-pentane and DMSO. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option of PLATON was used to model the missing electron density. The given chemical formula and other crystal data do not take into account these solvent molecules.

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

Directory of Open Access Journals (Sweden)

Tara Shahani

2010-01-01

Full Text Available In the title compound, C11H17N3O3, the pyrazole ring is approximately planar, with a maximum deviation of 0.005 (2 Å, and forms a dihedral angle of 5.69 (13° with the plane through the six atoms of the piperidine ring. In the crystal, pairs of intermolecular N—H...O hydrogen bonds form dimers with neighbouring molecules, generating R22(8 ring motifs. These dimers are further linked into two-dimensional arrays parallel to the bc plane by intermolecular N—H...O and C—H...O hydrogen bonds.

Hydrogen-bonded Three-Dimensional Networks Encapsulating One-dimensional Covalent Chains: [Cu(3-ampy)(H2O)4](SO4)·(H2O) (3-ampy = 3-Aminopyridine)

Institute of Scientific and Technical Information of China (English)

无

2007-01-01

A three-dimensional complex [Cu(3-ampy)(H2O)4](SO4)·(H2O) (3-ampy = 3-aminopyridine) has been synthesized. Crystallographic data: C5H16CuN2O9S, Mr = 343.80, triclinic, space group P, a = 7.675(2), b = 8.225(3), c = 10.845(3) (A), α= 86.996(4), β = 76.292(4),γ = 68.890(4)°, V = 620.0(3) (A)3, Z = 2, Dc = 1.841 g/cm3, F(000) = 354 and μ = 1.971 mm-1. The structure was refined to R = 0.0269 and wR = 0.0659 for 1838 observed reflections (I ＞ 2σ(Ⅰ)). The structure consists of [Cu(3-ampy)(H2O)4]2+ cations, SO42- anions and lattice water molecules. 3-Ampy acting as a bidentate bridging ligand generates a 1D covalent chain. A supramolecular 2D framework is formed through π-π stacking of pyridine rings. The lattice water molecules and SO42- anions are located between the adjacent 2D frameworks. The hydrogen bonding interactions from lattice water molecules and SO42- anions to coordinate water extend the 2D framework into a 3D network.

Synthesis, characterization and inhibitory activities of (4-N3[3,5-3H]Phe10)PKI(6-22)amide and its precursors: photoaffinity labeling peptides for the active site of cyclic AMP-dependent protein kinase.

Science.gov (United States)

Katz, B M; Lundquist, L J; Walsh, D A; Glass, D B

1989-06-01

PKI(6-22)amide is a 17 residue peptide corresponding to the active portion of the heat-stable inhibitor of cAMP-dependent protein kinase. The peptide is a potent (Ki = 1.6 nM), competitive inhibitor of the enzyme. The photoreactive peptide analog (4-azidophenylalanine10)PKI(6-22)amide was synthesized in both its non-radiolabeled and tritiated forms by chemical modification of precursor peptides that were prepared by stepwise solid-phase synthesis. (4-Amino[3,5-3H]phenylalanine10)PKI(6-22)amide, the precursor for the radiolabeled arylazide peptide, was obtained by catalytic reduction of the corresponding peptide containing the 3,5-diiodo-4-aminophenylalanine residue at position 10. The purified PKI peptides were analyzed by HPLC, amino acid analysis, and u.v. spectra. In the dark, (4-azidophenylalanine10)PKI(6-22)amide inhibited the catalytic subunit of cAMP-dependent protein kinase with a Ki value of 2.8 nM. The photoreactivity of the arylazide peptide was demonstrated by time-dependent u.v. spectral changes on exposure to light. Photolysis of the catalytic subunit (4-azido[3,5-3H]phenylalanine10)PKI(6-22)amide complex resulted in specific covalent labeling of the enzyme. The data indicate that this peptide is a useful photoaffinity labeling reagent for the active site of the protein kinase.

Rate constants for the reaction of CF3O radicals with hydrocarbons at 298 K

DEFF Research Database (Denmark)

Kelly, C.; Treacy, J.; Sidebottom, H.W.

1993-01-01

Rate constant ratios of the reactions of CF3O radicals with a number of hydrocarbons have been determined at 298 +/- 2 K and atmospheric pressure using a relative rate method. Using a previously determined value k(CF30 + C2H6) = 1.2 x 10(-12) cm3 molecule-1 s-1 these rate constant ratios provide...... estimates of the rate constants: k(CF3O + CH4) = (1.2 +/- 0.1) x 10(-14), k(CF3O + c-C3H6) = (3.6 +/- 0.2) x 10(-13), k(CF3O + C3H8) = (4.7 +/- 0.7) x 10(-12), k(CF3O + (CH3)3CH) = (7.2 +/- 0.5) x 10(-12), k(CF3O + C2H4) = (3.0 +/- 0.1) x 10(-11) and k(CF3O + C6H6) = (3.6 +/- 0.1) x 10(-11) cm3 molecule-1 s......-1. The importance of the reactions of CF3O radicals with hydrocarbons under atmospheric conditions is discussed....

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

Directory of Open Access Journals (Sweden)

Mohamed El Hafi

2018-02-01

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

N2,N2,N5,N5-Tetrakis(2-chloroethyl-3,4-dimethylthiophene-2,5-dicarboxamide

Directory of Open Access Journals (Sweden)

Yi-Dan Tang

2010-01-01

Full Text Available In the title compound, C16H22Cl4N2O2S, the two imide groups adopt a trans arrangement relative to the central thienyl ring, so the four terminal 2-chloroethyl arms adopt different orientations. In the crystal, molecules are linked by weak C—H...Cl and C—H...O hydrogen bonds into a three-dimensional network.

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

Directory of Open Access Journals (Sweden)

M. N. Ponnuswamy

2008-10-01

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

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

Directory of Open Access Journals (Sweden)

Yan-Lin Zhang

2011-10-01

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

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

International Nuclear Information System (INIS)

Sinyakova, G.S.

1979-01-01

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

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Myotonin protein-kinase [AGC]n trinucleotide repeat in seven nonhuman primates

Energy Technology Data Exchange (ETDEWEB)

Novelli, G.; Sineo, L.; Pontieri, E. [Catholic Univ. of Rome (Italy)]|[Univ. of Milan (Italy)]|[Univ. Florence (Italy)] [and others

1994-09-01

Myotonic dystrophy (DM) is due to a genomic instability of a trinucleotide [AGC]n motif, located at the 3{prime} UTR region of a protein-kinase gene (myotonin protein kinase, MT-PK). The [AGC] repeat is meiotically and mitotically unstable, and it is directly related to the manifestations of the disorder. Although a gene dosage effect of the MT-PK has been demonstrated n DM muscle, the mechanism(s) by which the intragenic repeat expansion leads to disease is largely unknown. This non-standard mutational event could reflect an evolutionary mechanism widespread among animal genomes. We have isolated and sequenced the complete 3{prime}UTR region of the MT-PK gene in seven primates (macaque, orangutan, gorilla, chimpanzee, gibbon, owl monkey, saimiri), and examined by comparative sequence nucleotide analysis the [AGC]n intragenic repeat and the surrounding nucleotides. The genomic organization, including the [AGC]n repeat structure, was conserved in all examined species, excluding the gibbon (Hylobates agilis), in which the [AGC]n upstream sequence (GGAA) is replaced by a GA dinucleotide. The number of [AGC]n in the examined species ranged between 7 (gorilla) and 13 repeats (owl monkeys), with a polymorphism informative content (PIC) similar to that observed in humans. These results indicate that the 3{prime}UTR [AGC] repeat within the MT-PK gene is evolutionarily conserved, supporting that this region has important regulatory functions.

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

Directory of Open Access Journals (Sweden)

Andrii I. Buvailo

2008-01-01

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

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

Directory of Open Access Journals (Sweden)

Kil Sik Min

2008-02-01

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

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

Directory of Open Access Journals (Sweden)

Ute Schmidt

2015-03-01

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

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

Directory of Open Access Journals (Sweden)

Shivanna Subhadramma

2015-08-01

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

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

Directory of Open Access Journals (Sweden)

Muhammad Nadeem Arshad

2008-03-01

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

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

Directory of Open Access Journals (Sweden)

Cevher Gündoğdu

2011-06-01

Full Text Available In the title compound, C15H15NO3, the carbazole skeleton includes an ethoxycarbonyl group at the 3-position. In the indole ring system, the benzene and pyrrole rings are nearly coplanar, forming a dihedral angle of 0.89 (4°. The cyclohexenone ring has an envelope conformation. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into a three dimensional network. A weak C—H...π interaction is also observed.

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

Directory of Open Access Journals (Sweden)

Lin Chen

2011-01-01

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

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

Directory of Open Access Journals (Sweden)

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.

Trifluoroethylation of Alkynes: Synthesis of Allylic-CF3 Compounds by Visible-Light Photocatalysis

Institute of Scientific and Technical Information of China (English)

Geum-bee Roh; Naeem Iqbal; Eun Jin Cho

2016-01-01

Two types of allylic trifluoromethylated compounds were synthesized by reacting alkynes with CF3CH2I using visible-light photocatalysis.Subtle differences in the catalytic system controlled the selectivity of iodotrifluoroethylation and hydrotrifluoroethylation.The iodotrifluoroethylated products were obtained in the presence of [Ru(bpy)3]C12 and TMEDA in CH3CN under visible-light irradiation,whereas hydrotrifluoroethylated products were synthesized usingfac-[Ir(ppy)3] and a mixture of DBU and K2CO3 in DMF.The iodotrifluoroethylation reaction worked particularly well,even at gram-scale,and the synthetic utility of iodotrifluoroethylated products was proved by their coupling reactions,providing complex CF3-containing products.

Electron and photon impact studies of CF3I

International Nuclear Information System (INIS)

Mason, N.J.; Eden, S.; Limao Vieire, P.; Kendall, P.; Pathak, S.; Dawes, A.; Tegeder, P.; Kitajima, M.; Okamoto, M.; Tanaka, H.; Samukawa, S.; Cho, H.; Hoffmann, S.

2002-01-01

The manufacture of ultra-large-scale-integrated circuits, requires a well collimated, specially uniform, high density plasma source operating under low pressure conditions. The main feed gases used are perfluorocarbons, however these are also strong greenhouse gases, therefore must be replaced by alternative compounds with low global warming potentials. CF 3 I is one possible replacement, due to its high photolysis rate, is expected to have a very short lifetime in the atmosphere. It is also predicted to be able to produced high yields of CF 3 radicals in any etching plasma, since its weak C - I bond should be possible to break by direct electron impact. Prior adapting existing industrial plasma reactors to use CF 3 I, it is necessary to run simulations of the reactant plasma, requiring a detailed database of the electron interactions with the feed gases, however such CF 3 I data does not exist. Thus an exhaustive series of experiments to measure elastic and inelastic scattering from CF 3 I including a study of its electronic state spectroscopy using photon absorption and electron scattering techniques were performed. Electron energy loss spectroscopy (EELS) and photo-absorption spectroscopy were employed. A comprehensive set of differential cross sections for the elastic scattering CF 3 I over the impact energy region from 1.5 to 60 eV for scattering angles between 20 and 130 were compiled. The photo-absorption spectrum is characterized by three regions, the first is a very weak continuum around centered about 4.7 eV; the second consists of four prominent band structures observed around 7.4, 8.1, 9.0 and 9.8 eV, respectively, containing vibrational structure from 7 to 10 eV; the third (above the ionization potentials) could only be studied by using EELS and additional broad peaks were observed. (nevyjel)

Insights into the degradation of (CF3)2CHOCH3 and its oxidative product (CF3)2CHOCHO & the formation and catalytic degradation of organic nitrates

Science.gov (United States)

Bai, Feng-Yang; Jia, Zi-Man; Pan, Xiu-Mei

2018-06-01

In this work, a systematic investigation of the atmospheric oxidation mechanism of (CF3)2CXOCH3 and their oxidative products (CF3)2CXOCHO (X = H, F) initiated by OH radical or Cl atom is performed by density functional theory. This study reveals that the introduction of NO and O2 promotes the formation of organic nitrates, which are hygroscopic and are inclined to form secondary organic aerosols (SOA) and can affect the air quality. The rate constants of the individual reactions are found to be in agreement with the experimental results. One of the intriguing findings of this work is that the peroxynitrite of (CF3)2CHOCH2OONO formed from the subsequent reactions of (CF3)2CHOCH3 is more favorable to isomerize to organic nitrate (CF3)2CHOCH2ONO2 than to dissociate into alkoxy radical (CF3)2CHOCH2O and NO2 because of the lower energy barrier of isomerization. The second significant observation is that the organic nitrate can be degraded more favorably with the presence of NH3, CH3NH2, and CH3NHCH3 than its naked decomposition reaction (CF3)2CHOCH2ONO2→(CF3)2CHOCHO + HONO. The ammonium salt, a vital part of haze, is harmful to human health and can be formed in the existence of the NH3, CH3NH2, and CH3NHCH3. In addition, the toxic substance of peroxyalkyl nitrate (CF3)2CHOC(O)ONO2 which can reduce the visibility of the atmosphere is produced as the primary subsequent oxidation product of (CF3)2CHOCHO in a NO-rich environment. The main species detected experimentally are confirmed by this study. The computational results are crucial to risk assessment and pollution prevention of the volatile organic compounds (VOCs).

Crystal structure of trans-(1,8-dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-κ4N3,N6,N10,N13bis(isonicotinato-κOcopper(II from synchrotron data

Directory of Open Access Journals (Sweden)

Jong Won Shin

2015-02-01

Full Text Available The title compound, [Cu(C6H4NO22(C16H38N6] has been synthesized and characterized by structure analysis based on synchrotron data and by FT–IR spectroscopy. The asymmetric unit consists of half of the CuII complex, the other half being completed by inversion symmetry. The CuII ion has a tetragonally distorted octahedral coordination sphere with four secondary N atoms of the azamacrocyclic ligand in the equatorial plane [Cu—Neq = 2.018 (12 Å] and two O atoms of the isonicotinate anions at the axial positions [Cu—Oax = 2.4100 (11 Å]. Intramolecular N—H...O hydrogen bonds between one of the secondary amine N—H groups of the azamacrocyclic ligand and the non-coordinating O atom of the isonicotinate ions stabilize the molecular structure. Intermolecular N—H...N hydrogen bonds between the other macrocyclic N—H group and the pyridine N atom of an adjacent isonicotinate anion as well as π–π interactions [centroid-to-centroid distance 3.711 (2 Å] lead to the formation of rods parallel to [001].

Atmospheric chemistry of (Z)-CF3CH═CHCF3: OH radical reaction rate coefficient and global warming potential.

Science.gov (United States)

Baasandorj, Munkhbayar; Ravishankara, A R; Burkholder, James B

2011-09-29

Rate coefficients, k, for the gas-phase reaction of the OH radical with (Z)-CF(3)CH═CHCF(3) (cis-1,1,1,4,4,4-hexafluoro-2-butene) were measured under pseudo-first-order conditions in OH using pulsed laser photolysis (PLP) to produce OH and laser-induced fluorescence (LIF) to detect it. Rate coefficients were measured over a range of temperatures (212-374 K) and bath gas pressures (20-200 Torr; He, N(2)) and found to be independent of pressure over this range of conditions. The rate coefficient has a non-Arrhenius behavior that is well-described by the expression k(1)(T) = (5.73 ± 0.60) × 10(-19) × T(2) × exp[(678 ± 10)/T] cm(3) molecule(-1) s(-1) where k(1)(296 K) was measured to be (4.91 ± 0.50) × 10(-13) cm(3) molecule(-1) s(-1) and the uncertainties are at the 2σ level and include estimated systematic errors. Rate coefficients for the analogous OD radical reaction were determined over a range of temperatures (262-374 K) at 100 Torr (He) to be k(2)(T) = (4.81 ± 0.20) × 10(-19) × T(2) × exp[(776 ± 15)/T], with k(2)(296 K) = (5.73 ± 0.50) × 10(-13) cm(3) molecule(-1) s(-1). OH radical rate coefficients were also measured at 296, 345, and 375 K using a relative rate technique and found to be in good agreement with the PLP-LIF results. A room-temperature rate coefficient for the O(3) + (Z)-CF(3)CH═CHCF(3) reaction was measured using an absolute method with O(3) in excess to be reaction was estimated to be ~20 days. Infrared absorption spectra of (Z)-CF(3)CH═CHCF(3) measured in this work were used to determine a (Z)-CF(3)CH═CHCF(3) global warming potential (GWP) of ~9 for the 100 year time horizon. A comparison of the OH reactivity of (Z)-CF(3)CH═CHCF(3) with other unsaturated fluorinated compounds is presented.

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

Directory of Open Access Journals (Sweden)

Vahid Amani

2010-10-01

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

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

Directory of Open Access Journals (Sweden)

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.

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

Directory of Open Access Journals (Sweden)

Yong-Sheng Yan

2012-03-01

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

ENDOR determination of the proton positions around Gd3+ in La(C2H5SO4)3.9H2O

International Nuclear Information System (INIS)

Beer, R. de; Biesboer, F.; Ormondt, D. van

1976-01-01

The water proton positions around Gd 3+ in La(C 2 H 5 SO 4 ) 3 .9H 2 O have been determined by means of ENDOR. The positions of the nearest neighbour water oxygens are discussed on the basis of a superposition model analysis of the ratios b 2 0 /A 2 0 2 >, b 6 6 /b 6 0 and mod(A 6 6 )modA 6 0 . (Auth.)

3-Chloro-2-ethyl-6-nitro-2H-indazole

Directory of Open Access Journals (Sweden)

Mohamed Mokhtar Mohamed Abdelahi

2017-05-01

Full Text Available In the title compound, C9H8ClN3O2, the orientation of the ethyl substituent is partly determined by an intramolecular C—H...Cl hydrogen bond. The indazole moiety is slightly folded with an angle of 0.70 (8° between the five- and six-membered rings. In the crystal, molecules pack in layers parallel to [100] through C—H...π(ring and N...;O...π(ring interactions.

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

Directory of Open Access Journals (Sweden)

Selma Bourichi

2016-05-01

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

Synthesis, X-ray Single Crystal Structure, Molecular Docking and DFT Computations on N-[(1E)-1-(2H-1,3-Benzodioxol-5-yl)-3-(1H-imidazol-1-yl)propylidene]-hydroxylamine: A New Potential Antifungal Agent Precursor.

Science.gov (United States)

Al-Wabli, Reem I; Al-Ghamdi, Alwah R; Ghabbour, Hazem A; Al-Agamy, Mohamed H; Monicka, James Clemy; Joe, Issac Hubert; Attia, Mohamed I

2017-02-28

Mycoses are serious health problem, especially in immunocompromised individuals. A new imidazole-bearing compound containing an oxime functionality was synthesized and characterized with different spectroscopic techniques to be used for the preparation of new antifungal agents. The stereochemistry of the oxime double bond was unequivocally determined via the single crystal X-ray technique. The title compound 4 , C 13 H 13 N₃O₃·C₃H₈O, crystallizes in the monoclinic space group P 2₁with a = 9.0963(3) Å, b = 14.7244(6) Å, c = 10.7035(4) Å, β = 94.298 (3)°, V = 1429.57(9) ų, Z = 2. The molecules were packed in the crystal structure by eight intermolecular hydrogen bond interactions. A comprehensive spectral analysis of the title molecule 4 has been performed based on the scaled quantum mechanical (SQM) force field obtained by density-functional theory (DFT) calculations. A molecular docking study illustrated the binding mode of the title compound 4 into its target protein. The preliminary antifungal activity of the title compound 4 was determined using a broth microdilution assay.

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

Directory of Open Access Journals (Sweden)

Hoong-Kun Fun

2011-01-01

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

Piezoelectric properties of nonstoichiometric Sr1-xBi2+2x/3Ta2O9 ceramics

International Nuclear Information System (INIS)

Jain, Rajni; Chauhan, Arun Kumar Singh; Gupta, Vinay; Sreenivas, K.

2005-01-01

The effect of poling on the structural, dielectric, and piezoelectric properties has been investigated for sol-gel-derived strontium bismuth tantalate (SBT) [Sr 1-x Bi 2+2x/3 Ta 2 O 9 ] ceramics with x=0.0,0.15,0.30,0.45. The dielectric and ferroelectric properties are found to improve with increase in x up to 0.3. Beyond x>0.3 the properties are found to degrade due to the limited solid solubility and the presence of a mixed phase of bismuth tantalate (BiTaO 4 ) is detected with x=0.45. Poling treatment reduces the dielectric dispersion and dielectric loss in the frequency range (0.1-100 kHz). The resonance and antiresonance frequencies increase with increase in x (x=0-0.30), and the corresponding minimum impedance decreases. The measured coupling coefficients (k p ) are small (0.0967-0.1) for x=0-0.30, and the electromechanical quality factor (Q m =915) is a maximum for the Sr 0.7 Bi 2.2 Ta 2 O 9 composition (x=0.30). The estimated piezoelectric charge coefficient (d 31 ) and piezoelectric voltage coefficient (g 31 ) are 5.2 pC/N and 5.8x10 -3 V m/N, respectively. The positive values of d 31 and g 31 and the low dielectric permittivity of SBT yield a high value for the hydrostatic coefficients, despite the low charge coefficient of d 33 =24 pC/N. The maximum values of charge coefficient (d h =34 pC/N) and voltage coefficient (g h =39x10 -3 V m/N) are obtained for Sr 0.7 Bi 2.2 Ta 2 O 9 composition, and the estimated hydrostatic figure of merit (d h g h x10 -15 =1215 m 2 /N) is high

Poly[bis(μ-hemihydrogen 2-phenylquinoline-4-carboxylato-κ2N,Osilver(I

Directory of Open Access Journals (Sweden)

Bin Li

2009-02-01

Full Text Available In the title compound, [Ag(C16H10.5NO22], the AgI cation (site symmetry 2 is coordinated by two N atoms in a near-linear AgN2 arrangement. Two carboxylate O atoms from two additional 2-phenylquinoline-4-carboxylate ligands form long Ag—O bonds [2.6585 (17 Å], resulting in a distorted square-planar arrangement. The bridging ligands result in infinite corrugated sheets propagating in (010. An O—H...O hydrogen bond, disordered about a twofold axis, completes the structure.

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

Directory of Open Access Journals (Sweden)

Irina A. Golenya

2012-10-01

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

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

Directory of Open Access Journals (Sweden)

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.

catena-Poly[[bis(μ-3-carboxybenzoatobis(1,10-phenanthrolinetricopper(II]-di-μ3-isophthalato

Directory of Open Access Journals (Sweden)

Yan-Sheng Yin

2008-12-01

Full Text Available The title copper coordination polymer, [Cu3(C8H4O42(C8H5O42(C10H8N22]n, was synthesized by reacting Cu(NO32, isophthalic acid and 1,10-phenanthroline under hydrothermal conditions. The trinuclear unit presents a central almost planar CuO4 chromophore with the cation on a symmetry center, and two symmetry-related CuN2O3 groups with the metal centre in a distorted square-pyramidal environment. These units are bridged by isophthalate ligands into one-dimensional double-chain coordination polymers which are, in turn, connected by various π–π stacking interactions (face-to-face distance ca 3.45 Å and O—H...O hydrogen bonds, forming a three-dimensional supramolecular network.

Crystal and molecular structure of 6,9-bis(trimethylamine)-nido-decarborane(12) B10H12[N(CH3)3]2

International Nuclear Information System (INIS)

Polyanskaya, T.M.; Volkov, V.V.

1989-01-01

The spatial structure of 6.9-bis(trimethylamine)-nido-decarborane (12) is established on the basis of X-ray diffraction analysis. Crystals are rhombic, a = 12.619, b = 11.804, c = 11.058A, Z=4, sp. gr. P na 2 1 . The structure is of molecular type. Main geometrical parameters of the molecule are: symmetry - C1, interatomic distances - B-B 1.66-1.90, B-N 1.61, N-C 1.50 A, angles - BBB 55.0-66.5, CNC 108, BBN 119.5 deg. The (B 10 H 12 ) cluster size between B(6) and B(9) is 3.30 A. Increase approximately by 0.1 A of lengths of external bonds B-B in comparison with internal ones and tightening approximately by 3 deg of valent angles BBB at external atoms of boron also in comparison with internal ones are observed

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

Directory of Open Access Journals (Sweden)

Mohammed El Fal

2014-09-01

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

N-(5-Benzylsulfanyl-1,3,4-thiadiazol-2-yl-2-(piperidin-1-ylacetamide

Directory of Open Access Journals (Sweden)

D. S. Ismailova

2014-03-01

Full Text Available The title compound, C16H20N4OS2, was synthesized by the reaction of 2-benzylsulfanyl-5-chloroacetamido-1,3,4-thiadiazole and piperidine in a 1:2 ratio. The planes of the acetamide and 1,3,4-thiadiazole units are twisted by 10.8 (4°. The thiadiazole S atom and the acetamide O atom are syn-oriented due to a hypervalent S...O interaction of 2.628 (4 Å. In the crystal, molecules form centrosymmetric dimers via N—H...N hydrogen bonds. These dimers are further connected by C—H...O interactions into (100 layers.

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

Directory of Open Access Journals (Sweden)

Terrill D. Smith

2010-01-01

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

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

Directory of Open Access Journals (Sweden)

Tadeusz Lis

2008-03-01

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

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

International Nuclear Information System (INIS)

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

1991-01-01

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

Synthesis, structure, terahertz spectroscopy and luminescent properties of copper (I) complexes with bis(diphenylphosphino)methane and N-donor ligands

Science.gov (United States)

Fan, Wei-Wei; Li, Zhong-Feng; Li, Jiao-Bao; Yang, Yu-Ping; Yuan, Yuan; Tang, Han-Qin; Gao, Ling-Xiao; Jin, Qiong-Hua; Zhang, Zhen-Wei; Zhang, Cun-Lin

2015-11-01

The reactions of copper(I) salts CuX [X = Cl, OTf (OTf = CF3SO3) and ClO4] and bis(diphenylphosphino)methane (dppm) with 4,4-bipyridine (4,4-bipy), 2,2-bipyridine (2,2-bipy), isoquinoline (i-C9H7N) and 1,10-phenanthroline (phen) lead to five new copper(I) complexes: [CuCl(dppm)(i-C9H7N)]2 (1), {[CuCl(dppm)(phen)]2•5H2O}n (2), [Cu2Cl2(dppm)2(4,4-bipy)]•4CH3CN (3), [Cu(dppm)(2,2-bipy)]2(OTf)2 (4), {[Cu2Cl(dppm)2(4,4-bipy)](ClO4)}n (5). Complexes 1, 3 and 4 are of dinuclear structure with eight-membered Cu2P4C2 rings. The structure of compound 2 can be simplified as three-dimensional topology. Complex 5 is of infinite chain structure linked by 4,4-bipy. All these complexes are characterized by IR, elemental analyses, single-crystal X-ray diffraction analysis, luminescence, NMR and terahertz time-domain spectroscopy.

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

Directory of Open Access Journals (Sweden)

Gary S. Nichol

2011-12-01

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

Detection of transient infrared absorption of SO3 and 1,3,2-dioxathietane-2,2-dioxide [cyc-(CH2)O(SO2)O] in the reaction CH2OO+SO2

Science.gov (United States)

Wang, Yi-Ying; Dash, Manas Ranjan; Chung, Chao-Yu; Lee, Yuan-Pern

2018-02-01

We recorded time-resolved infrared absorption spectra of transient species produced on irradiation at 308 nm of a flowing mixture of CH2I2/O2/N2/SO2 at 298 K. Bands of CH2OO were observed initially upon irradiation; their decrease in intensity was accompanied by the appearance of an intense band at 1391.5 cm-1 that is associated with the degenerate SO-stretching mode of SO3, two major bands of HCHO at 1502 and 1745 cm-1, and five new bands near >1340, 1225, 1100, 940, and 880 cm-1. The band near 1340 cm-1 was interfered by absorption of SO2 and SO3, so its band maximum might be greater than 1340 cm-1. SO3 in its internally excited states was produced initially and became thermalized at a later period. The rotational contour of the band of thermalized SO3 agrees satisfactorily with the reported spectrum of SO3. These five new bands are tentatively assigned to an intermediate 1,3,2-dioxathietane-2,2-dioxide [cyc-(CH2)O(SO2)O] according to comparison with anharmonic vibrational wavenumbers and relative IR intensities predicted for this intermediate. Observation of a small amount of cyc-(CH2)O(SO2)O is consistent with the expected reaction according to the potential energy scheme predicted previously. SO3+HCHO are the major products of the title reaction. The other predicted product channel HCOOH+SO2 was unobserved and its branching ratio was estimated to be <5%.

Bis[N,N-bis(1-allyl-1H-benzimidazol-2-ylmethyl-κN3benzylamine-κN]cadmium dipicrate

Directory of Open Access Journals (Sweden)

Jing-Kun Yuan

2011-06-01

Full Text Available The crystal structure of the title compound, [Cd(C29H29N52](C6H2N3O72, consists of CdII complex cations and picrate anions. In the complex cation, the CdII ion is chelated by two bis(1-allylbenzimidazol-2-ylmethylbenzylamine (babb ligands in a distorted octahedral geometry. Extensive C—H...O hydrogen bonding occurs between cations and anions in the crystal structure.

(E-N-(3,3-Diphenylallylidene-3-nitroaniline

Directory of Open Access Journals (Sweden)

Joo Hwan Cha

2012-10-01

Full Text Available In the title compound, C21H16N2O2, the 3-nitrophenyl and two phenyl rings are twisted from the mean plane of the enimino fragment by 44.4 (1, 37.2 (1 and 74.1 (1°, respectively. The crystal packing exhibits no classical intermolecular contacts.

Atmospheric chemistry of C₄F₉O(CH₂)₃OC₄F₉ and CF₃CFHCF₂O (CH₂)₃OCF₃CFHCF₂

DEFF Research Database (Denmark)

Toft, A. M.; Hurley, M. D.; Wallington, T. J.

2006-01-01

FTIR smog chamber techniques were used to measure k(Cl + CF3CFHCF2O(CH2)(3)OCF2CFHCF3) = (2.97 +/- 0.17) x 10(-12) k(OH + CF3CFHCF2O(CH2)(3)OCF2CFHCF3) = (2.45 +/- 0.14) x 10(-13), k(Cl + C4F9O(CH2)(3)OC4F9) = (1.45 +/- 0.16) x 10(-12), and k(OH + C4F9O(CH2)(3)OC4F9) = (1.44 +/- 0.10) x 10(-13) c...

Crystal structure of an unknown tetrahydrofuran solvate of tetrakis(μ3-cyanato-κ3N:N:Ntetrakis[(triphenylphosphane-κPsilver(I

Directory of Open Access Journals (Sweden)

Peter Frenzel

2015-10-01

Full Text Available In the title compound, [{[(C6H53P]Ag}4{NCO}4], a distorted Ag4N4-heterocubane core is set up by four AgI ions being coordinated by the N atoms of the cyanato anions in a μ3-bridging mode. In addition, a triphenylphosphine ligand is datively bonded to each of the AgI ions. Intramolecular Ag...Ag distances as short as 3.133 (9 Å suggest the presence of argentophilic (d10...d10 interactions. Five moderate-to-weak C—H...O hydrogen-bonding interactions are observed in the crystal structure, spanning a three-dimensional network. A region of electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as being part of disordered tetrahydrofuran solvent molecules. The given chemical formula and other crystal data do not take into account these solvent molecules.

Bis[μ-3-(1H-benzimidazol-2-ylbenzoato]dicopper(I

Directory of Open Access Journals (Sweden)

Zheng-Yu Su

2010-12-01

Full Text Available The dimeric title complex, [Cu2(C14H9N2O22], resides on a center of symmetry. In the crystal, the molecules are packed via π–π stacking interactions alternating between imidazole and benzene rings [mean interplanar distances = 3.754 (3 and 3.624 (3 Å]. An intermolecular N—H...O hydrogen bond links the dimers together. The two-coordinate CuI atom displays an O—Cu—N bond angle of 176.3 (2°. The Cu...Cu distance within the dimer is 5.100 (2 Å.

Identification and analytical characterization of six synthetic cannabinoids NNL-3, 5F-NPB-22-7N, 5F-AKB-48-7N, 5F-EDMB-PINACA, EMB-FUBINACA, and EG-018.

Science.gov (United States)

Liu, Cuimei; Jia, Wei; Hua, Zhendong; Qian, Zhenhua

2017-08-01

Clinical and forensic toxicology laboratories are continuously confronted by analytical challenges when dealing with the new psychoactive substances phenomenon. The number of synthetic cannabinoids, the chemical diversity, and the speed of emergence make this group of compounds particularly challenging in terms of detection, monitoring, and responding. Three indazole 7N positional isomer synthetic cannabinoids, two ethyl 2-amino-3-methylbutanoate-type synthetic cannabinoids, and one 9H-carbazole substituted synthetic cannabinoid were identified in seized materials. These six synthetic cannabinoid derivatives included: 1H-benzo[d] [1,2,3]triazol-1-yl 1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate (NNL-3, 1), quinolin-8-yl 1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate (5F-NPB-22-7N, 2), N-((1 s,3 s)-adamantan-1-yl)-1-(5-fluoropentyl)-1H-pyrrolo[2,3-b]pyridine-3-carboxamide (5F-AKB-48-7N, 3), ethyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate (5F-EDMB-PINACA, 4), ethyl 2-(1-(4-fluorobenzyl)-1H-indazole-3-carboxamido)-3-methylbutanoate (EMB-FUBINACA, 5), and naphthalen-1-yl(9-pentyl-9H-carbazol-3-yl)methanone (EG-018, 6). The identification was based on ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry (UHPLC-QTOF-MS), gas chromatography-mass spectrometry (GC-MS), and nuclear magnetic resonance spectroscopy (NMR). The analytical characterization of these six synthetic cannabinoids was described, so as to assist forensic laboratories in identifying these compounds or other substances with similar structure in their case work. To our knowledge, no analytical data about the compounds 1-5 have appeared until now, making this the first report on these compounds. The GC-MS data of 6 has been reported, but this study added the LC-MS, NMR, and Fourier transform infrared (FTIR), data to render the analytical data collection process more complete. Copyright © 2017 John Wiley & Sons, Ltd

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

Science.gov (United States)

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

2016-03-21

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

Poly[bis[μ4-N-(2-hydroxyiminopropionyl-N′-(2-oxidoiminopropionylpropane-1,3-diaminato]dimethanolcalciumdicopper(II

Directory of Open Access Journals (Sweden)

Valentina A. Kalibabchuk

2009-09-01

Full Text Available In the title compound, [CaCu2(C9H13N4O42(CH3OH2]n, the CaII atom lies on an inversion center and is situated in a moderately distorted octahedral environment. The CuII atom is in a distorted square-pyramidal geometry, defined by four N atoms belonging to the amide and oxime groups of the triply deprotonated residue of N,N′-bis(2-hydroxyiminopropanoylpropane-1,3-diamine (H4pap and one oxime O atom from a neighboring Hpap ligand at the apical site, forming a dimeric [Cu2(Hpap2]2− unit. Each dimeric unit connects four Ca atoms and each Ca atom links four [Cu2(Hpap2]2− units through Ca—O(amide bonds, leading to a three-dimensional framework. The crystal structure involves intra- and intermolecular O—H...O hydrogen bonds.

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

Directory of Open Access Journals (Sweden)

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.

(Z-N-[3-(4-Bromobenzoyl-1,3-thiazolidin-2-ylidene]cyanamide

Directory of Open Access Journals (Sweden)

Ling Xu

2010-12-01

Full Text Available In the title compound, C11H8BrN3OS, the dihedral angle between the benzene and thiazolidine rings is 63.4 (2°. Intermolecular C—H...N interactions help to stabilize the crystal structure.

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

Directory of Open Access Journals (Sweden)

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.

Chlorination-promoted skeletal transformation of IPR C76 discovered via trifluoromethylation under the formation of non-IPR C76(CF3)nFm.

Science.gov (United States)

Tamm, Nadezhda B; Brotsman, Victor A; Markov, Vitaliy Yu; Kemnitz, Erhard; Troyanov, Sergey I

2018-05-22

High-temperature chlorination of an Isolated-Pentagon Rule (IPR) D2-C76 fullerene followed by high-temperature trifluoromethylation of non-IPR C76 chlorides with CF3I unexpectedly resulted in a series of non-IPR C76(CF3)nFm compounds. X-ray diffraction study with the use of synchrotron radiation revealed the mixed CF3/F structures of non-classical, non-IPR C76(CF3)14, C76(CF3)14F2, and C76(CF3)16F6.

Crystal and electronic structure of (N-CH3-2,2'-bipyridinium)(dodecahydro-dicarba-nido-undecaborate)

International Nuclear Information System (INIS)

Il'inchik, E.A.; Polyanskaya, T.M.; Volkov, V.V.

2007-01-01

The compound (N-CH 3 -2,2'-bipyridinium)(dodecahydro-dicarba-nido-undecaborate) is synthesized, and its structure is determined. The compound is characterized by IR, 11 B, 14 N NMR and X-ray photoelectron spectroscopy methods. Crystallographic data are: C 13 H 23 B 9 N 2 , M=304.62, monoclinic lattice, space group P2 1 /c, a=11.840(4), b=10.051(3), c=15.573(6) A, β=102.43(3) Deg, V=1809.8(10) A 3 , Z=4, d cal =1.118 g/cm 3 , R=0.0607 [ru

Synthesis of 3H-3-azido-salicyl-N-(n-decyl) amide

International Nuclear Information System (INIS)

Lu Bin; Xu Jianxing; Chen Shizhi

2000-01-01

A novel method for the synthesis of molecular probe of ubiquinone-binding protein is described. With 3-nitrosalicylic acid and decylamine as initial compounds and under the existence of DCC, the 3-nitro-salicyl-N-(n-decyl)amide is synthesized at room temperature. Then, 3-nitro-salicyl-N-(n-decyl)amide is reduced by hydrogen with 5 % Pd/C as catalyst to form 3-amino-salicyl-N-(n-decyl)amide which is exchanged with tritium to be 3 H-3-amino-salicyl-N-(n-decyl)amide. At the temperature below 5 degree C, 3 H-3-amino-salicyl-N-(n-decyl)amide reacts with NaNO 2 and HCl, and the 3-diazo-salicyl-N-(n-decyl)amide is formed in an ice salt bath. As soon as the reaction is completed, NaN 3 is added to the mixture and stirred for 3 h at the temperature between 0 - 5 degree C and in the dark, the molecular probe of studying ubiquinone-binding protein, i. e., 3 H-3-azido-salicyl-N-(n-decyl)amide is produced

The Cs2SO4-Ce2(SO4)3-H2SO4-H2O system at 150 and 200 deg C

International Nuclear Information System (INIS)

Bondar', S.A.; Belokoskov, V.I.; Trofimov, G.V.

1982-01-01

Solubility in the system Cs 2 SO 4 -Ce 2 (SO 4 ) 3 -H 2 SO 4 -H 2 O using the isothermal method at 150 and 200 deg C at molar ratios Cs 2 SO 4 :Ce 2 (SO 4 ) 3 =1:5 and conditions of sulfate crystallization Cs 2 SO 4 xCe 2 (SO 4 ) 3 , Ce 2 (SO 4 ) 3 x0.5H 2 SO 4 xnH 2 O (n=2-3) and Ce 2 (SO 4 ) 3 x3H 2 SO 4 are determined. Double sulfate Cs 2 SO 4 xCe 2 (SO 4 ) 3 is studied using the methods of crystallooptical, thermal, X-ray phase analyses and IR spectroscopy

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

Directory of Open Access Journals (Sweden)

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.

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

Science.gov (United States)

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

2018-01-01

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

Atmospheric chemistry of 4 : 2 fluorotelomer alcohol (CF3(CF2)(3)CH2CH2OH): Products and mechanism of Cl atom initiated oxidation

DEFF Research Database (Denmark)

Hurley, MD; Ball, JC; Wallington, TJ

2004-01-01

Smog chamber/FTIR techniques were used to study the products and mechanism of the Cl atom initiated oxidation of 4:2 fluorotelomer alcohol (CF3(CF2)(3)CH2CH2OH) in 700 Torr of N-2/O-2 diluent at 296 K. CF3(CF2)(3)CH2CHO is the sole primary oxidation product. CF3(CF2)(3)CHO, CF3(CF2)(3)CH2COOH...... respectively. Using relative rate techniques, a value of k(Cl + CF3(CF2)(3)CH2CHO) = (1.84 +/- 0.30) x 10(-11) cm(3) molecule(-1) s(-1) was determined. The yield of the perfluorinated acid, CF3(CF2)(3)COOH, from the 4:2 fluorotelomer alcohol increased with the diluent gas oxygen concentration......, and CF3(CF2)(3)CH2C(O)OOH are secondary oxidation products. Further irradiation results in the formation of CF3(CF2)(3)COOH, COF2, and CF3OH. CF3(CF2)(3)CHO, CF3(CF2)(3)CH2COOH, and CF3(CF2)(3)CH2C(O)OOH are formed from CF3(CF2)(3)CH2CHO oxidation in yields of 46 27 and less than or equal to 27...

Crystal structure of 4,6-diamino-2,2-dimethyl-3-[3-(2,4,5-trichlorophenoxypropoxy]-2,3-dihydro-1,3,5-triazin-1-ium chloride methanol monosolvate

Directory of Open Access Journals (Sweden)

Pattarapol Khongsuk

2015-08-01

Full Text Available In the title methanol-solvated salt, C14H19Cl3N5O2+·Cl−·CH3OH, the triazine molecule is protonated at one of the triazine N atoms. In the crystal, the triazine cations are linked through a pair of N—H...N hydrogen bonds, with graph-set R22(8, forming an inversion dimer. The protonated N atom and the 2- and 4-amino groups of the triazine cation interact with the chloride anion through N—H...Cl hydrogen bonds, leading to the formation of a tape structure running along the b-axis direction. A short Cl...Cl contact [3.2937 (9 Å] is observed in the tape. The methanol molecule is linked to the chloride anion and the triazine cation, respectively, by an O—H...Cl hydrogen bond and a C—H...O interaction.

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....

Potassium (2,2'-bipyridine-κN,N')bis-(carbonato-κO,O')cobaltate(III) dihydrate.

Science.gov (United States)

Wang, Jian-Fei; Lin, Jian-Li

2010-09-30

In the title compound, K[Co(CO(3))(2)(C(10)H(8)N(2))]·2H(2)O, the Co(III) atom is coordinated by two bipyridine N atoms and four O atoms from two bidentate chelating carbonate anions, and thus adopts a distorted octa-hedral N(2)O(4) environment. The [Co(bipy)(CO(3))(2)](-) (bipy is 2,2'-bipyridine) -units are stacked along [100] via π-π stacking inter-actions, with inter-planar distances between the bipyridine rings of 3.36 (4) and 3.44 (6) Å, forming chains. Classical O-H⋯O hydrogen-bonding inter-actions link the chains, forming channels along (100) in which the K(+) ions reside and leading to a three-dimensional supra-molecular architecture.

Crystal structure of catena-poly[silver(I-μ-l-tyrosinato-κ2O:N

Directory of Open Access Journals (Sweden)

Aqsa Yousaf

2015-03-01

Full Text Available The title compound, [Ag(C9H10NO3]n, is a polymeric silver(I complex of l-tyrosine. The AgI atom is connected to N and O atoms of two different l-tyrosine ligands in an almost linear arrangement, with an Ni—Ag—O1 bond angle of 173.4 (2° [symmetry code: (i x + 1, y, z]. The Ag—Ni and Ag—O bond lengths are 2.156 (5 and 2.162 (4 Å, respectively. The polymeric chains extend along the crystallographic a axis. Strong hydrogen bonds of the N—H...O and O—H...O types and additional C—H...O interactions connect these chains into a double-layer polymeric network in the ab plane.

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

Directory of Open Access Journals (Sweden)

Jiang-Sheng Li

2009-08-01

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

Synthesis and characterization of technetium(III) complexes containing 2,2'-bipyridine and 1,10-phenanthroline. X-ray crystal structures of cis (Cl),trans(P)-[TcCl2(P(CH3)2C6H5)2(bpy)]B(C6H5)4, cis (Cl),trans(P)-[TcCl2(P(CH3)2C6H5)2(phen)]B(C6H5)4, and cis (Cl),trans(P)-[TcCl2(P(CH3CH2)(C6H5)2)2(bpy)]SO3CF3

International Nuclear Information System (INIS)

Wilcox, B.E.; Ho, D.M.; Deutsch, E.

1989-01-01

Technetium(III) complexes of the general formula cis(Cl),trans(P)-[TcCl 2 (P) 2 L] + , where (P) is dimethylphenylphosphine (PMe 2 Ph) or ethyldiphenylphosphine (PEtPh 2 ) and L is 2,2'-bipyridine (bpy), 4,4'-dimethyl-2,2'-bipyridine (Me 2 bpy), or 1,10-phenanthroline (phen), have been synthesized and characterized. They are prepared by L substitution onto, with concomitant displacement of one chloride and one phosphine ligand from, the mer-TcCl 3 (P) 3 starting material in refluxing ethanol. Analysis of these complexes by fast atom bombardment mass spectrometry (in the positive ion mode) provides fingerprint mass spectra that exhibit peaks assigned to the molecular ion M + as well as peaks assigned to M + minus one or more monodentate ligands. Results of single-crystal x-ray structure determinations of cis(Cl),trans(P)-[TcCl 2 (PMe 2 Ph) 2 (bpy)]BPh 4 (A), cis(Cl),trans(P)-[TcCl 2- (PMe 2 Ph) 2 (phen)]BPh 4 (B), and cis(Cl),trans(P)-[TcCl 2 (PEtPh 2 ) 2 (bpy)]SO 3 CF 3 (C), with formula weights of 921.62, 945.64, and 903.65, respectively are reported. 26 refs., 5 figs., 5 tabs

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

Directory of Open Access Journals (Sweden)

Chin Wei Ooi

2012-08-01

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

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

Directory of Open Access Journals (Sweden)

R. Vishnupriya

2014-10-01

Full Text Available In the title compound, C27H19N3O, the dihedral angles between the plane of the pyridine ring and those of the indole (r.m.s. deviation = 0.018 Å, phenyl and methoxybenzene substituents are 33.60 (6, 25.28 (7 and 49.31 (7°, respectively. The N atom of the carbonitrile group is significantly displaced [0.288 (2 Å] from the plane of the pyridine ring, perhaps due to steric crowding. In the crystal, inversion dimers linked by pairs of N—H...Nn (n = nitrile hydrogen bonds generate R22(16 loops. Aromatic π–π stacking [centroid–centroid separation = 3.6906 (7 Å] and very weak C—H...π interactions are also observed".

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

Directory of Open Access Journals (Sweden)

Raju Suresh Kumar

2010-08-01

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

3-Chloro-N-(4-sulfamoylphenylpropanamide

Directory of Open Access Journals (Sweden)

Mehmet Akkurt

2010-07-01

Full Text Available In the title compound, C9H11ClN2O3S, the dihedral angle between the benzene ring and the amido –NHCO– plane is 15.0 (2°. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, the amino NH2 group is involved in intermolecular N—H...O hydrogen bonds, which connect the molecules into a double layer structure expanding parallel to the bc plane. The layers are further linked by an amido N—H...O hydrogen bond. Between the layers, a weak π–π interaction with a centroid–centroid distance of 3.7447 (12 Å is also observed.

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

Directory of Open Access Journals (Sweden)

Jia Hao Goh

2010-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-09-15

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

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

Directory of Open Access Journals (Sweden)

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.

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

Directory of Open Access Journals (Sweden)

Abdullah M. Asiri

2009-10-01

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

H2SO4-HNO3-H2O ternary system in the stratosphere

Science.gov (United States)

Kiang, C. S.; Hamill, P.

1974-01-01

Estimation of the equilibrium vapor pressure over the ternary system H2SO4-HNO3-H2O to study the possibility of stratospheric aerosol formation involving HNO3. It is shown that the vapor pressures for the ternary system H2SO4-HNO3-H2O with weight composition around 70-80% H2SO4, 10-20% HNO3, 10-20% H2O at -50 C are below the order of 10 to the minus 8th mm Hg. It is concluded that there exists more than sufficient nitric acid and water vapor in the stratosphere to participate in ternary system aerosol formation at -50 C. Therefore, HNO3 should be present in stratospheric aerosols, provided that H2SO4 is also present.

Addition compounds of lanthanide-and yttrium trifluoromethanesulfonates and N,N-dimethylacetamide (DMA)

International Nuclear Information System (INIS)

Vicentini, G.; Tamura, T.

1982-01-01

Preparation of addition compounds of hydrated lanthanide trifluoromethanesulfonates and DMA, with general formula Ln (CF 3 SO 3 ) 3 .6H 2 O.x DMA is described. The compounds obtained are characterized by elemental analysis, X-ray diagrams, infrared absorption spectra, electrolytical conductance in nitromethane and acetonitrile, absorption spectra of the neodymium compound and emission spectra of the europium compound. (A.R.H.) [pt

Tetrakis(6-methyl-2,2′-bipyridine-1κ2N,N′;2κ2N,N′;3κ2N,N′;4κ2N,N′-tetra-μ-nitrato-1:2κ2O:O′;2:3κ3O:O′,O′′;2:3κ3O,O′:O′′;3:4κ2O:O′-tetranitrato-1κ4O,O′;4κ2O,O′-tetralead(II

Directory of Open Access Journals (Sweden)

Roya Ahmadi

2009-10-01

Full Text Available In the tetranuclear centrosymmetric title compound, [Pb4(NO38(C11H10N24], irregular PbN2O5 and PbN2O4 coordination polyhedra occur. The heptacoordinated lead(II ion is bonded to two bidentate and one monodentate nitrate ion and one bidentate 6-methyl-2,2′-bipyridine (mbpy ligand. The six-coordinate lead(II ion is bonded to one bidentate and two monodentate nitrate anions and one mbpy ligand. In the crystal, bridging nitrate anions lead to infinite chains propagating in [111]. A number of C—H...O hydrogen bonds may stabilize the structure.

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

Directory of Open Access Journals (Sweden)

Augusto Rivera

2011-11-01

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

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

Directory of Open Access Journals (Sweden)

Jamshid Mengnorovich Ashurov

2016-04-01

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

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

Directory of Open Access Journals (Sweden)

Konan René Kambo

2017-05-01

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

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

Directory of Open Access Journals (Sweden)

Ulrich S. Schubert

2009-05-01

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

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

Directory of Open Access Journals (Sweden)

Tara Shahani

2010-07-01

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

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

Directory of Open Access Journals (Sweden)

Yordanka Ivanova

2016-04-01

Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone, was synthesized by Claisen-Schmidt condensation of 3-methyl-2(3H-benzothiazolone-6-carbaldehyde with 2-acetylthiophene in 94% yield. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

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

Directory of Open Access Journals (Sweden)

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.

A convenient preparation of 9 H -carbazole-3,6-dicarbonitrile and 9 H -carbazole-3,6-dicarboxylic acid

KAUST Repository

Weselinski, Lukasz Jan

2014-01-23

A catalytic, high yielding and scalable procedure for the synthesis of 9H-carbazole-3,6-dicarbonitrile has been developed. Subsequent hydrolysis of the dinitrile in the presence of a catalytic copper species (i.e., CuI) yields 9H-carbazole-3,6-dicarboxylic acid. Both compounds are versatile and fine-tunable organic building blocks and therefore offer potential in material science, medicinal and supramolecular chemistry. © Georg Thieme Verlag Stuttgart New York.

3-(Pyridin-2-ylcoumarin

Directory of Open Access Journals (Sweden)

Yu-Xia Da

2010-11-01

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

Ionic conduction studies in Li3+ ion irradiated P(VDF-HFP)-(PC + DEC)-LiCF3SO3 gel polymer electrolyte

International Nuclear Information System (INIS)

Saikia, D.; Hussain, A.M.P.; Kumar, A.; Singh, F.; Avasthi, D.K.

2006-01-01

In an attempt to increase the Li ion diffusivity in gel polymer electrolytes, the effects of Li 3+ ion irradiation in P(VDF-HFP)-(PC + DEC)-LiCF 3 SO 3 electrolyte system, with five different fluences, is studied. Irradiation with swift heavy ions shows enhancement in conductivity at low fluences and decreased in conductivity at higher fluences with respect to pristine polymer electrolyte films. Maximum room temperature ionic conductivity after irradiation is found to be 2.6 x 10 -3 S/cm. This interesting result could be attributed to the fact that, higher fluence provides critical activation energy for cross-linking and crystallization to occur, which results in decrease in ionic conductivity. XRD results show decrease in the degree of crystallinity upon ion irradiation at low fluences (≤10 11 ions/cm 2 ) and increase in crystallinity at high fluences (>10 11 ions/cm 2 ). In FTIR spectra the absorption band intensities around 3025 cm -1 and 2985 cm -1 decrease upon irradiation with a fluence of 5 x 10 1 ions/cm 2 suggesting chain scission and increase upon irradiation with a fluence of 5 x 10 12 ions/cm 2 indicating cross-linking. FTIR analyses corroborate the conductivity and XRD results

(4′-Phenyl-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′bis(thiocyanato-κNzinc(II unknown solvate

Directory of Open Access Journals (Sweden)

An-ran Wang

2016-11-01

Full Text Available The title compound, [Zn(NCS2(C21H15N3], crystallizes with three independent complex molecules in the asymmetric unit. In each complex molecule, the ZnII atom is coordinated by three N atoms of a 4′-phenyl-2,2′:6′,2′′-terpyridine ligand, and by the N atoms of two NCS− anions. The ZnII atoms are therefore five-coordinate, ZnN5, with distorted square-pyramidal geometries. In the crystal, the three independent molecules are linked by a series of offset π–π interactions [intercentroid distances vary between 3.680 (5 and 3.791 (5 Å], forming columns along the a-axis direction. The columns are linked via C—H...S interactions, forming a fence-like arrangement parallel to the ab plane. A small region of disordered electron density was corrected for using the SQUEEZE routine in PLATON [Spek (2015. Acta Cryst. C71, 9–18], but the formula mass and unit-cell characteristics were not taken into account during the refinement.

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

Directory of Open Access Journals (Sweden)

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.

1-(3-Bromo-6-nitro-1H-indazol-1-ylethan-1-one

Directory of Open Access Journals (Sweden)

Mohamed Mokhtar Mohamed Abdelahi

2017-05-01

Full Text Available The asymmetric unit of the title compound, C9H6BrN3O3, consists of two independent molecules differing in the rotational orientations of the nitro and acetyl substituents. In the crystal, head-to-head π-stacking between pairs of adjacent molecules forms dimers which are associated into stacks by C—Br...π(ring interactions. C—H...O hydrogen bonds tie the stacks together.

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

Directory of Open Access Journals (Sweden)

Joseph Nirmala

2009-08-01

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

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.

Crystal structure of meso-di-μ-chlorido-bis[bis(2,2′-bipyridinecadmium] bis(1,1,3,3-tetracyano-2-ethoxypropenide 0.81-hydrate

Directory of Open Access Journals (Sweden)

Fatima Setifi

2017-01-01

Full Text Available The hydrated title salt, [Cd2Cl2(C10H8N24](C9H5N4O2·0.81H2O, was obtained from the hydrothermal reaction between 2,2′-bipyridine, cadmium(II chloride and potassium 1,1,3,3-tetracyano-2-ethoxypropenide. The binuclear cation lies across a centre of inversion in the space group P21/c, with the other components in general positions. The cation has approximate, but non-crystallographic 2/m symmetry and each of the CdII atoms is a stereogenic centre, one having the Δ configuration and the other the Λ configuration. In the anion, one of the C(CN2 units is disordered over two sets of atomic sites having occupancies 0.75 (2 and 0.25 (2. The cations are linked by two independent C—H...Cl hydrogen bonds to form a sheet of R22(14 and R42(24 rings.

Rate Coefficient Measurements and Theoretical Analysis of the OH + ( E) CF3CH=CHCF3 Reaction.

Science.gov (United States)

Baasandorj, Munkhbayar; Marshall, Paul; Waterland, Robert L; Ravishankara, Akkihebbal R; Burkholder, James B

2018-04-25

Rate coefficients, k, for the gas-phase reaction of the OH radical with (E) CF3CH=CHCF3 ((E)-1,1,14,4,4-hexafluoro-2-butene, HFO-1336mzz(E)) were measured over a range of temperature (211-374 K) and bath gas pressure (20-300 Torr; He, N2) using a pulsed laser photolysis-laser induced fluorescence (PLP-LIF) technique. k1(T) was independent of pressure over this range of conditions with k1(296 K) = (1.31 ± 0.15) × 10 13 cm3 molecule 1 s 1 and k1(T) = (6.94 ± 0.80) × 10 13 exp[ (496 ± 10)/T] cm3 molecule 1 s 1, where the uncertainties are 2 and the pre-exponential term includes estimated systematic error. Rate coefficients for the OD reaction were also determined over a range of temperature (262-374 K) at 100 Torr (He). The OD rate coefficients were ~15% greater than the OH values and showed similar temperature dependent behavior with k2(T) = (7.52 ± 0.44) × 10 13 exp[ (476 ± 20)/T] and k2(296 K) = (1.53 ± 0.15) × 10 13 cm3 molecule 1 s 1. The rate coefficients for reaction 1 were also measured using a relative rate technique between 296 and 375 K with k1(296 K) measured to be (1.22 ± 0.1) × 10 13 cm3 molecule 1 s 1 in agreement with the PLP-LIF results. In addition, the 296 K rate coefficient for the O3 + (E) CF3CH=CHCF3 reaction was determined to be reaction and the significant decrease in OH reactivity compared to the (Z) CF3CH=CHCF3 stereoisomer reaction. The estimated atmospheric lifetime of (E) CF3CH=CHCF3, due to loss by reaction with OH, is estimated to be ~90 days, while the actual lifetime will depend on the location and season of its emission. Infrared absorption spectra of (E) CF3CH=CHCF3 were measured and used to estimate the 100-year time horizon global warming potentials (GWP) of 32 (atmospherically well-mixed) and 14 (lifetime-adjusted).

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 of 3-benzamido-1-(4-nitrobenzylquinolinium trifluoromethanesulfonate

Directory of Open Access Journals (Sweden)

Mariana Nicolas-Gomez

2016-05-01

Full Text Available In the title compound, C23H18N3O3+·CF3SO3−, the asymmetric unit contains two crystallographically independent organic cations with similar conformations. Each cation shows a moderate distortion between the planes of the amide groups and the quinolinium rings with dihedral angles of 14.90 (2 and 31.66 (2°. The quinolinium and phenyl rings are slightly twisted with respect to each other at dihedral angles of 6.99 (4 and 8.54 (4°. The trifluoromethanesulfonate anions are linked to the organic cations via N—H...O hydrogen-bonding interactions involving the NH amide groups. In the crystal, the organic cations are linked by weak C—H...O(nitro group interactions into supramolecular chains propagating along the b-axis direction.

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

Science.gov (United States)

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

2016-08-15

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

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

Directory of Open Access Journals (Sweden)

Jan Světlík

2009-05-01

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

Crystal structure of tetrakis[μ2-2-(dimethylaminoethanolato-κ3N,O:O]di-μ3-hydroxido-dithiocyanato-κ2N-dichromium(IIIdilead(II dithiocyanate acetonitrile monosolvate

Directory of Open Access Journals (Sweden)

Julia A. Rusanova

2016-04-01

Full Text Available The tetranuclear complex cation of the title compound, [Cr2Pb2(NCS2(OH2(C4H10NO4](SCN2·CH3CN, lies on an inversion centre. The main structural feature of the cation is a distorted seco-norcubane Pb2Cr2O6 cage with a central four-membered Cr2O2 ring. The CrIII ion is coordinated in a distorted octahedron, which involves two N atoms of one bidentate ligand and one thiocyanate anion, two μ2-O atoms of 2-(dimethylaminoethanolate ligands and two μ3-O atoms of hydroxide ions. The coordination geometry of the PbII ion is a distorted disphenoid, which involves one N atom, two μ2-O atoms and one μ3-O atom. In addition, weak Pb...S interactions involving the coordinating and non-coordinating thiocyanate anions are observed. In the crystal, the complex cations are linked through the thiocyanate anions via the Pb...S interactions and O—H...N hydrogen bonds into chains along the c axis. The chains are further linked together via S...S contacts. The contribution of the disordered solvent acetonitrile molecule was removed with the SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] procedure in PLATON. The solvent is included in the reported molecular formula, weight and density.

Bis(2,3,5,6-tetra-2-pyridylpyrazine-κ3N2,N1,N6iron(II bis(dicyanamidate 4.5-hydrate

Directory of Open Access Journals (Sweden)

R. Cortés

2010-03-01

Full Text Available In the title compound, [Fe(C24H16N62][N(CN2]2·4.5H2O, the central iron(II ion is hexacoordinated by six N atoms of two tridentate 2,3,5,6-tetra-2-pyridylpyrazine (tppz ligands. Two dicyanamide anions [dca or N(CN2−] act as counter-ions, and 4.5 water molecules act as solvation agents. The structure contains isolated cationic iron(II–tppz complexes and the final neutrality is obtained with the two dicyanamide anions. One of the dicyanamide anions and a water molecule are disordered with an occupancy ratio of 0.614 (8:0.386 (8. O—H...O, O—H...N and C—H...O hydrogen bonds involving dca, water and tppz molecules are observed.

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

Directory of Open Access Journals (Sweden)

Khusnutdin M. Shakhidoyatov

2010-03-01

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

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