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....
Energy Technology Data Exchange (ETDEWEB)
Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül
2017-12-01
The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7
International Nuclear Information System (INIS)
Adams, R.D.; Golembski, N.M.
1979-01-01
The structures of the compounds (μ-H)(H)Os 3 (CO) 10 (CN-t-C 4 H 9 ) and (μ-H) 2 Os 3 (CO) 9 (CN-t-C 4 H 9 ) have been revealed by x-ray crystallographic techniques. For (μ-H)(H)Os 3 (CO) 10 (CN-t-C 4 H 9 ): a = 9.064 (3), b = 12.225 (3), c = 20.364 (4) A; β = 98.73 (3) 0 ; space group P2 1 /c[C/sub 2h/ 5 ], No. 14; Z = 4; d/sub calcd/ = 2.79 g cm -3 . This compound contains a triangular cluster of three osmium atoms; Os(1)--Os(2) = 2.930 (1) A, Os(1)--Os(3) = 2.876 (1) A, and Os(2)--Os(3) = 3.000 (1) A. There are ten linear terminal carbonyl groups and one linear terminal isocyanide ligand which occupies an axial coordination site. The hydrogen atoms were not observed crystallographically, but their positions are strongly inferred from considerations of molecular geometry. For (μ-H) 2 Os 3 (CO) 9 (CN-t-C 4 H 9 ): a = 15.220 (8), b = 12.093 (6), c = 23.454 (5) A; space group Pbcn [D/sub 2h/ 14 ], No. 60; Z = 8; d/sub calcd/ = 2.79 g cm -3 . The compound is analogous to the parent carbonyl (μ-H) 2 Os 3 (CO) 10 and has two normal and one short osmium--osmium bonds: Os(1)--Os(2) = 2.827 (1) A, Os(1)--Os(3) = 2.828 (1) A, Os(2)--Os(3) = 2.691 (1) A. The isocyanide ligand resides in an equatorial coordination site on osmium Os(2). The hydrogen atoms were not observed but are believed to occupy bridging positions as in the parent carbonyl complex. 2 figures, 7 tables
International Nuclear Information System (INIS)
Adams, R.D.; Golembeski, N.M.
1979-01-01
The crystal and molecular structure of the compound (μ-H)(μ-eta 1 -C==N(H)(t-C 4 H 9 ))Os 3 (CO) 10 has been determined by X-ray crystallographic methods. The compound crystallizes in the centrosymmetric monoclinic space group P2 1 /n[C/sub 2h/ 5 ]:a = 13.651 (4) A, b = 9.156 (4) A, c = 18.275 (5) A, β = 111.42 (2) 0 , V = 2126.3 (25) A 3 , Z = 4, rho/sub calcd/ = 2.92 g cm -3 . A uniform triangular cluster of three osmium atoms contains ten linear carbonyl groups and a μ-eta 1 -C==N(H)(t-C 4 H 9 ) iminyl ligand. The carbon atom of the iminyl ligand symmetrically bridges one osmium-osmium bond, as is shown by the internuclear separations Os(2)-C(11) = 2.066 (8) A and Os(3)-C(11) = 2.043 (8) A. The iminyl bond, C(11)-N, is double with the C-N distance being 1.298 (10) A
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Gene-Hsiang Lee
2006-03-01
Full Text Available The title compound 6-amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]-triazin-8(7H-one (4, molecular formula C11H10N6OS, was obtained by the reaction of3-amino-2-benzyl-6-hydrazino-1,2,4-triazin-5(2H-one (3 with carbon disulfide in awater/pyridine mixture. Compound 4 can also be synthesized by reacting6-amino-3(2Hmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (7 with benzylbromide in methanolic ammonia water. The compound crystallizes in the monoclinicspace group P21/c with a = 7.2926(15, b = 14.456(2, c = 11.436(2 Ã¥, β = 105.30(2°, V= 1162.9(4 Ã¥3 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 À-À stacking interactions. 2
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Xi-Li Li
2009-09-01
Full Text Available In the title compound, [Gd(C15H11O23(C17H18N2], the GdIII atom is coordinated by six O atoms from three β-diketonate ligands and two N atoms from a chiral ligand LS,S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline, in a coordination geometry best described as distorted square-antiprismatic.
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Wolfgang Holzer
2010-09-01
Full Text Available The synthesis of the title compounds is described. Reaction of 1-substituted 2-pyrazolin-5-ones with 5-chloro-1-phenyl-1H-pyrazole-4-carbonyl chloride or 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carbonyl chloride, respectively, using calcium hydroxide in refluxing 1,4-dioxane gave the corresponding 4-heteroaroylpyrazol-5-ols, which were cyclized into 1H-pyrano[2,3-c:6,5-c]dipyrazol-4(7H-ones by treatment with K2CO3/DMF. The latter were converted into the corresponding thiones upon reaction with Lawesson’s reagent. Detailed NMR spectroscopic investigations (1H, 13C, 15N of the ring systems and their precursors are presented.
International Nuclear Information System (INIS)
Weng Shengfeng; Wang, Yun-Hsin; Lee, Chi-Shen
2012-01-01
Two novel materials, [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2), with a metal-organic framework (MOF) were prepared with hydrothermal reactions and characterized with photoluminescence, magnetic susceptibility, thermogravimetric analysis and X-ray powder diffraction in situ. The crystal structures were determined by single-crystal X-ray diffraction. Compound 1 crystallized in triclinic space group P1-bar (No. 2); compound 2 crystallized in monoclinic space group P2 1 /c (No. 14). The structure of 1 is built from a 1D MOF, composed of deprotonated citric ligands of three kinds. Compound 2 contains a 2D MOF structure consisting of citrate and oxalate ligands; the oxalate ligand arose from the decomposition in situ of citric acid in the presence of Cu II ions. Photoluminescence spectra of compounds 1b and 2 revealed transitions between the 5d 1 excited state and two levels of the 4f 1 ground state ( 2 F 5/2 and 2 F 7/2 ). Compounds 1b and 2 containing Ce III ion exhibit a paramagnetic property with weak antiferromagnetic interactions between the two adjacent magnetic centers. - Graphical Abstract: [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2)—with 1D and 2D structures were synthesized and characterized. Highlights: ► Two MOF – [M(C 6 H 5 O 7 )(C 6 H 6 O 7 )(C 6 H 7 O 7 )(H 2 O)] . H 2 O (M=La(1a), Ce(1b)) and [Ce 2 (C 2 O 4 )(C 6 H 6 O 7 ) 2 ] . 4H 2 O (2) – with 1D and 2D structures. ► The adjacent chains of the 1D framework were correlated with each other through an oxalate ligand to form a 2D layer structure. ► The source of the oxalate ligand was the decomposition in situ of citric acid oxidized in the presence of Cu II ions.
NCI calculations for understanding a physical phase transition in (C6H14N2)[Mn(H2O)6](SeO4)2
Naïli, Houcine; François, Michel; Norquist, Alexander J.; Rekik, Walid
2017-12-01
An organically templated manganese selenate, (C6H14N2)[Mn(H2O)6](SeO4)2, has been synthesized by slow evaporation and crystallographically characterized. The title compound crystallizes at room temperature in the monoclinic centrosymmetric space group P21/n, with the following unit cell parameters: a = 7.2373(4) Å; b = 12.5600(7) Å; c = 10.1945(7) Å; β = 91.155(4)°, V = 926.50(10) Å3and Z = 2. Its crystal structure is built of manganese(II) cations coordinated by six water molecules in octahedral geometry, disordered dabcodiium cations and selenate anions, resulting in an extensive hydrogen-bonding network. Differential scanning calorimetry (DSC) measurement indicated that the precursor undergoes a reversible phase transition at about 216 and 218 K during the cooling and heating processes respectively. Below this temperature the title compound is noncentrosymmetric with space group P21 and lattice parameters a = 7.2033(8) Å; b = 12.4981(13) Å; c = 10.0888(11) Å; β = 91.281(2)°, V = 908.04(17) Å3 and Z = 2. The disorder-order transformation of the C atoms of (C6H14N2)2+ cation may drive the structural phase transition. The low temperature phase obtained by breaking symmetry presents a fully ordered structure. The noncovalent interaction (NCI) method was used not only to locate, quantify, and visualize intermolecular interactions in the high and low temperature phases but also to confirm the phase transition detected by DSC measurement. The thermal decomposition of this new compound proceeds through four stages giving rise to the manganese oxide as final product at 850 °C.
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Abdellah N'ait Ousidi
2016-03-01
Full Text Available The title compound, C13H19N3OS, is a new thiazolidin-4-one derivative prepared and isolated as the pure (3aS,6R-diastereisomer from (R-thiosemicarbazone pulegone. It crystallized with two independent molecules (A and B in the asymmetric unit. The compound is composed of a hexhydroindazole ring system (viz. a five-membered dihydropyrazole ring fused to a cyclohexyl ring with a thiazole-4-one ring system attached to one of the pyrazole N atoms (at position 2. The overall geometry of the two molecules differs slightly, with the mean planes of the pyrazole and thiazole rings being inclined to one another by 10.4 (1° in molecule A and 0.9 (1° in molecule B. In the crystal, the A and B molecules are linked via C—H...O hydrogen bonds, forming slabs parallel to the ab plane. There are C—H...π interactions present within the layers, and between the layers, so forming a three-dimensional structure.
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Assem Barakat
2016-09-01
Full Text Available 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-yl-methyl]-6-hydroxy-1,3-di-methylpyrimidine-2,4(1H,3H-dione 3 was synthesized via a multicomponent reaction. The Aldol–Michael addition reactions of N,N-dimethylbarbituric acid, cyclohexane-1,3-dione, and 3-fluorobenzaldehyde in aqueous solution gave the product in high yield. The molecular structure of the compound was confirmed by spectroscopic methods and X-ray crystallography. The title compound (C19H19FN2O5·H2O crystallizes in the Monoclinic form, P21/c, a = 7.8630 (5 Å, b = 20.0308 (13 Å, c = 11.3987 (8 Å, β = 104.274 (3°, V = 1739.9 (2° Å3, Z = 4, Rint = 0.117, wR(F2 = 0.124, T = 100 K.
Synthesis and 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
(E-N-[2-(9-Fluorenylidene-3a,5,7-trimethyl-3,3a-dihydro-2H-indol-3-ylidene]-2,4,6-trimethylaniline
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Norihiro Tokitoh
2008-02-01
Full Text Available The title compound, C33H30N2, has an E configuration at the imine double bond. The angle between the least-squares planes of the imine C=N—C group and the benzene ring of the 2,4,6-trimethylphenyl substituent is 85.38 (11°. The crystal structure is sustained mainly by intermolecular π–π interactions (3.510 Å between the two fluorene rings and some C—H...π interactions.
Crystal structure of tetraaquabis(1,3-dimethyl-2,6-dioxo-7H-purin-7-ido-κN7cobalt(II
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Hicham El Hamdani
2017-09-01
Full Text Available The title complex, [Co(C7H7N4O22(H2O4], comprises mononuclear molecules consisting of a CoII ion, two deprotonated theophylline ligands (systematic name: 1,3-dimethyl-7H-purine-2,6-dione and four coordinating water molecules. The CoII atom lies on an inversion centre and has a slightly distorted octahedral coordination environment, with two N atoms of two trans-oriented theophylline ligands and the O atoms of four water molecules. An intramolecular hydrogen bond stabilizes this conformation. A three-dimensional supramolecular network structure is formed by intermolecular O—H...O and O—H...N hydrogen bonds.
Ethyl 2-[(2-hydroxybenzylideneamino]-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate
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Naki Çolak
2013-07-01
Full Text Available The title compound, C18H20N2O3S, exists as the phenol–imine form in the crystal and there are bifurcated intramolecular O—H...(N/O hydrogen bonds present. The conformation about the C=N bond is anti (1E; the C=N imine bond length is 1.287 (4 Å and the C=N—C angle is 122.5 (3°. In the tetrahydrothienopyridine moiety, the six-membered ring has a flattened-boat conformation. In the crystal, molecules are stacked nearly parallel to (110 and a weak C—H...π interaction is observed. The carbonyl O atom is disordered over two positions and was refined with a fixed occupancy ratio of 0.7:0.3.
N-Cyano-7α-methoxycarbonyl-6,14-endo-ethenotetrahydronorthebaine
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Mustafa Odabaşoğlu
2009-09-01
Full Text Available In the title compound (systematic name: methyl 17-cyano-3,6-dimethoxy-4,5α-epoxy-6,14-endo-ethenomorphinan-7-carboxylate, C23H24N2O5, the dihydrofuran ring adopts a twist conformation, while the piperidine ring is in a chair conformation. The benzene-fused cyclohexene ring adopts an envelope conformation. An intramolecular C—H...O hydrogen bond is observed. Intermolecular C—H...N and C—H...O hydrogen bonds form C(5 chains along the a and b axes, respectively, and together they form a three-dimensional network.
Ali, Mohamed A; Ismail, Rusli; Choon, Tan S; Yoon, Yeong K; Wei, Ang C; Pandian, Suresh; Samy, Jeyabalan G; De Clercq, Eric; Pannecouque, Christophe
2011-01-01
A series of novel 3-(substituted phenyl)-6,7-dimethoxy-3a,4-dihydro-3H-indeno[1,2-c]isoxazole analogues were synthesized by the reaction of 5,6-dimethoxy-2-[(E)-1-phenylmethylidene]-1-indanone with hydroxylamine hydrochloride. The title compounds were tested for their in vitro anti-HIV activity. Among the compounds, (4g) showed a promising anti-HIV activity in the in vitro testing against IIIB and ROD strains. The IC50 of both IIIB and ROD were found to be 9.05 microM and > 125 microM, respectively.
2-(7-Methyl-1H-indol-3-ylacetonitrile
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Yu-Hua Ge
2012-01-01
Full Text Available In the title compound, C11H10N2, the carbonitrile group is twisted away from the indole plane [Ccy—Cme—Car—Car = 66.6 (2°; cy = cyanide, me = methylene and ar = aromatic]. In the crystal, N—H...N hydrogen bonds link the molecules into C(7 chains propagating in the [001] direction.
High-pressure pyrolysis study of C sub 3 N sub 6 H sub 6 : a route to preparing bulk C sub 3 N sub 4
Ma, H A; Chen, L X; Zhu, P W; Guo, W L; Guo, X B; Wang, Y D; Li, S Q; Zou Guang Tian; Zhang, G; Bex, P
2002-01-01
In order to prepare bulk C sub 3 N sub 4 , high-pressure pyrolysis of melamine (C sub 3 N sub 6 H sub 6) at different temperatures was carried out. The products were characterized by C, N, H element analysis, Fourier transform infrared spectroscopy, x-ray photoelectron spectroscopy, and x-ray diffractometry. The results of the analysis reveal that graphitic phase C sub 3 N sub 4 has been synthesized. It provides a novel route to synthesis of the theoretical superhard cubic C sub 3 N sub 4 and other C sub 3 N sub 4 phases from organic compounds by a high-pressure and high-temperature method.
Ethyl 3-[7-ethoxy-6-(4-methoxybenzenesulfonamido-2H-indazol-2-yl]propanoate
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Najat Abbassi
2012-04-01
Full Text Available In the title compound, C21H25N3O6S, the dihedral angle between the methoxybenzene and indazole rings is 74.96 (5°. The crystal packing is stabilized by an N—H...O hydrogen bond into a two-dimensional network. In addition, C—H...π interactions and a π–π contact, with a centroid–centroid distance of 3.5333 (6 Å, are observed. The crystal packing is stabilized by N—H...O and C—H...O hydrogen bonds.
5-tert-Butyl 3-ethyl 1-isopropyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine-3,5-dicarboxylate
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Huan-Mei Guo
2011-12-01
Full Text Available In the title compound, C17H27N3O4, the six-membered ring adopts a half-chair conformation with the N atom and the adjacent methylene C atom displaced by −0.391 (2 and 0.358 (2 Å, respectively, from the plane of the other four atoms. In the crystal, molecules are linked by weak C—H...O interactions.
6-Butyl-5-(4-methoxyphenoxy-3-phenyl-3H-1,2,3-triazolo[4,5-d]pyrimidin-7(6H-one
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Hong-Mei Wang
2009-12-01
Full Text Available The asymmetric unit of the title compound, C21H21N5O3, consists of two geometrically similar molecules. The fused rings of the triazolo[4,5-d]pyrimidine system are nearly coplanar, making dihedral angels of 1.48 (18 and 1.34 (16°, and the phenyl rings are twisted by 12.3 (1 and 8.7 (1° with respect to the triazolopyrimidine plane. The ethyl groups of the n-butyl side chains are disordered over two sites in each of the independent molecules, the ratios of occupancies being 0.60:0.40 and 0.61:0.39.
Neutron diffraction analysis of HRh[P(C6H5)3]4
International Nuclear Information System (INIS)
Bau, R.; Stevens, R.C.; McLean, M.; Koetzle, T.F.
1987-01-01
We have collected neutron diffraction data on a large single crystal of the title compound. The most surprising result is an extremely short Rh-H distance of 1.31(8) A, presumably caused by steric interactions involving the bulky triphenyl phosphine ligands. Crystallographic details: HRh[P(C 6 H 5 ) 3 ] 4 . 1 / 2 C 6 H 6 crystallizes in the space group Pa3, with a = b = c = 22.776(3) A, Z = 8. Data were collected at the Brookhaven High Flux Beam reactor at a temperature of -23 0 C, λ = 1.15882(7) A -1 . Least-squares refinement (in which the phenyl rings were treated as rigid groups) resulted in an R factor [based on data with f > 4σ(F)] of 0.12 for 914 reflections and 95 parameters. 10 refs
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Augusto Rivera
2011-09-01
Full Text Available The complete molecule of the title compound, C31H42N2O6, is generated by crystallographic twofold symmetry, with one C atom lying on the axis. The dihedral angle between the aromatic rings is 57.03 (6°. The central heterocyclic ring adopts a half-chair conformation. The molecular conformation is stabilized by two intramolecular O—H...N hydrogen bonds with the N atoms of the heterocyclic ring as the acceptors. In the crystal, molecules are linked into chains along the c axis by non-classical C—H...O hydrogen bonds.
Crystal structure of 2-amino-N-(2-fluorophenyl-4,5,6,7-tetrahydro-1-benzothiophene-3-carboxamide
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K. Chandra Kumar
2015-11-01
Full Text Available In the title compound, C15H15FN2OS, the dihedral angle between the planes of the benzothiophene ring system and the fluorobenzene ring is 3.74 (14°. The six-membered ring of the benzothiophene moiety adopts a half-chair conformation. The molecular conformation is consolidated by intramolecular N—H...F and N—H...O hydrogen bonds. In the crystal, molecules are linked by N—H...O hydrogen bonds, generating C(6 [001] chains.
5-Fluoro-6′H,7′H,8′H-spiro[indoline-3,7′-pyrano[3,2-c:5,6-c′]di-1-benzopyran]-2,6′,8′-trione
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J. Suresh
2012-03-01
Full Text Available In the title compound, C26H12FNO6, the central pyran ring and both benzopyran systems are nonplanar, having total puckering amplitudes of 0.139 (2, 0.050 (1 and 0.112 (2 Å, respectively. The central pyran ring adopts a boat conformation. The crystal structure is stabilized by C—H...O, N—H...O, N—H...F and C—H...π interactions.
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.
3′,6′-Bis(diethylamino-3H-spiro[2-benzothiophene-1,9′-xanthene]-3-thione
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Bing-Yuan Su
2008-11-01
Full Text Available The title compound, C28H30N2OS2, was obtained by thionation of 3′,6′-bis(diethylamino-3H-spiro[isobenzofuran-1,9′-xanthene]-3-one with 2,4-bis(p-methoxyphenyl-1,3-dithiadiphosphetane disulfide (Lawesson's reagent. The planes of the two benzene rings of the xanthene system are inclined at a dihedral angle of 17.4 (1°, and the plane of the dithiophthalide group and the planes through the two benzene rings of the xanthene system make dihedral angles of 80.2 (1 and 82.8 (1°, respectively.
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Huichun Zhu
2010-01-01
Full Text Available rac-Benzyl 3-oxohexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H-carboxylate was separated by chiral chromatography, and one of the enantiomers ([α]22D = +10° was hydrogenated in the presence of Pd/C in methanol, producing octahydro-3H-pyrrolo[3,4-c]pyridin-3-one. The latter was reacted with (2R-3,3,3-trifluoro-2-methoxy-2-phenylpropanoyl chloride [(R-(−-Mosher acid chloride], giving rise to the title compound, C17H19F3N2O3·H2O. The present structure established the absolute configuration of the pyrrolopiperidine fragment based on the known configuration of the (R-Mosher acid chloride. The piperidine ring has a somewhat distorted chair conformation and is cis-fused with the five-membered envelope-shaped ring; the plane of the exocyclic amide bond is approximately orthogonal to the plane of the phenyl ring, making a dihedral angle of 82.31 (3°. The water molecule acts as an acceptor to the proton of the amino group in an N—H...O interaction, and as a double proton donor in O—H...O hydrogen bonds, generating infinite bands along the a axis.
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Shoaib Anwar
2012-08-01
Full Text Available The synthesis, structure and properties of the bimetallic layered coordination polymer, [KDy(C8H3NO63(C8H5NO6]n·2n(C10H9N2·5n(H2O = [KDy(Hptc3(H3ptc]n·2n(Hbipy·5n(H2O, are described. The Dy3+ ion is coordinated by three O,N,O-tridentate doubly-deprotonated pyridine tri-carboxylate (Hptc ligands to generate a fairly regular DyO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The potassium ion is coordinated by an O,N,O-tridentate H3ptc molecule as well as monodentate and bidentate Hptc ligands to result in an irregular KNO9 coordination geometry. The ligands bridge the metal-atom nodes into a bimetallic, layered, coordination polymer, which extends as corrugated layers in the (010 plane, with the mono-protonated bipyridine cations and water molecules occupying the inter-layer regions: Unlike related structures, there are no dysprosium–water bonds. Many O–HLO and N–HLO hydrogen bonds consolidate the structure. Characterization and bioactivity data are described. Crystal data: C52H42DyKN8O29, Mr = 1444.54, triclinic, (No. 2, Z = 2, a = 9.188(2 Å, b = 15.7332(17 Å, c = 19.1664(19 Å, α = 92.797(6°, β = 92.319(7°, γ = 91.273(9°, V = 2764.3(7 Å3, R(F = 0.029, wR(F2 = 0.084.
(3R,6S,7aS-3-Phenyl-6-(phenylsulfanylperhydropyrrolo[1,2-c]oxazol-5-one
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Anthony D. Woolhouse
2009-05-01
Full Text Available Molecules of the title compound [systematic name: (2R,5S,7S-2-phenyl-7-phenylsulfanyl-1-aza-3-oxabicyclo[3.3.0]octan-8-one], C18H17NO2S, form high quality crystals even though they are only packed using C—H...O(carbonyl and weak C—H...S interactions. The dihedral angle between the aromatic rings is 85.53 (5°. The fused rings adopt envelope and twist conformations.
Tert-butyl 3-oxo-2,3,4,5,6,7-hexahydro-1H-pyrazolo[4,3-c]pyridine-5-carboxylate
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Tara Shahani
2010-01-01
Full Text Available In the title compound, C11H17N3O3, the pyrazole ring is approximately planar, with a maximum deviation of 0.005 (2 Å, and forms a dihedral angle of 5.69 (13° with the plane through the six atoms of the piperidine ring. In the crystal, pairs of intermolecular N—H...O hydrogen bonds form dimers with neighbouring molecules, generating R22(8 ring motifs. These dimers are further linked into two-dimensional arrays parallel to the bc plane by intermolecular N—H...O and C—H...O hydrogen bonds.
Energy Technology Data Exchange (ETDEWEB)
Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Baker Lab.; Schulz, Armin [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)
2016-07-01
Transparent colorless crystals of NaA{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O (A = Rb, Cs) were obtained by blending aqueous solutions of Na{sub 3}[C{sub 6}N{sub 9}] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group P2{sub 1}/m (no. 11) with the cell parameters a = 815.56(16), b = 1637.7(4) and c = 1036.4(3) pm, and β = 110.738(12) for NaRb{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O and a = 843.32(6), b = 1708.47(11) and c = 1052.42(7) pm, and β = 112.034(2) for NaCs{sub 5}[C{sub 6}N{sub 9}]{sub 2} . 4 H{sub 2}O, respectively. Raman spectra of the title compounds complement our results.
Study of the unimolecular decompositions of the (C3H6)+2 and (c-C3H6)+2 complexes
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Tzeng, W.; Ono, Y.; Linn, S.H.; Ng, C.Y.
1985-01-01
The major product channels identified in the unimolecular decompositions ofC 3 H + 6 xC 3 H 6 and c-C 3 H + 6 xc-C 3 H 6 in the total energy [neutral (C 3 H 6 ) 2 or (c-C 3 H 6 ) 2 heat of formation plus excitation energy] range of approx.230--450 kcal/mol are C 3 H + 7 +C 3 H 5 , C 4 H + 7 +C 2 H 5 , C 4 H + 8 +C 2 H 4 , and C 5 H + 9 +CH 3 . The measured appearance energy for C 4 H + 7 (9.54 +- 0.04 eV) from (C 3 H 6 ) 2 is equal to the thermochemical threshold for the formation of C 4 H + 7 +C 2 H 5 from (C 3 H 6 ) 2 , indicating that the exit potential energy barrier for the ion--molecule reaction C 3 H + 6 +C 3 H 6 →C 4 H + 7 +C 2 H 5 is negligible. There is evidence that the formations of C 4 H + 7 +C 2 H 4 +H from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 also proceed with high probabilities when they are energetically allowed. The variations of the relative abundances for C 4 H + 7 ,C 4 H + 8 , and C 5 H + 9 from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 as a function of ionizing photon energy are in qualitative agreement, suggesting that (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 rearrange to similar C 6 H + 12 isomers prior to fragmentation. The fact that C 6 H + 11 is found to be a primary ion from the unimolecular decomposition of (c-C 3 H 6 ) + 2 but not (C 3 H 6 ) + 2 supports the conclusion that the distribution of C 6 H + 12 collision complexes involved in the C 3 H + 6 +C 3 H 6 reactions is different from that in the cyclopropane ion--molecule reactions
Uludağ, Nesimi; Serdaroğlu, Goncagul; Yinanc, Abdullah
2018-06-01
In this study, we performed a novel synthesis of the octahydropyrido[3,2-c]carbazole derivative 6 from 1 in five steps with a 34% overall yield. We also developed a unique compound 2 by a cyclization reaction from the cyanoethylation of compound 1, which is an intermediate step in the synthesis of Aspidospermidine. The parent compound of Aspidospermidine alkaloids, comprise a large family of diverse structures. As a result, we obtained octahydropyrido[3,2-c]carbazole (6)and the proposed method may be applicable to other alkaloids. All quantum chemical calculations of the cis-4a-Ethyl-1-(2-hydroxyethyl)-2,3,4,4a,5,6,7,11c-octahydro-1H-pyrido[3,2-c]carbazole have been performed with the DFT/B3LYP and HF methods by using the Gaussian 09W software package. The most stable conformer obtained from the Potential Energy Surface (PES) scan analysis at the B3LYP/6-31G** level of theory in the gas phase was used as the starting structure of the title compound to further computational analysis. The Natural Bond Orbital (NBO) and NLO analyses were performed to evaluate the intra-molecular interactions contributing to the molecular stability and to predict the optical properties of the title compound, respectively. Gauge-Independent Atomic Orbital (GIAO) approach was used to determine the 1H and 1C NMR chemical shifts of the title compound by subtracting the shielding constants of TMS at both methods. The calculated vibrational frequencies of the title compound were assigned by using the VEDA program and were scaled down by using the scaling factor 0.9668 for B3LYP/6-311++G(d, p) and 0.9050 for HF/6-311++G(d, p) to improve the calculated vibrational frequencies. The FMO (frontier molecular orbital) analysis was evaluated to predict the chemical and physical properties of the title compound and the HOMO, LUMO, and MEP diagrams were visualized by GaussView 4.1 program to present the reactive site of the title compound.
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Augusto Rivera
2013-02-01
Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, there are two intramolecular O—H...N hydrogen bonds involving the N atoms of the imidazolidine ring and the hydroxy groups. The crystal studied was a meso compound obtained by the reaction of the aminal (2S,7R,11S,16R-1,8,10,17-tetraazapentacyclo[8.8.1.18,17.02,7.011,16]cosane with 4-fluorophenol. The imidazolidine ring has a twisted conformation with a CH—CH—N—CH2 torsion angle of 44.99 (14° and, surprisingly, the lone pairs of the N atoms are disposed in a syn isomerism, making the title compound an exception to the typical `rabbit-ear effect' in 1,2-diamines. In the crystal, molecules are linked via C—H...F hydrogen bonds, forming chains along the c-axis direction. These chains are linked via another C—H...F hydrogen bond, forming a three-dimensional network.
1-[(6-Chloro-3-pyridylmethyl]-N-(4-ethoxyphenyl-3-phenyl-1H-pyrazole-5-carboxamide
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Zheng Tang
2009-04-01
Full Text Available In the title compound, C24H21ClN4O2, the pyrazole ring makes dihedral angles of 7.70 (11, 89.17 (11 and 40.68 (11° with the phenyl, pyridine and ethoxyphenyl rings, respectively. There are some intramolecular C—H...O and C—H...π bonds giving rigidity to the molecule, while weak intermolecular N—H...N and C—H...π hydrogen bonds link the molecules into a two-dimensional structure.
2,6-Diaminopyridinium bis(4-hydroxypyridine-2,6-dicarboxylato-κ3O2,N,O6ferrate(III dihydrate
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Andya Nemati
2008-10-01
Full Text Available The reaction of iron(II sulfate heptahydrate with the proton-transfer compound (pydaH(hypydcH (pyda = pyridine-2,6-diamine; hypydcH2 = 4-hydroxypyridine-2,6-dicarboxylic acid in an aqueous solution led to the formation of the title compound, (C5H8N3[Fe(C7H3NO52]·2H2O. The anion is a six-coordinated complex with a distorted octahedral geometry around the FeIII atom. Extensive intermolecular O—H...O, N—H...O and C—H...O hydrogen bonds, involving the complex anion, (pydaH+ counter-ion and two uncoordinated water molecules, and π–π [centroid-to-centroid distance 3.323 (11 Å] and C—O...π [O–centroid distance 3.150 (15 Å] interactions connect the various components into a supramolecular structure.
2-Ethyl-6-(2-pyridyl-5,6,6a,11b-tetrahydro-7H-indeno[2,1-c]quinoline
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Alexander Briceño
2010-03-01
Full Text Available The title compound, C23H22N2, was obtained using the three-component imino Diels–Alder reaction via a one-pot condensation between anilines, α-pyridinecarboxyaldehyde and indene using BF3·OEt2 as the catalyst. The molecular structure reveals the cis-form as the unique diastereoisomer. The crystal structure comprises one-dimensional zigzag ribbons connected via N—H...N hydrogen bonds. C—H...π interactions also occur.
Sleymi, Samira; Lahbib, Karima; Rahmouni, Nihed; Rzaigui, Mohamed; Besbes-Hentati, Salma; Abid, Sonia
2017-09-01
A new organic-inorganic hybrid transition metal phosphate, Cu1.5Li(C2H10N2)P6O18·7H2O, has been prepared and characterized by X-ray diffraction, spectroscopy (infrared, Raman, diffuse reflectance and UV-Vis) and thermal analysis (TG). In addition, its electrochemical behaviors, as well as its antioxidant and antibacterial activities, have been investigated. Its structure is built up by the alternate linkages between copper and phosphate polyhedra, forming puckered layers with intersecting 12-membered rings, in which the ethylenediammonium cations reside. This compound is the first framework structure constructed from cyclohexaphosphates and three distinct copper cations. Cyclic voltammetry study in an acetonitrile solution reveals the facile anodic oxidation of its organic part on a platinum disk and a progressive growing of a thin film, though the repetitive cycling of potential. The title compound was tested for its in vitro antioxidant activities by 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2‧-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS), Ferrous chelating ability (FIC) and Ferric Reducing Power (FRP) methods. The antioxidant activity of Cu1.5Li(C2H10N2)P6O18·7H2O was analyzed simultaneously with its antibacterial capacity against Escherichia coli, Salmonella typhimurium, Staphylococus aureus, Enterococcus feacium, Streptococcus agalactiae and Candida albicans. The tested compound showed significant antioxidant activities with low antibacterial properties.
Sagar, Belakavadi K; Harsha, Kachigere B; Yathirajan, Hemmige S; Rangappa, Kanchugarakoppal S; Rathore, Ravindranath S; Glidewell, Christopher
2017-03-01
In each of 1-(4-fluorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 F 4 N 3 O 2 S, (I), 1-(4-chlorophenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 21 H 19 ClF 3 N 3 O 2 S, (II), and 1-(3-methylphenyl)-5-methylsulfonyl-3-[4-(trifluoromethyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine, C 22 H 22 F 3 N 3 O 2 S, (III), the reduced pyridine ring adopts a half-chair conformation with the methylsulfonyl substituent occupying an equatorial site. Although compounds (I) and (II) are not isostructural, having the space groups Pbca and P2 1 2 1 2 1 , respectively, their molecular conformations are very similar, but the conformation of compound (III) differs from those of (I) and (II) in the relative orientation of the N-benzyl and methylsulfonyl substituents. In compounds (II) and (III), but not in (I), the trifluoromethyl groups are disordered over two sets of atomic sites. Molecules of (I) are linked into centrosymmetric dimers by C-H...π(arene) hydrogen bonds, molecules of (II) are linked by two C-H...O hydrogen bonds to form ribbons of R 3 3 (18) rings, which are themselves further linked by a C-Cl...π(arene) interaction, and a combination of C-H...O and C-H...π(arene) hydrogen bonds links the molecules of (III) into sheets. Comparisons are made with the structures of some related compounds.
Lee, Dong Woo; Jo, Vinna; Ok, Kang Min
2012-10-01
A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C3H7)4]3Ga3[C6H3(CO2)3]4 (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO3)3·xH2O, 1,3,5-C6H3(CO2H)3, N(C3H7)4Cl, HNO3, and HCON(CH3)2 at 180 °C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO4 tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of α-SiO2 and the material is phase-matchable (type-1).
Nqrs Data for C6H7F7N2OSb2 (Subst. No. 0880)
Chihara, H.; Nakamura, N.
This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C6H7F7N2OSb2 (Subst. No. 0880)
rac-1-[6-Hydroxy-4-(4-methoxyphenyl-3,6-dimethyl-4,5,6,7-tetrahydro-2H-indazol-5-yl]ethanone
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Konstantin A. Potekhin
2013-02-01
Full Text Available The title compound, C18H22N2O3, represents a (4S,5R,6S-stereoisomer, crystallizing as a racemate in a centrosymmetric space group. The six-membered aliphatic ring adopts a half-chair conformation, with the hydroxy- and acetyl-substituted C atoms deviating by 0.458 (2 and −0.366 (2 Å, respectively, from the plane defined by other four ring atoms. The pyrazole ring is essentially planar [r.m.s deviation = 0.004 (2 Å]. In the crystal, the molecules are linked into chains along the b axis by N—H...N hydrogen bonds. The chains are linked by O—H...N hydrogen bonds into layers parallel to the bc plane.
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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.
2-Isobutyl-6-(4-methoxyphenylimidazo[2,1-b][1,3,4]thiadiazole
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Hoong-Kun Fun
2011-02-01
Full Text Available In the title compound, C15H17N3OS, the dihedral angle between the statistically planar imidazo[2,1-b][1,3,4]thiadiazole fused-ring system (r.m.s. deviation = 0.002 Å and the methyoxbenzene ring is 4.52 (6°. In the crystal, molecules are arranged into columns and stacked down the a axis. The crystal structure is stabilized by weak C—H...π and π–π interactions [centroid–centroid separations = 3.6053 (8 and 3.7088 (7 Å].
International Nuclear Information System (INIS)
Hayes, B.A.; Gupta, Surendra; Shaochieh Chang; Utecht, R.E.; Lewis, D.E.
1996-01-01
The synthesis of N,N'-bis-{2-[(5-bromo-2-[1- 14 C]hexyl-1H-benz[de]isoquinolin-1, 3(2H)-dion-6-yl)amino]ethyl}hexanediamide from 1-[1- 14 C]-hexylamine and 4-chloro-1,8-naphthalic anhydride is described. The anhydride is first converted to the 4-chloro-n-[1- 14 C]hexyl-1,8-naphthalimide by condensation with 1-[1- 14 C]-hexylamine, and the chlorine is then displaced with ethylenediamine to give the 4-(2-aminoethylamino-N-[1- 14 C]hexyl-1,8-naphthalimide. Coupling of this monomeric naphthalimide with adipoyl chloride affords the dimeric naphthalimide which is brominated regiospecifically with elemental bromine in carbon tetrachloride to afford the title compound. (author)
2,3-Diaminopyridinium 6-carboxypyridine-2-carboxylate
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Mahsa Foroughian
2011-12-01
Full Text Available The asymmetric unit of the title proton-transfer compound, C5H8N3+·C7H4NO4−, consists of one mono-deprotonated pyridine-2,6-dicarboxylic acid as anion and one protonated 2,3-diaminopyridine as cation. The crystal packing shows extensive O—H...O, N—H...O and N—H...N hydrogen bonds. Thre are also several π–π interactions between the anions and also between the cations [centriod–centroid distances = 3.6634 (7, 3.7269 (7, 3.6705 (7 and 3.4164 (7 Å].
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Peter W. Dibble
2008-09-01
Full Text Available The title compound, C25H18N2O6, is a naphthalenophane styled in the manner of Warrener's alicyclic cyclophanes or molecular racks wherein a trimethylene tether is perfectly staggered between the two N atoms such that the central methylene H atoms point toward the naphthalene π-system. The dihedral angle between the mean planes of the two benzene rings is 7.61 (7°.
International Nuclear Information System (INIS)
Yu Xiaohong; Zhang Hanhui; Cao Yanning; Chen Yiping; Wang Zhen
2006-01-01
A novel 3-D compound of (enH 2 ) 1.5 [Bi 3 (C 2 O 4 ) 6 (CO 2 CONHCH 2 CH 2 NH 3 )].6.5H 2 O has been hydrothermally synthesized and characterized by IR, ultraviolet-visible diffuse reflection integral spectrum (UV-Vis DRIS), fluorescence spectra, TGA and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group C2/c with a=31.110(8)A, b=11.544(3)A, c=22.583(6)A, β=112.419(3) o , V=7497(3)A 3 , Z=8, R 1 =0.0463 and wR 2 =0.1393 for unique 7686 reflections I>2σ(I). In the title compound, the Bi atoms have eight-fold and nine-fold coordination with respect to the oxygen atoms, with the Bi atoms in distorted dodecahedron and monocapped square antiprism, respectively. The 3-D framework of the title compound contains channels and is composed of linkages between Bi atoms and oxalate units, forming honeycomb-like layers with two kinds of 6+6 membered aperture, and pillared by oxalate ligands and monamide groups. The channels have N-ethylamine oxalate monamide group - CO 2 CONHCH 2 CH 2 NH 3 + , which is formed by the in situ reaction of en and oxalate acid. At room temperature, the complex exhibits intense blue luminescence with an emission peak at 445nm
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Armen Ayvazyan
2014-10-01
Full Text Available The title compound, C20H18N6O5·0.5C3H7NO, crystallized as a dimethylformamide (DMF solvate. In the main molecule, the dihedral angle between the pyridodipyrimidine fused-ring system and the benzamide substituent is 82.26 (11°. In the crystal, the benzamide molecules are linked by N—H...O hydrogen bonds to generate tetramers with an approximate square-prismatic shape, which appears to correlate with the tetragonal crystal symmetry. The DMF molecule is disordered about a crystallographic twofold axis and accepts a C—H...O interaction from the benzamide molecule.
Studies of the pressure-induced phase transition of C sub 3 N sub 6 H sub 6
Ma Hong An; Cui Qi Liang; Pan Yue Wu; Zhu Pin Wen; Guo Wei; Chen Li Xue; Ren Guo Zheng; Zou Guang Tian; LiuJing
2002-01-01
In situ high pressure energy dispersive X-ray diffraction experiments have been carried out on C sub 3 N sub 6 H sub 6 by using diamond anvil cell (DAC) device with synchrotron radiation source. Two structural phase transitions of C sub 3 N sub 6 H sub 6 have been observed within 14.7 GPa pressure range, from monoclinic to triclinic structure at 1.3 GPa and from triclinic to orthorhombic structure at 8.2 GPa, respectively
7,7′-(3,3′-Dibenzyl-3H,3′H-4,4′-bi-1,2,3-triazole-5,5′-diylbis(4-methyl-2H-chromen-2-one
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Michael J. Ferguson
2008-10-01
Full Text Available The title compound, a bis-5,5′-triazole, C38H28N6O4, was observed as a side-product from the Sharpless–Meldal click reaction of the corresponding coumarin alkyne and benzylazide. Although the compound was present as a minor component, it crystallized in preference to the major product. The two triazole rings are almost orthogonal to each other [dihedral angle = 83.8 (1°]. However the 4 and 4′ coumarin systems are close to coplanar with their respective triazole rings [23.6 (1 and 15.1 (1°]. Each of the benzene rings packs approximately face-to-face with the opposing coumarin ring systems, with interplanar angles of 7.7 (1 and 25.3 (1° and distances of 3.567 (2 and 3.929 (2 Å between the respective centroids of the opposing rings.
Crystal structure of 4-(1H-indol-3-yl-2-(4-methoxyphenyl-6-phenylpyridine-3-carbonitrile
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R. Vishnupriya
2014-10-01
Full Text Available In the title compound, C27H19N3O, the dihedral angles between the plane of the pyridine ring and those of the indole (r.m.s. deviation = 0.018 Å, phenyl and methoxybenzene substituents are 33.60 (6, 25.28 (7 and 49.31 (7°, respectively. The N atom of the carbonitrile group is significantly displaced [0.288 (2 Å] from the plane of the pyridine ring, perhaps due to steric crowding. In the crystal, inversion dimers linked by pairs of N—H...Nn (n = nitrile hydrogen bonds generate R22(16 loops. Aromatic π–π stacking [centroid–centroid separation = 3.6906 (7 Å] and very weak C—H...π interactions are also observed".
International Nuclear Information System (INIS)
Boeddinghaus, M. Bele; Klein, Wilhelm; Wahl, Bernhard; Faessler, Thomas F.; Jakes, Peter; Eichel, Ruediger A.
2014-01-01
Five new compounds, [Rb(18crown-6)]_3[C_6_0] (1), [Rb(18crown-6)]_6[C_6_0]_2(C_3H_7NO)_2(C_4H_8O)_2 (2), [Rb(benzo18crown-6)]_6[C_6_0]_2(C_2H_8N_2)_5 (3), [Cs(benzo18crown-6)]_3C_6_0(C_2H_8N_2)_2 (4), and [Cs_3(benzo18crown-6)_5]C_6_0(C_2H_8N_2)_(_4_._5_+_x_) (5) were synthesized and characterized by single-crystal X-ray structure determination. All compounds contain discrete C_6_0 anions, which are ordered in 1, 2, and 4, where direct cation-anion contacts occur. The unit cells of 1 and 2 contain two independent fullerides, which coordinate to the rubidium atoms either of two or of four [Rb(18crown-6)] units. Owing to the presence of differently coordinated fullerene units in compounds 1 and 2, a possible disproportionation of C_6_0"3"- into C_6_0"2"- and C_6_0"4"- anions is discussed. In 3 and 4 the C_6_0 anions are coordinated by three Rb and Cs atoms, respectively. In all compounds the average charge of the anion is -3. Magnetic data reveal a doublet spin state for 3. The EPR spectra are discussed for compounds 3 and 5. The role of a dynamic Jahn-Teller distortion is discussed, and we report the first IR spectroscopic data of fullerene trianions, which have been obtained in solution. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)
N6,3′-cyclo-5′-O-Cyanomethylthymidine
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Jingbo Sun
2010-06-01
Full Text Available The title compound, C19H20N4O4, is a cyclonucleoside with a C—N linkage. The furanose ring adopts a twist C3′-endo/C2′-exo (close to 3T2 conformation with a pseudorotational phase angle (P of 8.1° and puckering amplitude (vm of 30.6°. The orientation of the pyrimidine ring with respect to the sugar group is anti. One intramolecular C—H...O hydrogen bond is observed. The packing features an N—H...O hydrogen bond.
6,7-Dichloro-3-(2,4-dichlorobenzylquinoxalin-2(1H-one
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Jinpeng Zhang
2012-08-01
Full Text Available In the title compound, C15H8Cl4N2O, the quinoxaline ring system is almost planar, with a dihedral angle between the benzene and pyrazine rings of 3.1 (2°. The 2,4-dichlorophenyl ring is approximately perpendicular to the pyrazine ring, with a dihedral angle of 86.47 (13° between them. The crystal packing features intermolecular N—H...O hydrogen bonds and π–π stacking interactions, with centroid–centroid distances in the range 3.699 (3–4.054 (3 Å.
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Gudilenkov, I.D.; Fukin, G.K.; Cherkasov, A.V.; Shavyrin, A.S.; Trifonov, A.A.; Larionova, Yu.E.
2008-01-01
Reaction of ytterbium bisindenyl complex (C 9 H 7 ) 2 Yb II (THF) 2 (1) with 1,4-diazabutadiene 2-MeC 6 H 4 N=C(Me)-C(Me)=NC 6 H 4 Me-2 ( Me DAD) is accompanied by the oxidation of metal atom until trivalent state and results in the formation of paramagnetic compound of metallocenes type (C 9 H 7 ) 2 Yb III ( Me DAD -. ) (3) containing 1,4-diazabutadiene anion-radical. Structure of complex 3 is ascertained by the X-ray structure analysis. Reactions of bisindenyl (1) and bisfluorenyl (C 13 H 9 ) 2 Yb II (THF) 2 (2) derivatives of bivalent ytterbium with 1,4-diazabutadiene PhN=C(Ph)-C(Ph)=NPh ( Ph DAD) (at 1:2 molar ratio of reagents) proceed with the complete break of Yb-C bonds, oxidation of ytterbium atom until trivalent state, and result in the formation of homoligand complex ( Ph DAD -. ) 3 Yb (6) containing three anion-radical 1,4-diazadiene ligands. Complex 6 was also prepared by the exchange reaction of YbCl 3 with Ph DAD -. K + (1:3) in THF. Complex 6 is characterized by the X-ray structure analysis [ru
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Irina A. Golenya
2012-10-01
Full Text Available In the title compound, [Co(C10H8N23][Co(C7H3NO42]2(ClO4·0.5C3H7NO·1.3H2O, the CoIII atom in the complex cation is pseudooctahedrally coordinated by six N atoms of three chelating bipyridine ligands. The CoIII atom in the complex anion is coordinated by two pyridine N atoms and four carboxylate O atoms of two doubly deprotonated pyridine-2,6-dicarboxylate ligands in a distorted octahedral geometry. One dimethylformamide solvent molecule and two water molecules are half-occupied and one water molecule is 0.3-occupied. O—H...O hydrogen bonds link the water molecules, the perchlorate anions and the complex anions. π–π interactions between the pyridine rings of the complex anions are also observed [centroid–centroid distance = 3.804 (3 Å].
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Augusto Rivera
2013-07-01
Full Text Available The title compound, C23H30N2O4, a di-Mannich base derived from 4-methoxyphenol and cis-1,2-diaminecyclohexane, has a perhydrobenzimidazolidine nucleus, in which the cyclohexane ring adopts a chair conformation and the heterocyclic ring has a half-chair conformation with a C—N—C—C torsion angles of −48.14 (15 and −14.57 (16°. The mean plane of the heterocycle makes dihedral angles of 86.29 (6 and 78.92 (6° with the pendant benzene rings. The molecular structure of the title compound shows the presence of two interactions between the N atoms of the imidazolidine ring and the hydroxyl groups through intramolecular O—H...N hydrogen bonds with graph-set motif S(6. The unobserved lone pairs of the N atoms are presumed to be disposed in a syn conformation, being only the second example of an exception to the typical `rabbit-ears' effect in 1,2-diamines.
(Z-N-[3-(4-Bromobenzoyl-1,3-thiazolidin-2-ylidene]cyanamide
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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.
(E-3-Methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone
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Yordanka Ivanova
2016-04-01
Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone, was synthesized by Claisen-Schmidt condensation of 3-methyl-2(3H-benzothiazolone-6-carbaldehyde with 2-acetylthiophene in 94% yield. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.
5-Bromo-N3-[(E-(6-bromopyridin-2-ylmethylidene]pyridine-3,4-diamine
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Mingjian Cai
2011-12-01
Full Text Available The title compound, C11H8Br2N4, is a Schiff base obtained from 6-bromopicolinaldehyde and 5-bromopyridine-3,4-diamine. The molecule has an E configuration about the C=N bond and the dihedral angle between the two pyridine rings is 14.02 (1°. The observed conformation is stabilised by an intramolecular N—H...N hydrogen bond. In the crystal, molecules are stacked along the b axis and are linked through N—H...N hydrogen bonds into chains along the c axis.
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S. Subasri
2017-04-01
Full Text Available The title compounds, C12H12ClN5OS, (I, and C12H12ClN5OS, (II, are 2-[(diaminopyrimidin-2-ylsulfanyl]acetamides. Compound (II, crystallizes with two independent molecules (A and B in the asymmetric unit. In each of the molecules, in both (I and (II, an intramolecular N—H...N hydrogen bond forms an S(7 ring motif. The pyrimidine ring is inclined to the benzene ring by 42.25 (14° in (I, and by 59.70 (16 and 62.18 (15° in molecules A and B, respectively, of compound (II. In the crystal of (I, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(8 ring motif. The dimers are linked via bifurcated N—H...O and C—H...O hydrogen bonds, forming corrugated layers parallel to the ac plane. In the crystal of (II, the A molecules are linked through N—H...O and N—H...Cl hydrogen bonds, forming layers parallel to (100. The B molecules are also linked by N—H...O and N—H...Cl hydrogen bonds, also forming layers parallel to (100. The parallel layers of A and B molecules are linked via N—H...N hydrogen bonds, forming a three-dimensional structure.
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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.
International Nuclear Information System (INIS)
Dammak, T.; Fourati, N.; Boughzala, H.; Mlayah, A.; Abid, Y.
2007-01-01
We have prepared new semiconductor H 3 N(CH 2 ) 6 NH 3 PbBr 4 crystals which are self-assembled organic-inorganic hybrid materials. The grown crystals have been studied by X-ray diffraction, infrared absorption and Raman spectroscopy scattering. We found that the title compound, abbreviated 2C 6 PbBr 4 , crystallizes in a two-dimensional (2D) structure with a P2 1 /a space group. In the inorganic semiconductor sub-lattice, the corner sharing PbBr 6 octahedra form infinite 2D chains. The organic C 6 H 18 N 2 + ions form the insulator barriers between the inorganic semiconductor layers. Such a packing leads to a self-assembled multiple quantum well structure. Raman and infrared spectra of the title compound were recorded in the 50-500 and 400-4000 cm -1 frequency regions, respectively. The assignment of the observed Raman lines was performed by comparison with the homologous compounds. Transmission measurements on thin films of 2C 6 PbBr 4 , obtained by the spin coating method, revealed a strong absorption peak at 380 nm. Luminescence measurements showed an emission line at 402 nm associated with radiative recombinations of excitons confined within the PbBr 6 layers. The electron-hole binding energy is estimated at 180 meV
3-Phenoxymethyl-6-phenyl-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole
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Shaaban K. Mohamed
2016-04-01
Full Text Available In the title compound, C16H12N4OS, the bicyclic triazolothiadiazole core is approximately planar, with an r.m.s. deviation of 0.018 Å. The phenyl rings are inclined to its mean plane by 7.66 (7 and 71.79 (7°. In the crystal, molecules are linked via a C—H...π interaction and a π–π interaction [intercentroid distance = 3.2942 (9 Å] involving inversion-related triazole rings. These interactions result in the formation of chains propagating along [10-1].
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Shahzad Sharif
2012-08-01
Full Text Available The synthesis, structure and some properties of the one-dimensional coordination polymer, [Pr2(pdc3(Hpdc]n·n(H3hp·8n(H2O, (H2pdc = pyridine 2,6-dicarboxylic acid, C7H5NO4; 3hp = 3-hydroxypyridine, C5H5NO are described. One of the Pr3+ ions is coordinated by two O,N,O-tridentate pdc2− ligands and one tridentate Hpdc− anion to generate a fairly regular PrO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The second Pr3+ ion is coordinated by one tridentate pdc2− dianion, four water molecules and two monodentate bridging pdc2− ligands to result in a PrO8N coordination polyhedron that approximates to a mono-capped square-anti-prism. The ligands bridge the metal-atom nodes into a chain, which extends in the [100] direction. The H3hp+ cation and uncoordinated water molecules occupy the inter-chain regions and an N–HLO and numerous O–HLO hydrogen bonds consolidate the structure. The H3hp+ species appears to intercalate between pendant pdc rings to consolidate the polymeric structure. Crystal data: 1 (C33H43N5O29Pr2, Mr = 1255.54, triclinic, (No. 2, Z = 2, a = 13.2567(1 Å, b = 13.6304(2 Å, c = 13.6409(2 Å, α = 89.695(1°, β = 63.049(1°, γ = 86.105(1°, V = 2191.16(5 Å3, R(F = 0.033, wR(F2 = 0.084.
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Lin Li
2008-01-01
Full Text Available The title compound, C30H24N6O2·0.5CH3OH, a glycoluril derivative with two pyridine substituents on the convex face of the glycoluril system, is an important intermediate for the synthesis of more complex glycoluril derivatives. The compound crystallizes with two independent molecules in the asymmetric unit, one of which exhibits disorder of one benzene ring over two orientations with refined site occupancy factors 0.65 (4:0.35 (4. The crystal structure contains several short C—H...O contacts, and the methanol molecule forms an O—H...O hydrogen bond to one of the glycoluril molecules.
N-(4-Fluorophenyl-2,6-dimethyl-1,3-dioxan-4-amine
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Gottimukkala Rambabu
2013-11-01
Full Text Available In the title compound, C12H16FNO2, the dioxane ring adopts a chair conformation with the methyl substituents and the C—N bond in equatorial orientations. Its mean plane subtends a dihedral angle of 40.17 (6° with the benzene ring. In the crystal, weak N—H...F hydrogen bonds link the molecules into C(7 chains propagating in [100].
5-[(E-(2-Hydroxybenzylideneamino]-1H-1,3-benzimidazole-2(3H-thione
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Hoong-Kun Fun
2011-01-01
Full Text Available There are two molecules in the asymmetric unit of the title compound, C14H11N3OS. In each, the benzimidazole ring system is essentially planar, with maximum deviations of 0.010 (2 and 0.006 (2 Å, and makes dihedral angles of 8.70 (9 and 13.75 (8°, respectively, with the hydroxy-substituted benzene rings. Each molecule adopts an E configuration about the central C=N double bond. In the crystal, the two independent molecules are connected via intermolecular N—H...S hydrogen bonds, forming dimers. Furthermore, the dimers are connected by N—H...O hydrogen bonds into molecular ribbons along the c axis. There is an intramolecular O—H...N hydrogen bond in each molecule, which generates an S(6 ring motif.
10-Ethyl-3-(5-methyl-1,3,4-oxadiazol-2-yl-10H-phenothiazine
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Li-Cheng Sun
2012-03-01
Full Text Available In the title compound, C17H15N3OS, the phenothiazine ring system is slightly bent, with a dihedral angle of 13.68 (7° between the benzene rings. The dihedral angle between the oxadiazole ring and the adjacent benzene ring is 7.72 (7°. In the crystal, a π–π interaction with a centroid–centroid distance of 3.752 (2 Å is observed between the benzene rings of neighbouring molecules.
Bis[N,N-bis(1-allyl-1H-benzimidazol-2-ylmethyl-κN3benzylamine-κN]cadmium dipicrate
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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.
t-3-Benzyl-r-2,c-6-diphenylpiperidin-4-one oxime
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R. Arulraj
2016-12-01
Full Text Available In the title compound, C24H24N2O [systematic name: (E-3-benzyl-2,6-diphenylpiperidin-4-one oxime], the piperidine ring adopts a slightly distorted chair conformation and the phenyl rings and the benzyl group substituents are attached equatorially. The oxime group makes a dihedral angle of 42.88 (12° with the piperidine ring. The dihedral angle between the phenyl rings is 71.96 (8°. The benzyl ring makes dihedral angles of 63.01 (8 and 59.35 (8° with the two phenyl rings. In the crystal, molecules are linked by O—H...N hydrogen bonds, forming C(7 chains along the c axis. The chains are linked by C—H...π interactions, forming slabs lying parallel to the bc plane.
Butane-1,4-diammonium bis(pyridine-2,6-dicarboxylato-κ3O2,N,O6cadmate(II dihydrate
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Najmeh Firoozi
2008-10-01
Full Text Available In the title compound, (C4H14N2[Cd(C7H3NO42]·2H2O, the CdII ion is coordinated by four O atoms [Cd—O = 2.2399 (17–2.2493 (17 Å] and two N atoms [Cd—N = 2.3113 (15 and 2.3917 (15 Å] from two tridentate pyridine-2,6-dicarboxylato ligands in a distorted octahedral geometry. The uncoordinated water molecules are involved in O—H...O and N—H...O hydrogen bonds, which contribute to the formation of a three-dimensional supramolecular structure, along with π–π stacking interactions [centroid–centroid distances of 3.5313 (13 and 3.6028 (11 Å between the pyridine rings of neighbouring dianions].
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Li-Qin Zhao
2010-12-01
Full Text Available The title spirooxindole compound, C26H23N3O3, was prepared by the reaction of isatin, 3-methyl-1-phenyl-2-pyrazolin-5-one and 5,5-dimethylcyclohexane-1,3-dione in an ethanol solution. The fused cyclohexene ring adopts an envelope conformation. The dihedral angle between the aromatic and pyrazoline rings is 23.70 (8°. An intramolecular C—H...O interaction occurs. The crystal structure is stabilized by N—H...N hydrogen-bonding interactions, leading to a zigzag chain along the b axis.
4,6-Dibromo-N-{3-[(4,6-dibromo-2,3-dimethylphenylimino]butan-2-ylidene}-2,3-dimethylaniline
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Lina Huang
2013-10-01
Full Text Available The title compound, C20H20Br4N2, is a product of the condensation reaction of 4,6-dibromo-2,3-dimethylaniline and butane-2,3-dione. The molecule has a center of symmetry at the mid-point of the central C—C bond. The dihedral angle between the benzene ring and the 1,4-diazabutadiene plane is 78.3 (2°. Niether hydrogen bonding nor aromatic stacking is observed in the crystal structure.
1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one
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Hualing Zhu
2011-07-01
Full Text Available In the title compound, C21H21N3O2, an intramolecular N—H...O interaction generates an S(6 ring, which stablizes the enamine–keto tautomer. The S(6 ring makes dihedral angles of 33.07 (7, 56.50 (8 and 38.59 (8°, respectively, with the benzoylacetone benzene ring and the antipyrine pyrazole and benzene rings.
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.
Energy Technology Data Exchange (ETDEWEB)
Thabet, Safa, E-mail: safathabet@hotmail.fr [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia); Ayed, Brahim, E-mail: brahimayed@yahoo.fr [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia); Haddad, Amor [Laboratoire de matériaux et cristallochimie, Département de chimie, Institut Supérieur des Sciences Appliquées et Technologier, Avenue El Mourouj, 5111 Mahdia (Tunisia)
2012-11-15
Graphical abstract: Display Omitted Highlights: ► Synthesis of a novel inorganic–organic hybrid compound based on Anderson polyoxomolybdates. ► Characterization by X-ray diffraction, IR and UV–Vis spectroscopies of the new compound. ► Potential applications in catalysis, biochemical analysis and electrical conductivity of the organic–inorganic compound. -- Abstract: A new organic–inorganic hybrid compound based on Anderson polyoxomolybdates, (C{sub 6}H{sub 10}N{sub 3}O{sub 2}){sub 2}Na(H{sub 2}O){sub 2}[Al(OH){sub 6}Mo{sub 6}O{sub 18}]·6H{sub 2}O (1) have been isolated by the conventional solution method and characterized by single-crystal X-ray diffraction, infrared, ultraviolet spectroscopy and Thermogravimetric Analysis (TGA). This compound crystallized in the triclinic system, space group P−1, with a = 94.635(1) Å, b = 10.958(1) Å, c = 11.602(1) Å, α = 67.525(1)°, β = 71.049(1)°, γ = 70.124(1)° and Z = 1. The crystal structures of the compounds exhibit three-dimensional supramolecular assembly based on the extensive hydrogen bonding interactions between organic cations, sodium cations, water molecules and Anderson polyoxoanions. The infrared spectrum fully confirms the X-ray crystal structure and the UV spectrum of the title compound exhibits an absorption peak at 210 nm.
Et2NH2C6H3(CO23SnBr2.4H2O: SYNTHESIS AND INFRARED STUDY
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DAOUDA NDOYE
2014-01-01
Full Text Available The title compound has been obtained on allowing [C6H3(CO23(Et2NH23] to react with SnBr4. The molecular structure of Et2NH2C6H3(CO23SnBr2.4H2O has been determined on the basis of the infrared data. The suggested structure is a dimer in which each tin atom is hexacoordinated by two chelating C6H3(CO233- anions and two Br atoms. Cy2NH2+cations are involved through hydrogen bonds with non-coordinating CO2 groups. The suggested structure is a cage.
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Augusto Rivera
2011-11-01
Full Text Available The title compound, C25H30N2O6, has the imidazolidine ring in an envelope conformation. There are two intramolecular O—H...N hydrogen-bond interactions with graph-set motif S(6. The cyclohexane ring adopts a slightly distorted chair conformation. One methyl carboxylate substituent forms a dihedral angle of 12.00 (5° with the plane of the benzene ring, while the other methyl carboxylate group is almost coplanar, making a dihedral angle of 2.26 (9°. In the crystal, pairs of intermolecular C—H...O hydrogen bonds form racemic dimers, corresponding to an R22(18 graph-set motif. Further weak C—H...O interactions generate a chain running along the c axis.
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Benjamin Sahlmann
2014-04-01
Full Text Available Although the molecular structure of the title compound, C22H32N4O8, displays a twofold symmetry of the molecule including the methoxy and methyl substituents, no crystallographic twofold symmetry is observed in the X-ray structure analysis. The carbonyl O atoms alternately point to different sides of the plane defined by the carbonyl C atoms. Two methoxy groups are oriented inside the molecules cavity. The H atoms of two methyl groups are disordered over two orientations and were refined using a split model.
2,3-Diamino-pyridinium 6-carb-oxy-pyridine-2-carboxyl-ate.
Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein
2011-12-01
The asymmetric unit of the title proton-transfer compound, C(5)H(8)N(3) (+)·C(7)H(4)NO(4) (-), consists of one mono-deprotonated pyridine-2,6-dicarb-oxy-lic acid as anion and one protonated 2,3-diamino-pyridine as cation. The crystal packing shows extensive O-H⋯O, N-H⋯O and N-H⋯N hydrogen bonds. Thre are also several π-π inter-actions between the anions and also between the cations [centriod-centroid distances = 3.6634 (7), 3.7269 (7), 3.6705 (7) and 3.4164 (7) Å].
Nqrs Data for C6H7F4N2OSb (Subst. No. 0879)
Chihara, H.; Nakamura, N.
This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C6H7F4N2OSb (Subst. No. 0879)
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Youngjin Kang
2017-12-01
Full Text Available The asymmetric unit of the title compound, [Ir(C17H11F2N23]·0.5CH3(CH24CH3·0.5CH2Cl2, comprises one IrIII atom, three 2,6-difluoro-3-[5-(2-fluorophenylpyridin-2-yl]pyridin-4-yl ligands and half each of an n-hexane and a dichloromethane solvent molecule located about crystallographic inversion centres. The IrIII atom displays a distorted octahedral coordination geometry, having three C,N-chelating 2,6-difluoro-3-[5-(2-fluorophenylpyridin-2-yl]pyridin-4-yl ligands arranged in a meridional manner. The IrIII ion lies almost in the equatorial plane [deviation = 0.0069 (15 Å]. The average distance [2.041 (3 Å] of Ir—C bonds is slightly shorter than that [2.076 (3 Å] of Ir—N bonds. A variety of intra- and intermolecular C—H...F and C—H...π hydrogen bonds, as well as intermolecular C—F...π interactions, contribute to the stabilization of the molecular and crystal structures, and result in the formation of a two-dimensional network parallel to the ab plane. No interactions between n-hexane solvent molecules and the other components in the title compound are observed.
(E-3-Methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone
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Yordanka Ivanova
2016-09-01
Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone, was synthesized by both an acid- and base-catalyzed aldol condensation of 3-methyl-6-acetyl-2(3H-benzothiazolone and 3,4,5-trimethoxyacetophenone. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.
Gerken, Michael; Dixon, David A; Schrobilgen, Gary J
2002-01-28
The fluoride ion donor properties of OsO(3)F(2) have been investigated. The salts [OsO(3)F][AsF(6)], [OsO(3)F][HF](2)[AsF(6)], mu-F(OsO(3)F)(2)[AsF(6)], [OsO(3)F][HF](2)[SbF(6)], and [OsO(3)F][HF][SbF(6)] have been prepared by reaction of OsO(3)F(2) with AsF(5) and SbF(5) in HF solvent and have been characterized in the solid state by Raman spectroscopy. The single-crystal X-ray diffraction studies of [OsO(3)F][AsF(6)] (P2(1)/n, a = 7.0001(11) A, c = 8.8629(13) A, beta = 92.270(7) degrees, Z = 4, and R(1) = 0.0401 at -126 degrees C), [OsO(3)F][SbF(6)] (P2(1)/c, a = 5.4772(14) A, b = 10.115(3) A, c = 12.234(3) A, beta = 99.321(5) degrees, Z = 4, and R(1) = 0.0325 at -173 degrees C), [OsO(3)F][HF](2)[AsF(6)] (P2(1)/n, a = 5.1491(9) A, b = 8.129(2) A, c = 19.636(7) A, beta = 95.099(7) degrees, Z = 4, and R(1) = 0.0348 at -117 degrees C), and [OsO(3)F][HF][SbF(6)] (Pc, a = 5.244(4) A, b = 9.646(6) A, c = 15.269(10) A, beta = 97.154(13) degrees, Z = 4, and R(1) = 0.0558 at -133 degrees C) have shown that the OsO(3)F(+) cations exhibit strong contacts to the anions and HF solvent molecules giving rise to cyclic, dimeric structures in which the osmium atoms have coordination numbers of 6. The reaction of OsO(3)F(2) with neat SbF(5) yielded [OsO(3)F][Sb(3)F(16)], which has been characterized by (19)F NMR spectroscopy in SbF(5) and SO(2)ClF solvents and by Raman spectroscopy and single-crystal X-ray diffraction in the solid state (P4(1)m, a = 10.076(6) A, c = 7.585(8) A, Z = 2, and R(1) = 0.0858 at -113 degrees C). The weak fluoride ion basicity of the Sb(3)F(16)(-) anion resulted in an OsO(3)F(+) cation (C(3)(v) point symmetry) that is well isolated from the anion and in which the osmium is four-coordinate. The geometrical parameters and vibrational frequencies of OsO(3)F(+), ReO(3)F, mu-F(OsO(3)F)(2)(+), (FO(3)Os--FPnF(5))(2), and (FO(3)Os--(HF)(2)--FPnF(5))(2) (Pn = As, Sb) have been calculated using density functional theory methods.
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Zheng Huang
2015-09-01
Full Text Available We have investigated the thermoelectric properties of the 3C, 2H, 4H, and 6H polytypes of the wide-band-gap(n-type semiconductors SiC, GaN, and ZnO based on first-principles calculations and Boltzmann transport theory. Our results show that the thermoelectric performance increases from 3C to 6H, 4H, and 2H structures with an increase of hexagonality for SiC. However, for GaN and ZnO, their power factors show a very weak dependence on the polytype. Detailed analysis of the thermoelectric properties with respect to temperature and carrier concentration of 4H-SiC, 2H-GaN, and 2H-ZnO shows that the figure of merit of these three compounds increases with temperature, indicating the promising potential applications of these thermoelectric materials at high temperature. The significant difference of the polytype-dependent thermoelectric properties among SiC, GaN, and ZnO might be related to the competition between covalency and ionicity in these semiconductors. Our calculations may provide a new way to enhance the thermoelectric properties of wide-band-gap semiconductors through atomic structure design, especially hexagonality design for SiC.
2-(6-Bromobenzo[d]thiazol-2-yl-5,5-dimethylthiazol-4(5H-one
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Rainer Beckert
2013-12-01
Full Text Available The title compound, C12H9BrN2OS2, was obtained by reacting 6-bromobenzo[d]thiazole-2-carbonitrile in iso-propanol with ethyl 2-mercapto-2-methylpropanoate at reflux temperature for several hours. The resulting dimethyloxyluciferin derivative shows partial double-bond character of the carbon–carbon bond between the two heterocyclic moieties [C—C = 1.461 (3 Å]. This double bond restricts rotation around this C—C axis, therefore leading to an almost planar molecular structure [N—C—C—S torsion angle = 9.7 (3°]. The five-membered thiazoline ring is not completely planar as a result of the bulky S atom [C—S—C—C torsion angle = 5.17 (12°].
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N. Sureshbabu
2013-11-01
Full Text Available In the title compound, C21H23N3O7, the pyrimidinedione ring adopts a screw-boat conformation, whereas the cyclohexenone ring adopts an envelope conformation, with the C atom bearing the methyl groups as the flap atom. The dihedral angle between the mean planes of the pyrimidinedione and cyclohexenone rings is 58.78 (2°. The pyrimidinedione and cyclohexenone rings form dihedral angles of 59.94 (3 and 54.73 (2°, respectively, with the 4-nitrophenyl ring. Relatively strong intramolecular O—H...O hydrogen bonds are observed. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a chain along the c-axis direction.
1-(3-Bromo-6-nitro-1H-indazol-1-ylethan-1-one
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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.
(5S,6R-6-Bromo-6-methyl-5-phenyl-3,4,5,6-tetrahydro-2H-cyclopenta[b]pyran-7-one
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Winai Ieawsuwan
2011-10-01
Full Text Available The title compound, C15H15BrO2, was synthesized by a Brønsted acid-catalysed domino electrocyclization-halogenation reaction. The five-membered ring is essentially planar (r.m.s. deviation 0.006 Å and forms a dihedral angle of 72.7 (3° with the attached phenyl ring. The six-membered heterocycle adopts a half-chair conformation. The crystal packing is stabilized by a C—H...O contact.
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Iwakiri, Takeharu; Ishihara, Hideta; Terao, Hiromitsu; Lork, Enno; Gesing, Thorsten M.
2017-01-01
The crystal structures of [C 2 H 5 NH 3 ] 4 InBr 7 (1), [C(NH 2 ) 3 ] 3 InBr 6 (2), and [H 3 NCH 2 C(CH 3 ) 2 CH 2 NH 3 ]InBr 5 (3) were determined at 100(2) K: monoclinic, P2 1 /n, a=1061.94(3), b=1186.40(4), c=2007.88(7) pm, β= 104.575(1) , Z=4 for 1; monoclinic, C2/c, a=3128.81(12), b=878.42(3), c=2816.50(10) pm, β=92.1320(10) , Z=16 for 2; orthorhombic, P2 1 2 1 2 1 , a=1250.33(5), b=1391.46(6), c=2503.22(9) pm, Z=4 for 3. The structure of 1 contains an isolated octahedral [InBr 6 ] 3- ion and a Br - ion. The structure of 2 contains three different isolated octahedral [InBr 6 ] 3- ions. The structure of 3 has a corner-shared double-octahedral [In 2 Br 11 ] 5- ion and an isolated tetrahedral [InBr 4 ] - ion. The 81 Br nuclear quadrupole resonance (NQR) lines of the terminal Br atoms of the compounds are widely spread in frequency, and some of them show unusual positive temperature dependence. These observations manifest the N-H..Br-In hydrogen bond networks developed between the cations and anions to stabilize the crystal structures. The 81 Br NQR and differential thermal analysis (DTA) measurements have revealed the occurrence of unique phase transitions in 1 and 3. When the bond angles were estimated from the electric field gradient (EFG) directions calculated by the molecular orbital (MO) methods, accurate values were obtained for [InBr 6 ] 3- of 1 and for [In 2 Br 11 ] 5- and [InBr 4 ] - of 3, except for several exceptions in those for the latter two ions. On the other hand, the calculations of 81 Br NQR frequencies have produced up to 1.4 times higher values than the observed ones.
[2,6-Difluoro-3-(pyridin-2-yl-κNpyridin-4-yl-κC4](pentane-2,4-dionato-κ2O,O′iridium(III
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Kaijun Luo
2013-11-01
Full Text Available The title compound, [Ir(C10H5F2N22(C5H7O2], has a distorted octahedral coordination geometry around the IrIII atom, retaining the cis-C,C/trans-N,N chelate disposition in two 2,6-difluoro-3-(pyridin-2-yl-κNpyridin-4-yl ligands which are nearly mutually perpendicular [dihedral angle = 82.75 (15°]. The molecular structure is stabilized by weak C—H...O and C—H...F hydrogen-bond interactions. The crystal structure is stabilized by π–π stacking interactions (centroid–centroid distance = 3.951 Å.
2-[(2-Chlorobenzylideneamino]-4,5,6,7-tetrahydro-1-benzothiophene-3-carbonitrile
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Abdullah M. Asiri
2011-09-01
Full Text Available In the title compound, C16H13ClN2S, the mean planes fitted through all non-H atoms of the heterocyclic five-membered and the benzene rings are oriented at a dihedral angle of 5.19 (7°. In the crystal, a weak C—H...π interaction occurs, along with weak π–π interactions [cenroid–centroid distance = 3.7698 (11 Å].
2,3-Diamino?pyridinium 6-carb?oxy?pyridine-2-carboxyl?ate
Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein
2011-01-01
The asymmetric unit of the title proton-transfer compound, C5H8N3+·C7H4NO4−, consists of one mono-deprotonated pyridine-2,6-dicarboxylic acid as anion and one protonated 2,3-diaminopyridine as cation. The crystal packing shows extensive O—H...O, N—H...O and N—H...N hydrogen bonds. Thre are also several π–π interactions between the anions and also between the cations [centriod–centroid distances = 3.6634&...
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Augusto Rivera
2011-09-01
Full Text Available The title compound, C23H30N2O4, is a Mannich base useful for studying the effect of an electron-donating phenol substituent on intramolecular hydrogen bonding. In the molecular structure, the cyclohexane ring adopts a chair conformation and the five-membered ring has a twisted envelope conformation. Each methoxy group is oriented in the same plane of the respective aromatic ring, showing torsion angles below 11.8 (3° and bond angles between the methoxy group and the aromatic ring of 116.6 (2 and 116.6 (1°. The structure shows interactions between two the N atoms of the heterocyclic ring and the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. In the crystal, C—H...O interactions are observed. The crystal studied was a racemic mixture of RR and SS enantiomers.
3,6-Dibromo-9-(4-tert-butylbenzyl-9H-carbazole
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Duan-Lin Cao
2008-08-01
Full Text Available In the title compound, C23H21Br2N, which was synthesized by the N-alkylation of 1-tert-butyl-4-(chloromethylbenzene with 3,6-dibromo-9H-carbazole, the asymmetric unit contains two unique molecules. Each carbazole ring system is essentially planar, with mean deviations of 0.0077 and 0.0089 Å for the two molecules. The carbazole planes make dihedral angles of 78.9 (2 and 81.8 (2° with the planes of the respective benzene rings.
6-Bromo-1,3-di-2-propynyl-1H-imidazo[4,5-b]pyridin-2(3H-one
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S. Dahmani
2010-04-01
Full Text Available The room-temperature reaction of propargyl bromide and 6-bromo-1,3-dihydroimidazo[4,5-b]pyridin-2-one in dimethylformamide yields the title compound, C12H8BrN3O, which features nitrogen-bound propynyl substituents. The imidazopyridine fused ring is almost planar (r.m.s. deviation = 0.011 Å; the propynyl chains point in opposite directions relative to the fused ring. One acetylenic H atom is hydrogen bonded to the carbonyl O atom of an inversion-related molecule, forming a dimer; adjacent dimers are linked by a second acetylene–pyridine C—H...N interaction, forming a layer motif.
N-(4-Chloro-1,3-benzothiazol-2-yl-2-(3-methylphenylacetamide monohydrate
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H. S. Yathirajan
2011-10-01
Full Text Available In the title compound, C16H13ClN2OS·H2O, the dihedral angle between the mean planes of the benzothiazole ring system and the methylphenyl ring is 79.3 (6°. The crystal packing features intermolecular O—H...N, O—H...O and N—H...O hydrogen bonds involving the water molecule and weak C—H...O, C—H...Cg and π–π stacking interactions [centroid–centroid distances = 3.8743 (7, 3.7229 (7 and 3.7076 (8 Å].
Karthikeyan, Ammasai; Jeeva Jasmine, Nithianantham; Thomas Muthiah, Packianathan; Perdih, Franc
2016-02-01
In the title molecular salt, C12H10N5O(+)·NO3 (-), the adenine unit has an N (9)-protonated N(7)-H tautomeric form with non-protonated N(1) and N(3) atoms. The dihedral angle between the adenine ring system and the phenyl ring is 51.10 (10)°. The typical intra-molecular N(7)-H⋯O hydrogen bond with an S(7) graph-set motif is also present. The benzoyl-adeninium cations also form base pairs through N-H⋯O and C-H⋯N hydrogen bonds involving the Watson-Crick face of the adenine ring and the C and O atoms of the benzoyl ring of an adjacent cation, forming a supra-molecular ribbon with R 2 (2)(9) rings. Benzoyl-adeninum cations are also bridged by one of the oxygen atoms of the nitrate anion, which acts as a double acceptor, forming a pair of N-H⋯O hydrogen bonds to generate a second ribbon motif. These ribbons together with π-π stacking inter-actions between the phenyl ring and the five- and six-membered adenine rings of adjacent mol-ecules generate a three-dimensional supra-molecular architecture.
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T. Anuradha
2014-01-01
Full Text Available In the title compound, C39H38N4O8, the quinoxaline and indene subunits are essentially planar, with maximum deviations of 0.071 (2 and 0.009 (2 Å, respectively. The indenoquinoxaline system forms a dihedral angle of 72.81 (3° with the chromenopyrrolizine system. The two dioxolane rings, as well as the pyran ring of the chromeno group and the terminal pyrrolizine, each adopt an envelope conformation with O and C as flap atoms. The central pyrrolizine ring adopts a twisted conformation. Intramolecular C—H...O and C—H...N hydrogen bonds occur. The crystal structure exhibits C—H...O hydrogen bonds, and is further stablized by C—H...π interactions, forming a two-dimensional network along the bc plane.
7-Diethylamino-2-oxo-2H-chromene-3-carbohydrazide
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Li-Jun Zhang
2011-05-01
Full Text Available The asymmetric unit of the title compound, C14H17N3O3, contains two independent molecules with different conformations of the ethyl groups. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into ribbons extending along the a axis.
Sortais, Jean-Baptiste; Brelot, Lydia; Pfeffer, Michel; Barloy, Laurent
2008-01-01
The title compound, [Ru3(C12H12N)3(CO3)(C6H6)3]PF6·CH2Cl2, was obtained unintentionally as the product of an attempted deprotonation of the monomeric parent ruthenium complex [Ru(C12H12N)(C6H6)(C2H3N)]PF6. The carbonate ligand bridges three half-sandwich cycloruthenated fragments, each of them exhibiting a pseudo-tetrahedral geometry. The configuration of the Ru atoms is S. The naphthyl groups of the enantiopure cycloruthenated benzylic amine ligands point in the same direction, adopting a propeller shape. PMID:21201869
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Shaaban K. Mohamed
2015-12-01
Full Text Available In the title compound, C23H20ClN3O, each of the cyclohexene and 1,4-dihydropyridine rings of the 1,4,5,6,7,8-hexahydroquinoline ring system adopts a twisted-boat conformation. The dihedral angle between the two benzene rings is 11.52 (7°. In the crystal, molecules are linked through a pair of amino–nitrile N—H...N hydrogen bonds, forming inversion dimers. These assemble into a three-dimensional network via C—H...O and C—H...π interactions.
Energy Technology Data Exchange (ETDEWEB)
Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül
2017-12-01
Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-
(E-6-Amino-1,3-dimethyl-5-[(pyridin-2-ylmethylideneamino]pyrimidine-2,4(1H,3H-dione
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Irvin Booysen
2011-09-01
Full Text Available In the title compound, C12H13N5O2, a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å. The N=C bond is E-configured. Intracyclic angles in the pyridine moiety cover the range 117.6 (2–124.1 (2°. Intra- and intermolecular N—H...N and N—H...O hydrogen bonds are observed in the crystal structure, as are intra- and intermolecular C—H...O contacts which, in total, connect the molecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14 Å is between the two different types of six-membered rings.
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Hong Chen
2011-11-01
Full Text Available In the title compound, C30H32N2O7·CH4O, the tetrahydrofuran ring and the six-membered ring fused to it both display envelope conformations, with the ring C atom opposite the carbonyl group and the adjacent bridgehead C atom as the flaps, respectively. In the crystal structure, intermolecular O—H...O hydrogen bonds link all moieties into ribbons along [010]. Weak intermolecular C—H...O interactions consolidate the crystal packing further.
1,4-Dimethyl-3-phenyl-3H-pyrazolo[3,4-c]isoquinolin-5(4H-one
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Giuseppe Daidone
2008-05-01
Full Text Available The title compound, C18H15N3O, is the product of the thermal decomposition of the diazonium salt derived from 2-amino-N-methyl-N-(3-methyl-1-phenyl-1H-pyrazol-5-ylbenzamide. It is characterized by a trans orientation of the methyl groups with respect to the tricyclic ring system. The molecule has a nearly planar phenylpyrazolo[3,4-c]isoquinolin-5-one system, the largest deviation from the mean plane being 0.066 (2 Å for the O atom. The dihedral angle between the phenyl substituent and the heterotricycle is 67 (1°. The packing is stabilized by C—H...N hydrogen-bond interactions, with the formation of molecular chains along the c axis.
4-(2,4-Dichlorophenyl-2-(1H-indol-3-yl-6-methoxypyridine-3,5-dicarbonitrile
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M. N. Ponnuswamy
2008-10-01
Full Text Available In the title compound, C22H12Cl2N4O, the indole ring system and the benzene ring form dihedral angles of 21.18 (7° and 68.43 (8°, respectively, with the pyridine ring. The methoxy group is coplanar with the pyridine ring. In the crystal structure N—H...N intermolecular hydrogen bonds link the molecules into C(10 chains running along [011]. Intramolecular C—H...N hydrogen bonds are also observed.
Bis(2,3,5,6-tetra-2-pyridylpyrazine-κ3N2,N1,N6iron(II bis(dicyanamidate 4.5-hydrate
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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.
Bould, J; Kennedy, J D; Thomas, R L; Rath, N P; Barton, L
2001-11-01
The structural characterization of the osmahexaborane 2-carbonyl-2,2-bis(triphenylphosphine)-nido-2-osmahexaborane(9), [Os(B(5)H(9))(C(18)H(15)P)(2)(CO)], (I), a metallaborane analogue of B(6)H(10), confirms the structure proposed from NMR spectroscopy. The structure of the osmadecaborane 6-carbonyl-6,6-bis(triphenylphosphine)-nido-6-osmadecaborane(13), [Os(B(9)H(13))(C(18)H(15)P)(2)(CO)], (IV), is similarly confirmed. The short basal B-B distance of 1.652 (8) A in (I), not bridged by an H atom, mirrors that in the parent hexaborane(10) [1.626 (4) A].
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Frankie White
2014-09-01
Full Text Available The title compound, [Co(C15H11N3(H2O{Pt(CN4}]n, is a one-dimensional coordination polymer formed under hydrothermal reaction conditions. The CoII site has sixfold coordination with a distorted octahedral geometry, while the PtII ion is coordinated by four cyanide groups in an almost regular square-planar geometry. The compound contains twofold rotation symmetry about its CoII ion, the water molecule and the terpyridine ligand, and the PtII atom resides on an inversion center. trans-Bridging by the tetracyanidoplatinate(II anions links the CoII cations, forming chains parallel to [-101]. Additionally, each CoII atom is coordinated by one water molecule and one tridentate 2,2′:6′,2′′-terpyridine ligand. O—H...N hydrogen-bonding interactions are found between adjacent chains and help to consolidate the crystal packing. In addition, relatively weak π–π stacking interactions exist between the terpyridine ligands of adjacent chains [interplanar distance = 3.464 (7 Å]. No Pt...Pt interactions are observed in the structure.
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Michal Dušek
2010-10-01
Full Text Available Molecules of the the title compound, C21H24Cl2N2O2, are located on a twofold rotation axis, which passes through the C atom linking the two N atoms. Two intramolecular O—H...N hydrogen bonds were observed. In the crystal, non-classical intermolecular C—H...O hydrogen bonds link the molecules into chains along the a axis. The crystal studied was a racemic twin.
(1S,3S,8R,9S,10R-9,10-Epoxy-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodecane
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Abdoullah Bimoussa
2014-04-01
Full Text Available The title compound, C16H26O, was synthesized by treating (1S,3S,8R-3,7,7,10-tetramethyltricyclo[6.4.0.01,3]dodec-9-ene with metachloroperbenzoic acid. The molecule is built up from two fused six- and seven-membered rings. The six-membered ring has a half-chair conformation, whereas the seven-membered ring displays a boat conformation. In the crystal, there are no significant intermolecular interactions present.
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S. Antony Inglebert
2014-05-01
Full Text Available In the title compound, C18H19BrN2O4, the chromene unit is not quite planar (r.m.s. deviation = 0.199 Å, with the methyl C atoms lying 0.027 (4 and 1.929 (4 Å from the mean plane of the chromene unit. The six-membered carbocyclic ring of the chromene moiety adopts an envelope conformation, with the dimethyl-substituted C atom as the flap. The methylamine and nitro groups are slightly twisted from the chromene moiety, with C—N—C—O and O—N—C—C torsion angles of 2.7 (4 and −0.4 (4°, respectively. The dihedral angle between the mean plane of the chromene unit and the benzene ring is 85.61 (13°. An intramolecular N—H...O hydrogen bond generates an S(6 ring motif, which stabilizes the molecular conformation. In the crystal, molecules are linked via N—H...O hydrogen bonds, forming hexagonal rings lying parallel to the ab plane. A region of disordered electron density, most probably disordered ethanol solvent molecules, occupying voids of ca 432 Å3 for an electron count of 158, was treated using the SQUEEZE routine in PLATON [Spek (2009. Acta Cryst. D65, 148–155]. Their formula mass and unit-cell characteristics were not taken into account during refinement.
International Nuclear Information System (INIS)
Larrea, Edurne S.; Mesa, Jose L.; Pizarro, Jose L.; Arriortua, Maria I.; Rojo, Teofilo
2007-01-01
Ni 2 (C 4 H 4 N 2 )(V 4 O 12 )(H 2 O) 2 , 1, and Ni 3 (C 4 H 4 N 2 ) 3 (V 8 O 23 ), 2, have been synthesized using mild hydrothermal conditions at 170 deg. C under autogenous pressure. Both phases crystallize in the P-1 triclinic space group, with the unit-cell parameters, a=7.437(7), b=7.571(3), c=7.564(4) A, α=65.64(4), β=76.09(4), γ=86.25(3) o for 1 and a=8.566(2), b=9.117(2), c=12.619(3) A, α=71.05(2), β=83.48(4), γ=61.32(3) o for 2, being Z=2 for both compounds. The crystal structure of the three-dimensional 1 is constructed from layers linked between them through the pyrazine molecules. The sheets are formed by edge-shared [Ni 2 O 6 (H 2 O) 2 N 2 ] nickel(II) dimers octahedra and rings composed by four [V 4 O 12 ] vanadium(V) tetrahedra linked through vertices. The crystal structure of 2 is formed from vertex shared [VO 4 ] tetrahedra that give rise to twelve member rings. [NiO 4 (C 4 H 4 N 2 ) 2 ] ∞ chains, resulting from [NiO 4 N 2 ] octahedra and pyrazine molecules, give rise to a 3D skeleton when connecting to [VO 4 ] tetrahedra. Diffuse reflectance measurements of 1 indicate a slightly distorted octahedral geometry with values of Dq=880, B=980 and C=2700 cm -1 . Magnetic measurements of 1, carried out in the 5.0-300 K range, indicate the existence of antiferromagnetic couplings with a Neel temperature near to 38 K. - Graphical abstract: Crystal structure of a sheet of Ni 2 (C 4 H 4 N 2 )(V 4 O 12 )(H 2 O) 2
Crystal structure of 4-(4-chlorophenyl-6-(morpholin-4-ylpyridazin-3(2H-one
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Abdullah Aydın
2015-08-01
Full Text Available In the title compound, C14H14ClN3O2, the morpholine ring adopts a chair conformation, with the exocyclic N—C bond in an equatorial orientation. The 1,6-dihydropyridazine ring is essentially planar, with a maximum deviation of 0.014 (1 Å, and forms a dihedral angle of 40.16 (7° with the plane of the benzene ring. In the crystal, pairs of centrosymmetrically related molecules are linked into dimers via N—H...O hydrogen bonds, forming R22(8 ring motifs. The dimers are connected via C—H...O and C—H...Cl hydrogen bonds, forming a three-dimensional network. Aromatic π–π stacking interactions [centroid–centroid distance = 3.6665 (9 Å] are also observed. Semi-empirical molecular orbital calculations were carried out using the AM1 method. The calculated dihedral angles between the pyridizine and benzene rings and between the pyridizine and morpholine (all atoms rings are 34.49 and 76.96°, respectively·The corresponding values obtained from the X-ray structure determination are 40.16 (7 and 12.97 (9°, respectively. The morpholine ring of the title compound in the calculated gas-phase seems to have a quite different orientation compared to that indicated by the X-ray structure determination.
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Salman A. Khan
2010-03-01
Full Text Available The title compound, 5-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione, has been synthesized by condensation of 1,3-diethyl-2-thiobarbituric acid and 3,5-dimethyl-1-phenylpyrazole-4-carbaldehyde in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and EI-MS spectral analysis.
1-Chloro-3-(6-nitro-1H-indazol-1-ylpropan-2-ol
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Mohamed Mokhtar Mohamed Abdelahi
2017-05-01
Full Text Available In the title compound, C10H10ClN3O3, the side chain is oriented nearly perpendicular to the mean plane of the indazole ring system. In the crystal, complementary sets of O—H...N and C—H...O hydrogen bonds form chains of molecules stacked along the a-axis direction
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Peter W. R. Corfield
2016-07-01
Full Text Available In the title compound, {(C6H16NO[Cu2(CN3]}n, the cyanide groups link the CuI atoms into an open three-dimensional anionic network, with the molecular formula Cu2(CN3−. One CuI atom is tetrahedrally bound to four CN groups, and the other CuI atom is bonded to three CN groups in an approximate trigonal-planar coordination. The tetrahedrally coordinated CuI atoms are linked into centrosymmetric dimers by the C atoms of two end-on bridging CN groups which bring the CuI atoms into close contact at 2.5171 (7 Å. Two of the cyanide groups bonded to the CuI atoms with trigonal-planar surrounding link the dimeric units into columns along the a axis, and the third links the columns together to form the network. The N,N-diethylethanolamine molecules used in the synthesis have become protonated at the N atoms and are situated in cavities in the network, providing charge neutrality, with no covalent interactions between the cations and the anionic network.
Koten, G. van; Ploeg, A.F.M.J. van der; Schmitz, J.E.J.; Linden, J.G.M. van der
1982-01-01
The organoplatinum(II) compounds [{2, 6-(Me{2}NCH{2}){2}C{6}H{3}}PtBr] and cis-[(C-N){2}Pt] (C-N = 2-Me{2}NCH{2}C{6}H{4}, 2-Me{2}NC{6}H{4}CH{2}) can be chemically irreversibly oxidized in the potential range 1.00 to 1.35 V vs. an Ag/AgCl electrode, whereas the organoplatinum@?mercury complexes
Jiang, Li-Li; Zuo, Yang; Wang, Zhi-Fang; Tan, Yin; Wu, Qiong-You; Xi, Zhen; Yang, Guang-Fu
2011-06-08
Discovery of protoporphyrinogen oxidase (PPO, EC 1.3.3.4) inhibitors has been one of the hottest research areas in the field of herbicide development for many years. As a continuation of our research work on the development of new PPO-inhibiting herbicides, a series of novel N-(benzothiazol-5-yl)-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-diones (1a-p) and N-(benzothiazol-5-yl)isoindoline-1,3-diones (2a-h) were designed and synthesized according to the ring-closing strategy of two ortho-substituents. The bioassay results indicated that some newly synthesized compounds exhibited higher PPO inhibition activity than the control of sulfentrazone. Compound 1a, S-(5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl) O-methyl carbonothioate, was identified as the most potent inhibitor with k(i) value of 0.08 μM, about 9 times higher than that of sulfentrazone (k(i) = 0.72 μM). Further green house assay showed that compound 1b, methyl 2-((5-(1,3-dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-6-fluorobenzothiazol-2-yl)thio)acetate, exhibited herbicidal activity comparable to that of sulfentrazone even at a concentration of 37.5 g ai/ha. In addition, among six tested crops, wheat exhibited high tolerance to compound 1b even at a dosage of 300 g ai/ha. These results indicated that compound 1b might have the potential to be developed as a new herbicide for weed control of wheat field.
N,N-Dimethyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine monohydrate
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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.
1,3-Diphenyl-3,4-dihydrobenzo[b][1,6]naphthyridine
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Werner Seebacher
2010-05-01
Full Text Available The title compound, C24H18N2, is the first structural example containing the 3,4-dihydrobenzo[b][1,6]naphthyridine fragment. It was synthesized from 2,4,6,8-tetraphenyl-3,7-diazabicyclo[3.3.1]nonan-9-one and was crystallized from a methanol–ethanol solution over two years as a racemate. The C=N double bond [1.2868 (15 Å] is bent significantly out of the plane of the aromatic bicyclic ring system [N—C—C—C = −157.63 (12°] and out of the plane of the phenyl ring bonded at the 1-position [N—C—C—C = 41.15 (16°].
2′-Methyl-2′-nitro-1′-phenyl-2′,3′,5′,6′,7′,7a'-hexahydrospiro[indoline-3,3′-1′H-pyrrolizin]-2-one
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Yaghoub Sarrafi
2008-08-01
Full Text Available The title compound, C21H21N3O3, was synthesized by a multi-component 1,3-dipolar cycloaddition of azomethine ylide, derived from isatin and proline by a decarboxylative route, and (E-1-phenyl-2-nitropropene. In the molecule, the spiro junction links a planar oxindole ring and a pyrrolidine ring in an envelope conformation. The molecular packing is stabilized by an intermolecular N—H...N interaction of the oxindole and pyrrolizidine rings.
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Peter G. Jones
2010-01-01
Full Text Available In the title compound, [Ir(C11H6F2N2(C22H17N4O]·CH3OH, the coordination at iridium is essentially octahedral, but with distortions associated with the bite angles of the ligands [76.25 (9–80.71 (12°] and the differing trans influences of C and N ligands [Ir—N = 2.04 Å (average trans to N but 2.14 Å trans to C]. All three bidentate ligands have coordinating ring systems that are almost coplanar [interplanar angles = 1.7 (1–3.8 (2°]. The vinylbenzyl group is disordered over two positions with occupations of 0.653 (4 and 0.347 (4. The methanol solvent molecule is involved in a classical O—H...N hydrogen bond to a triazole N atom.
Golenya, Irina A.; Boyko, Alexander N.; Kotova, Natalia V.; Haukka, Matti; Iskenderov, Turganbay S.
2012-01-01
In the title compound, [Co(C10H8N2)3][Co(C7H3NO4)2]2(ClO4)·0.5C3H7NO·1.3H2O, the CoIII atom in the complex cation is pseudooctahedrally coordinated by six N atoms of three chelating bipyridine ligands. The CoIII atom in the complex anion is coordinated by two pyridine N atoms and four carboxylate O atoms of two doubly deprotonated pyridine-2,6-dicarboxylate ligands in a distorted octahedral geometry. One dimethylformamide solvent molecule and two water molecules are half-occupied and one water molecule is 0.3-occupied. O—H⋯O hydrogen bonds link the water molecules, the perchlorate anions and the complex anions. π–π interactions between the pyridine rings of the complex anions are also observed [centroid–centroid distance = 3.804 (3) Å]. PMID:23125573
4-Bromo-N-(di-n-propyl-carbamothioyl)-benzamide.
Binzet, Gün; Flörke, Ulrich; Külcü, Nevzat; Arslan, Hakan
2009-02-04
The synthesis of the title compound, C(14)H(19)BrN(2)OS, involves the reaction of 4-bromo-benzoyl chloride with potassium thio-cyanate in acetone followed by condensation of the resulting 4-bromo-benzoyl isothio-cyanate with di-n-propyl-amine. Typical thio-urea carbonyl and thio-carbonyl double bonds, as well as shortened C-N bonds, are observed in the title compound. The short C-N bond lengths in the centre of the mol-ecule reveal the effects of resonance in this part of the mol-ecule. The asymmetric unit of the title compound contains two crystallographically independent mol-ecules, A and B. There is very little difference between the bond lengths and angles of these mol-ecules. In mol-ecule B, one di-n-propyl group is twisted in a -anti-periplanar conformation with C-C-C-H = -179.1 (3)° and the other adopts a -synclinal conformation with C-C-C-H = -56.7 (4)°; in mol-ecule A the two di-n-propyl groups are twisted in + and -anti-periplanar conformations, with C-C-C-H = -179.9 (3) and 178.2 (3)°, respectively. In the crystal, the mol-ecules are linked into dimeric pairs via pairs of N-H⋯S hydrogen bonds.
2,5-Bis[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctylsulfanyl]-1,3,4-thiadiazole
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Gabriel Partl
2017-02-01
Full Text Available The title compound, C18H8F26N2S3, was obtained by double S-perfluorohexylethylation of dipotassium 1,3,4-thiadiazole-2,5-dithiolate in methanol. The molecule exhibits twofold rotational symmetry, with the S atom lying on the rotation axis. The fluorocarbon chains adopt helical conformations and the F atoms of the two terminal C atoms are disordered over two sets of sites. No directional intermolecular interactions occur in the crystal.
International Nuclear Information System (INIS)
Jaitner, P.; Wohlgenannt, W.
1982-01-01
Molybdenum-95 NMR spectra of a series of phosphine and phosphite substituted molybdenum carbonyls Mo(CO)sub(6-n)Lsub(n)n[L = P(OCH 3 ) 3 n = 1,2,3,4,5, L = P(OC 2 H 5 ) 3 n = 1,2,3, L = P(C 6 H 5 ) 3 n = 1] including isomers (cis, trans, fac, mer) are reported. A large range of chemical shifts is found for the title compounds. The coupling constants 1 J( 95 Mo- 31 P) are derived either from 95 Mo-NMR spectra or 31 P-NMR spectra. Syntheses of the measured compounds were performed by thermal or photochemical ligand sustitution. (Author)
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Augusto Rivera
2011-09-01
Full Text Available In the crystal structure of the title compound, C21H24I2N2O2, the two N atoms of the imidazolidine moiety are linked to the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. The cyclohexane ring adopts a chair conformation and the heterocyclic ring to which it is fused has a twisted envelope conformation.
3-Chloro-2-ethyl-6-nitro-2H-indazole
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Mohamed Mokhtar Mohamed Abdelahi
2017-05-01
Full Text Available In the title compound, C9H8ClN3O2, the orientation of the ethyl substituent is partly determined by an intramolecular C—H...Cl hydrogen bond. The indazole moiety is slightly folded with an angle of 0.70 (8° between the five- and six-membered rings. In the crystal, molecules pack in layers parallel to [100] through C—H...π(ring and N...;O...π(ring interactions.
1-Allyl-3-amino-1H-pyrazole-4-carboxylic acid
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Feng-Ling Yang
2008-12-01
Full Text Available The title compound, C7H9N3O2, was prepared by alkaline hydrolysis of ethyl 1-allyl-3-amino-1H-pyrazole-4-carboxylate. The crystal structure is stabilized by three types of intermolecular hydrogen bond (N—H...O, N—H...N and O—H...N.
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Rajamani Raja
2015-09-01
Full Text Available In the title compound, C23H16N2O7, the mean planes of the two chromene units (r.m.s. deviations = 0.031 and 0.064 Å are almost normal to one another with a dihedral angle of 85.59 (6°. The central six-membered pyran ring has a distorted envelope conformation, with the methine C atom at the flap. There is an intramolecular N—H...O hydrogen bond, which generates an S(6 ring motif. In the crystal, molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R22(12 ring motif. The dimers are linked by pairs of C—H...O hydrogen bonds, enclosing R22(6 ring motifs, forming zigzag chains along [001]. The chains are linked by a second pair of C—H...O hydrogen bonds, forming slabs parallel to (110. Within the slabs there are C—H...π interactions present. A region of disordered electron density was treated with the SQUEEZE procedure in PLATON [Spek (2015. Acta Cryst. C71, 9–18] following unsuccessful attempts to model it as plausible solvent molecule(s. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s.
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Robert Swinton Darious
2016-06-01
Full Text Available The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one molecule of N6-benzoyladenine (BA and one half-molecule of adipic acid (AA, the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7°. The N6-benzoyladenine molecule crystallizes in the N(7—H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intramolecular N—H...O hydrogen bonding between the carbonyl (C=O group and the N(7—H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7 ring motif. The two carboxyl groups of adipic acid interact with the Watson–Crick face of the BA molecules through O—H...N and N—H...O hydrogen bonds, generating an R22(8 ring motif. The latter units are linked by N—H...N hydrogen bonds, forming layers parallel to (10-5. A weak C—H...O hydrogen bond is also present, linking adipic acid molecules in neighbouring layers, enclosing R22(10 ring motifs and forming a three-dimensional structure. C=O...π and C—H...π interactions are also present in the structure.
International Nuclear Information System (INIS)
Baba, Shigeo; Kuroki, Michitake; Kasuya, Yasuji; Suzuki, Kenji.
1975-01-01
N-benzoyl-N'-phenyl-2, 6-diaminobenzoic acid (F-1) is a new anti-inflammatory agent. Two isotopically labeled compounds of F-1 ( 3 H-F-1 and 14 C-F-1) were synthesized and their absorption and distribution were investigated in rats and guinea pigs. When 3 H-F-1 was orally administered to rats and guinea pigs, about 20% of the administered radioactivity was excreted in the urine and approximately 70% of it was excreted in the feces during 7 days after 3 H-F-1 administration. A higher concentration of 3 H-F-1 in the blood was observed in rats than in guinea pigs. The maximum blood concentration of 3 H-activity appeared one hour after the oral administration of 3 H-F-1 to rats, while in guinea pigs in appeared three hours later. These facts are in good agreement with the difference in the anti-inflammatory effect between rats and guinea pigs. The highest concentration of 3 H-activity in various organs, such as liver, adrenal, kidney, and lung, was found three hours after the oral administration of 3 H-F-1. (auth.)
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Eyad Mallah
2015-01-01
Full Text Available In the title compound, C10H16N2O9S3, the pyrimidine ring of the 1,3-dimethyl barbituric acid moiety has an envelope conformation with the C atom carrying the methylsulfonyl and bis(methylsulfonylmethyl substituents as the flap. The dihedral angle between mean plane of the pyrimidine ring and the S/C/S plane is 72.4 (3°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure.
International Nuclear Information System (INIS)
Lin Zhien; Fan Wei; Gao Feifei; Chino, Naotaka; Yokoi, Toshiyuki; Okubo, Tatsuya
2006-01-01
A new layered cobalt-zinc phosphite, Co(H 2 O) 4 Zn 4 (HPO 3 ) 6 .C 2 N 2 H 1 has been synthesized in the presence of ethylenediamine as the structure-directing agent. The compound crystallizes in the monoclinic system, space group Cc (No. 9), a=18.2090(8), b=9.9264(7), c=15.4080(7) A, β=114.098(4) o , V=2542.3(2) A 3 , Z=4, R=0.0323, wR=0.0846. The structure consists of ZnO 4 tetrahedra, CoO 6 octahedra and HPO 3 pseudopyramids through their vertices forming bimetallic phosphite layers parallel to the ab plane. Organic cations, which reside between the inorganic layers, are mobile and can be exchanged by NH 4 + cations without the collapse of the framework
Poly[(6-carboxypicolinato-κ3O2,N,O6(μ3-pyridine-2,6-dicarboxylato-κ5O2,N,O6:O2′:O6′dysprosium(III
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Xu Li
2009-11-01
Full Text Available In the title complex, [Dy(C7H3NO4(C7H4NO4]n, one of the ligands is fully deprotonated while the second has lost only one H atom. Each DyIII ion is coordinated by six O atoms and two N atoms from two pyridine-2,6-dicarboxylate and two 6-carboxypicolinate ligands, displaying a bicapped trigonal-prismatic geometry. The average Dy—O bond distance is 2.40 Å, some 0.1Å longer than the corresponding Ho—O distance in the isotypic holmium complex. Adjacent DyIII ions are linked by the pyridine-2,6-dicarboxylate ligands, forming a layer in (100. These layers are further connected by π–π stacking interactions between neighboring pyridyl rings [centroid–centroid distance = 3.827 (3 Å] and C—H...O hydrogen-bonding interactions, assembling a three-dimensional supramolecular network. Within each layer, there are other π–π stacking interactions between neighboring pyridyl rings [centroid–centroid distance = 3.501 (2 Å] and O—H...O and C—H...O hydrogen-bonding interactions, which further stabilize the structure.
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Xiangfeng Chen
2012-02-01
Full Text Available The title compound, C21H26NO4+·Br−, also known as R-methylnaltrexone (MNTX bromide, is a selective peripherally acting μ-opioid receptor antagonist with a oroxymorphone skeleton, synthesized by hydroxyl protection, N-methylation, deprotection and anion exchange of naltrexone. It comprises a five-ring system A/B/C/D/E. Rings C and E adopt distorted chair conformations, whereas ring D is in half-chair conformation. The C/E ring junctions are trans fused. The dihedral angle between rings D and E is 82.3 (1°, while the dihedral angles between the planes of rings C and A, and rings D and E are respectively 81.7 (1, 75.9 (1 and 12.2 (1°. In the crystal, molecules are linked by O—H...Br hydrogen bonds.
(E)-6-Amino-1,3-dimethyl-5-[(pyridin-2-yl-methyl-idene)amino]-pyrimidine-2,4(1H,3H)-dione.
Booysen, Irvin; Hlela, Thulani; Ismail, Muhammed; Gerber, Thomas; Hosten, Eric; Betz, Richard
2011-09-01
In the title compound, C(12)H(13)N(5)O(2), a Schiff-base-derived chelate ligand, the non-aromatic heterocycle and its substituents essentially occupy one common plane (r.m.s. of fitted non-H atoms = 0.0503 Å). The N=C bond is E-configured. Intra-cyclic angles in the pyridine moiety cover the range 117.6 (2)-124.1 (2)°. Intra- and inter-molecular N-H⋯N and N-H⋯O hydrogen bonds are observed in the crystal structure, as are intra- and inter-molecular C-H⋯O contacts which, in total, connect the mol-ecules into a three-dimensional network. The shortest ring-centroid-to-ring-centroid distance of 3.5831 (14) Å is between the two different types of six-membered rings.
Crystal structure of 1-ethylpyrazolo[3,4-d]pyrimidine-4(5H-thione
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Mohammed El Fal
2014-09-01
Full Text Available In the title compound, C7H8N4S, the methyl C atom is displaced by 1.232 (7 Å from the mean plane of the pyrazolo[3,4-d]pyrimidine ring system (r.m.s. deviation = 0.007 Å. The N—N—C—Cm (m = methyl torsion angle is −60.3 (6°. In the crystal, molecules are linked by N—H...S hydrogen bonds, generating [010] chains, which are reinforced by C—H...N interactions. The chains are cross-linked by weak C—H...S hydrogen bonds, generating (001 sheets.
Modelling of phase equilibria in CH4–C2H6–C3H8–nC4H10–NaCl–H2O systems
International Nuclear Information System (INIS)
Li, Jun; Zhang, Zhigang; Luo, Xiaorong; Li, Xiaochun
2015-01-01
Highlights: • A new model was established for the phase equilibria of C1–C2–C3–nC4–brine systems. • The model can reproduce of hydrocarbon–brine equilibria to high T&P and salinity. • The model can well predict H 2 O solubility in light hydrocarbon rich phases. - Abstract: A thermodynamic model is presented for the mutual solubility of CH 4 –C 2 H 6 –C 3 H 8 –nC 4 H 10 –brine systems up to high temperature, pressure and salinity. The Peng–Robinson model is used for non-aqueous phase fugacity calculations, and the Pitzer model is used for aqueous phase activity calculations. The model can accurately reproduce the experimental solubilities of CH 4 , C 2 H 6 , C 3 H 8 and nC 4 H 10 in water or NaCl solutions and H 2 O solubility in the non-aqueous phase. The experimental data of mutual solubility for the CH 4 –brine subsystem are sufficient for temperatures exceeding 250 °C, pressures exceeding 1000 bar and NaCl molalities greater than 6 molal. Compared to the CH 4 –brine system, the mutual solubility data of C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine are not sufficient. Based on the comparison with the experimental data of H 2 O solubility in C 2 H 6 -, C 3 H 8 - or nC 4 H 10 -rich phases, the model has an excellent capability for the prediction of H 2 O solubility in hydrocarbon-rich phases, as these experimental data were not used in the modelling. Predictions of hydrocarbon solubility (at temperatures up to 200 °C, pressures up to 1000 bar and NaCl molalities greater than 6 molal) were made for the C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine systems. The predictions suggest that increasing pressure generally increases the hydrocarbon solubility in water or brine, especially in the lower-pressure region. Increasing temperature usually decreases the hydrocarbon solubility at lower temperatures but increases the hydrocarbon solubility at higher temperatures. Increasing water salinity dramatically decreases
International Nuclear Information System (INIS)
Swigor, J.E.; Algieri, A.A.; Standridge, R.T.; Pittman, K.A.
1985-01-01
The synthesis of the title compound is described. The condensation of 3-aminopropanol with phthalic anhydride and subsequent treatment with phosphorous tribromide produced N-[3-bromopropyl] phthalimide. Acylation with 3-hydroxybenzaldehyde, reduction with hydrogen over Raney nickel and subsequent treatment with thionyl chloride gave N-[3-(3-chloromethylphenoxy) propyl] phthalimide. Treatment with [2,6 - 14 C] piperidine introduced the radiolabel. Deprotection of the amino group with hydrazine and treatment with 3-methoxy-4-amino-3-cyclobutene-1,2-dione produced 1-amino-2-[3-(3-[2,6- 14 C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3, 4-dione. Treatment with hydrochloric acid yielded the title compound in an overall chemical yield of 22%. (author)
6-Methoxy-1-(4-methoxyphenyl-1,2,3,4-tetrahydro-9H-β-carbolin-2-ium acetate
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Mohd Mustaqim Rosli
2012-05-01
Full Text Available In the title compound, C19H21N2O2+·C2H3O2−, the 1H-indole ring system is essentially planar [maximum deviation = 0.0257 (14 Å] and forms a dihedral angle of 87.92 (7 Å with the benzene ring attached to the tetrahydropyridinium fragment. The tetrahydropyridinium ring adopts a half-chair conformation. In the crystal, cations and anions are linked by interionic N—H...O, C—H...O and C—H...N hydrogen bonds into chains along the a axis.
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Gene-Hsiang Lee
2006-06-01
Full Text Available 1-Allyl- (2 and 7-allyl-6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (3 were obtained via the 18-crown-6-ether catalyzed room temperature reactionof 6-amino-3-methyl-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (1 with potassiumcarbonate and allyl bromide in dry acetone. The structures of these two derivatives wereverified by 2D-NMR measurements, including gHSQC and gHMBC measurements. Theminor compound 2 may possess aromatic character. A single crystal X-ray diffractionexperiment indicated that the major compound 3 crystallizes from dimethyl sulfoxide in themonoclinic space group P21/n and its molecular structure includes an attached dimethylsulfoxide molecule, resulting in the molecular formula C10H16N6O2S. Molecular structuresof 3 are linked by extensive intermolecular N-H···N hydrogen bonding [graph set C 1 (7]. 1Each molecule is attached to the dimethyl sulfoxide oxygen via N-H···O intermolecularhydrogen bonding. The structure is further stabilized by À-À stacking interactions.
Ethyl 3-[7-ethoxy-6-(4-methoxybenzenesulfonamido)-2H-indazol-2-yl]propanoate
Abbassi, Najat; Oulemda, Bassou; Rakib, El Mostapha; Geffken, Detlef; Zouihri, Hafid
2012-01-01
In the title compound, C21H25N3O6S, the dihedral angle between the methoxybenzene and indazole rings is 74.96 (5)°. The crystal packing is stabilized by an N—H⋯O hydrogen bond into a two-dimensional network. In addition, C—H⋯π interactions and a π–π contact, with a centroid–centroid distance of 3.5333 (6) Å, are observed. The crystal packing is stabilized by N—H⋯O and C—H⋯O hydrogen bonds. PMID:22589994
2-Benzyl-6-chloro-1-(4-methylphenyl-1H-indole-3-carbonitrile
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Qiao Yan
2011-12-01
Full Text Available In the title compound, C23H17ClN2, the dihedral angle between the indole ring and the attached tolyl ring is 86.97 (8°. Weak C—H...N(nitrile hydrogen bonding, and C—H...π(aromatic and short Cl...π(aromatic [3.628 (1 Å] interactions consolidate the crystal packing.
Density effects on high-n molecular Rydberg states: CH3I and C6H6 in H2 and Ar
International Nuclear Information System (INIS)
Asaf, U.; Felps, W.S.; Rupnik, K.; McGlynn, S.P.; Ascarelli, G.
1989-01-01
The absorption spectra of high-n Rydberg states of methyl iodide and benzene perturbed by varying number densities of hydrogen or argon, range 0.9x10 20 --10.5x10 20 cm -3 for H 2 and 0.6x10 20 --7.5x10 20 cm -3 for Ar, have been investigated. The high-n molecular states of both absorbers were found to shift linearly with the number density of atomic Ar and molecular H 2 scatterers. The Fermi formula modified by the Alekseev--Sobel'man polarization term provides an excellent fit of the shift data. The electron scattering lengths obtained are: 0.93 a 0 for H 2 and -1.63 a 0 for Ar using the CH 3 I absorber; and 0.99 a 0 for H 2 and -1.57 a 0 for Ar using the C 6 H 6 absorber. The electron scattering lengths for H 2 and Ar agree with the results of an empirical model that correlates scattering lengths and the polarizabilities α(spherical) for inert atoms and α 2 (nonspherical) for H 2 molecule
Crystal structure of diquabis (3-hydroxybenzoato-κO)bis(nicotinamide-κN)zinc(II)
International Nuclear Information System (INIS)
Sahin, O.; Buyukgungor, O.; Koese, D. A.; Necefoglu, H.
2010-01-01
The title compound, [Zn(C 7 H 5 O 3 ) 2 (C 6 H 6 N 2 O) 2 (H 2 O) 2 ], is a two-dimensional hydrogen-bonded supramolecular complex. The Zn I I ion resides on the centre of symmetry and is in an octahedral coordination environment comprising two pyridyl N atoms, two carboxylate O atoms and two O atoms from water molecules. Intermolecular N-H...O and O-H...O hydrogen bonds produce R 1 1 (6), R 2 2 (7), R 2 2 (8), R 2 2 (16), R 2 2 (20), R 2 2 (22) and R 3 3 (30) rings which lead to a one-dimensional polymeric chains. An extensive two-dimensional network of N-H...O, O-H...O, C-H...O hydrogen bonds, and C-H...π interactions are responsible for crystal stabilization.
3-Nitrophenol–1,3,5-triazine-2,4,6-triamine (2/1
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V. Sangeetha
2013-06-01
Full Text Available The asymmetric unit of the title compound, C3H6N6·2C6H5NO3, contains one melamine and two 3-nitrophenol molecules. The mean planes of the 3-nitrophenol molecules are almost orthogonal to the plane of melamine, making dihedral angles of 82.77 (4 and 88.36 (5°. In the crystal, molecules are linked via O—H...N, N—H...N and N—H...O hydrogen bonds, forming a three-dimensional network. The crystal also features weak C—H...π and π–π interactions [centroid–centroid distance = 3.9823 (9 Å].
1,3-Dibenzyl-6-bromo-1H-imidazo[4,5-b]pyridin-2(3H-one
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S. Dahmani
2010-04-01
Full Text Available The imidazopyridine fused-ring in the title compound, C20H16BrN3O, is planar (r.m.s. deviation = 0.011 Å. The phenyl rings of the benzyl substitutents twist away from the central five-membered ring in opposite directions; the rings are aligned at 61.3 (1 and 71.2 (1° with respect to this ring.
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Rui Guo
2012-05-01
Full Text Available The title compound, C33H34N4O2S·CH3OH, was prepared as a spirolactam ring formation of rhodamine 6 G dye for comparison with a ring-opened form. The xanthene and spirolactam rings are approximately planar [r.m.s. deviations from planarity = 0.122 (3 and 0.072 (6 Å, respectively]. The dihedral angles formed by the spirolactam and thiophene rings with the xanthene ring system are 89.7 (6 and 86.5 (2°, respectively. The crystal structure features N—H...O and C—H...O hydrogen bonds.
2-(1H-Imidazol-1-yl)-3-isopropyl-1-benzothieno[3,2-d]pyrimidin-4(3H)-one
Xu, Sheng-Zhen
2007-01-01
In the title compound, C16H14N4OS, the three fused rings of the benzothieno[3,2-d]pyrimidinone unit are essentially coplanar, the maximum deviation from the mean plane being 0.067 (3) Å. The dihedral angle between the mean plane of the fused rings and the imidazole ring is 72.00 (3)°. Offset π–π stacking interactions involving the fused rings are effective in the stabilization of the crystal structure. The centroid–centroid distances between t...
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Hossein Aghabozorg
2008-08-01
Full Text Available The reaction of mercury(II chloride dihydrate, propane-1,3-diamine and 4-hydroxypyridine-2,6-dicarboxylic acid in a 1:1:1 molar ratio in aqueous solution, resulted in the formation of the title compound, (C3H12N2[Hg(C7H3NO5Cl(H2O]2·4H2O or (pnH2[Hg(hypydcCl(H2O]2·4H2O (where pn is propane-1,3-diamine and hypydcH2 is 4-hydroxypyridine-2,6-dicarboxylic acid. The metal atom is coordinated by one chloride group, one water molecule cis to the chloride ligand and one (hypydc2− ligand. The coordinated water molecule is almost perpendicular to the plane of the aromatic ring of (hypydc2−. The geometry of the resulting HgClNO3 coordination can be described as distorted square-pyramidal. This structure also contains propane-1,3-diammonium (site symmetry 2 as a counter-ion and four uncoordinated water molecules. There is a wide range of non-covalent interactions consisting of hydrogen bonding [of the types O—H...O, N—H...O and C—H...O, with D...A ranging from 2.548 (5 to 3.393 (6 Å] and ion pairing.
2,3-Diaminopyridinium 6-carboxypyridine-2-carboxylate
Foroughian, Mahsa; Foroumadi, Alireza; Notash, Behrouz; Bruno, Giuseppe; Amiri Rudbari, Hadi; Aghabozorg, Hossein
2011-01-01
The asymmetric unit of the title proton-transfer compound, C5H8N3 +·C7H4NO4 −, consists of one mono-deprotonated pyridine-2,6-dicarboxylic acid as anion and one protonated 2,3-diaminopyridine as cation. The crystal packing shows extensive O—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds. Thre are also several π–π interactions between the anions and also between the cations [centriod–centroid distances = 3.6634 (7), 3.7269 (7), 3.6705 (7) and 3.4164 (7) Å]. PMID:22199823
International Nuclear Information System (INIS)
Nogawa, N.; Morikawa, Naotake; Oohashi, Kunio; Matuoka, H.; Moki, T.; Moriya, T.
1986-01-01
Reactions of recoil tritium with benzoic acid, acetanilide and β-phenethyl alcohol were studied using the 3 He(=n,p) 3 H reaction. The tritium distribution in the aromatic ring is approximately uniform in all the irradiated compounds and the tritium activity per C-H bond in the methyl and ethylene groups is 7 to 8 relative to that of the corresponding ring as standard. These findings are substantially the same as those obtained previously by the 6 Li(n,α) 3 H reactions, suggesting the same mechanism of tritiation for both recoil reactions. The tritiated parent compounds were obtained in high radiochemical yields: 45% for benzoic acid, 30% for acetanilide, 12% for β-phenethyl alcohol. (author)
Hexaaquabis[3,5-bis(hydroxyimino-1-methyl-2,4,6-trioxocyclohexanido-κ2N3,O4]barium tetrahydrate
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Nguyen Dinh Do
2013-11-01
Full Text Available In the title compound, [Ba(C7H5N2O52(H2O6]·4H2O, the Ba2+ cation lies on a twofold rotation axis and is ten-coordinated by two 3,5-bis(hydroxyimino-1-methyl-2,4,6-trioxocyclohexanide oxo O atoms [Ba—O = 2.8715 (17 Å], two hydroxyimino N atoms [Ba—N = 3.036 (2 Å], and six water molecules [Ba—O = 2.847 (2, 2.848 (2, and 2.880 (2 Å]. The 3,5-bis(hydroxyimino-1-methyl-2,4,6-trioxocyclohexanide monoanions act in a bidentate chelating manner, coordinating through an N atom of the non-deprotonated hydroxyimino group and an O atom of the neighboring oxo group. Two lattice water molecules are located in the cavities of the framework and are involved in hydrogen bonding to O atoms of one of the coordinating water molecules and the O atom of a keto group of the ligand. As a result, a three-dimensional network is formed.
Synthesis, spectroscopic, structural and thermal characterizations of [(C7H6NO42TeBr6·4H2O
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S. Smaoui
2018-02-01
Full Text Available Tellurium (IV complexes with pyridine-2,6-dicarboxylate ligand were synthesized by slow evaporation from aqueous solutions yielding a new compound: [(C7H6NO42TeBr6·4H2O]. The structure of this compound was solved and refined by single-crystal X-ray diffraction. The compound is centrosymmetric P21/c (N°: 14 with the parameters a = 8.875(5 Å, b = 15.174(5 Å, c = 10.199(5 Å, β = 94.271° (5 and Z = 2. The structure consists of isolated H2O, isolated [TeBr6]2− octahedral anions and (pyridine-2,6-dicarboxylate [C7H6NO4]+ cations. The stability of the structure was ensured by ionic and hydrogen bonding contacts (N–H⋯Br and O–H⋯Br and Van-Der Walls interaction. The thermal decomposition of the compound was studied by thermogravimetric analysis (TGA and differential scanning calorimetry (DSC. The FTIR and Raman spectroscopy at different temperatures confirm the existence of vibrational modes that correspond to the organic, inorganic and water molecular groups. Additionally, the UV–Vis diffuse reflectance spectrum was recorded in order to investigate the band gap nature. The measurements show that this compound exhibits a semiconducting behavior with an optical band gap of 2.66 eV.
Swinton Darious, Robert; Thomas Muthiah, Packianathan; Perdih, Franc
2016-06-01
The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one mol-ecule of N (6)-benzoyl-adenine (BA) and one half-mol-ecule of adipic acid (AA), the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7)°. The N (6)-benzoyl-adenine mol-ecule crystallizes in the N(7)-H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intra-molecular N-H⋯O hydrogen bonding between the carbonyl (C=O) group and the N(7)-H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7) ring motif. The two carboxyl groups of adipic acid inter-act with the Watson-Crick face of the BA mol-ecules through O-H⋯N and N-H⋯O hydrogen bonds, generating an R 2 (2)(8) ring motif. The latter units are linked by N-H⋯N hydrogen bonds, forming layers parallel to (10-5). A weak C-H⋯O hydrogen bond is also present, linking adipic acid mol-ecules in neighbouring layers, enclosing R (2) 2(10) ring motifs and forming a three-dimensional structure. C=O⋯π and C-H⋯π inter-actions are also present in the structure.
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
6-Chloro-7-fluoro-4-oxo-4H-chromene-3-carbaldehyde
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Yoshinobu Ishikawa
2014-07-01
Full Text Available In the title compound, C10H4ClFO3, a chlorinated and fluorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. = 0.0336 Å for the non-H atoms, with the largest deviation from the least-squares plane [0.062 (2 Å] being for a benzene-ring C atom. In the crystal, molecules are linked through stacking interactions [centroid–centroid distance between the benzene and pyran rings = 3.958 (3 Å and interplanar distance = 3.259 (3 Å], C—H...O hydrogen bonds, and short C...O contacts [2.879 (3 Å]. Unsymmetrical halogen–halogen interactions between the Cl and F atoms [Cl...F = 3.049 (3 Å, C—Cl...F = 148.10 (9° and C—F...Cl = 162.06 (13°] are also formed, giving a meandering two-dimensional network along the a axis.
2-[(2,4,4,6,6-Pentachloro-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinin-2-ylazanidyl]pyridinium
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Safaa A. Ahmed
2012-02-01
Full Text Available The title compound, C5H5Cl5N5P3, crystallizes as a zwitterion in which the pyridine N atom is protonated. An S(6 ring motif is formed via an intramolecular C—H...N hydrogen bond. The triazatriphosphinine ring adopts an envelope conformation, with one N atom displaced by 0.145 (1 Å from the other atoms. In the crystal, N—H...N and C—H...N hydrogen bonds link the molecules into centrosymmetric dimers containing one R22(7 ring motif and two R22(8 ring motifs.
(1R,3R,4R,6S-4-(7-Methoxy-2-oxo-2H-chromen-6-yl-1-methyl-3,6-dioxabicyclo[3.1.0]hexan-2-yl acetate
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Wong Phakhodee
2012-12-01
Full Text Available In the title compound, C17H16O7, which was isolated from the leaves of Micromelum integerrimum, the furan ring adopts an envelope conformation with the O atom as the flap. An intramolecular C—H...O hydrogen bond occurs. The carbonyl O atom is disordered in a 0.57 (8:0.43 (8 ratio. In the crystal, molecules are linked by weak C—H...O hydrogen bonds into a C(10 chain along [010].
International Nuclear Information System (INIS)
Dammak, T.; Elleuch, S.; Bougzhala, H.; Mlayah, A.; Chtourou, R.; Abid, Y.
2009-01-01
An organic-inorganic hybrid perovskite (C 4 H 9 NH 3 ) 4 Pb 3 I 4 Br 6 was synthesized and studied by X-ray diffraction, Raman and infrared spectroscopies, optical transmission and photoluminescence. The title compound, abbreviated (C 4 ) 4 Pb 3 I 4 Br 6 , crystallises in a periodic two-dimensional multilayer structure with P2 1 /a space group. The structure is built up from alternating inorganic and organic layers. Each inorganic layer consists of three sheets of PbX 6 (X=I, Br) octahedra. Raman and infrared spectra of the title compound were recorded in the 100-3500 and 400-4000 cm -1 frequency ranges, respectively. An assignment of the observed vibration modes is reported. Optical transmission measurements, performed on thin films of (C 4 ) 4 Pb 3 I 4 Br 6 , revealed two absorption bands at 474 and 508 nm. Photoluminescence measurements have shown a green emission peak at 519 nm.
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
Bis(1-benzyl-1H-benzimidazole-κN3dichloridozinc
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Rachid Bouhfid
2014-03-01
Full Text Available In the title compound, [ZnCl2(C14H12N22], the ZnII atom exhibits a distorted tetrahedral coordination geometry involving two chloride anions and two N-atom donors from 1-benzyl-1H-benzimidazole ligands. In both ligands, the benzyl and benzimidazole rings are nearly perpendicular [dihedral angles = 81.7 (2 and 81.5 (2°]. The two benzimidazole systems are essentially planar [maximum deviations = 0.015 (3 and 0.020 (2 Å] and form a dihedral angle of 78.09 (8°. In the crystal, centrosymmetrically related molecules are linked by pairs of C—H...Cl hydrogen bonds into chains parallel to the a axis.
Bis(acetylacetonato-κ2O,O′(2-amino-1-methyl-1H-benzimidazole-κN3oxidovanadium(IV
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Zukhra Ch. Kadirova
2009-07-01
Full Text Available The title mixed-ligand oxidovanadium(IV compound, [VO(C5H7O22(C8H9N3], contains a VIV atom in a distorted octahedral coordination, which is typical for such complexes. The vanadyl group and the N-heterocyclic ligand are cis to each other. The coordination bond is located at the endocyclic N atom of the benzimidazole ligand. Intramolecular hydrogen bonds between the exo-NH2 group H atoms and acetylacetonate O atoms stabilize the crystal structure.
4-Hydroxy-6-methyl-3-[3-(thiophen-2-ylacryloyl]-2H-pyran-2-one
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Salima Thabti
2013-04-01
Full Text Available The title compound, C13H10O4S, crystallizes with two molecules in the asymmetric unit in which the rings make dihedral angles of 3.9 (1 and 6.0 (1°; this planarity is due in part to the presence of an intramolecular O—H...O hydrogen bond, which generates an S(6 ring in each molecule. Both molecules represent E isomers with respect to the central C=C bond. In the crystal, molecules are linked by C—H...O interactions into a three-dimensional network.
Corfield, Peter W R; Cleary, Emma; Michalski, Joseph F
2016-07-01
In the title compound, {(C6H16NO)[Cu2(CN)3]} n , the cyanide groups link the Cu(I) atoms into an open three-dimensional anionic network, with the mol-ecular formula Cu2(CN)3 (-). One Cu(I) atom is tetra-hedrally bound to four CN groups, and the other Cu(I) atom is bonded to three CN groups in an approximate trigonal-planar coordination. The tetra-hedrally coordinated Cu(I) atoms are linked into centrosymmetric dimers by the C atoms of two end-on bridging CN groups which bring the Cu(I) atoms into close contact at 2.5171 (7) Å. Two of the cyanide groups bonded to the Cu(I) atoms with trigonal-planar surrounding link the dimeric units into columns along the a axis, and the third links the columns together to form the network. The N,N-di-ethyl-ethano-lamine mol-ecules used in the synthesis have become protonated at the N atoms and are situated in cavities in the network, providing charge neutrality, with no covalent inter-actions between the cations and the anionic network.
Zhou, Bing; Chen, Zhaoqiang; Yang, Yaxi; Ai, Wen; Tang, Huanyu; Wu, Yunxiang; Zhu, Weiliang; Li, Yuanchao
2015-10-05
An unprecedented rhodium(III)-catalyzed regioselective redox-neutral annulation reaction of 1-naphthylamine N-oxides with diazo compounds was developed to afford various biologically important 1H-benzo[g]indolines. This coupling reaction proceeds under mild reaction conditions and does not require external oxidants. The only by-products are dinitrogen and water. More significantly, this reaction represents the first example of dual functiaonalization of unactivated a primary C(sp(3) )H bond and C(sp(2) )H bond with diazocarbonyl compounds. DFT calculations revealed that an intermediate iminium is most likely involved in the catalytic cycle. Moreover, a rhodium(III)-catalyzed coupling of readily available tertiary aniline N-oxides with α-diazomalonates was also developed under external oxidant-free conditions to access various aminomandelic acid derivatives by an O-atom-transfer reaction. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Augusto Rivera
2011-04-01
Full Text Available The cyclohexane ring in the title compound, C21H24Br2N2O2, adopts a chair conformation and the five-membered ring to which it is fused has a twisted envelope conformation. The asymmetric unit contains one half-molecule, which is related to the other half by a twofold rotation axis. The two N atoms of the five-membered ring are linked to the hydroxy groups by intramolecular O—H...N hydrogen bonds. In the crystal, intermolecular C—H...O and C—H...π interactions occur.
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Augusto Rivera
2011-06-01
Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, the two N atoms of the imidazolidine moiety are linked to the hydroxy groups by intramolecular O—H...N hydrogen-bonding interactions. The crystal studied was a racemic mixture of RR and SS enatiomers. The cyclohexane ring adopts a chair conformation and the imidazolidine group to which it is fused has a twisted envelope conformation.
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Uzma Yunus
2008-08-01
Full Text Available The title compound, C5H6N2OS, was synthesized from acetyl chloride and 2-aminothiazole in dry acetone. The asymmetric unit contains two molecules. The crystal structure is stabilized by N—H...N and C—H...O hydrogen bonds.
3-(Aminocarbonylpyridinium diaqua-bis(pyridine-2,6-dicarboxylatobismuthate(III monohydrate
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Janet Soleimannejad
2012-07-01
Full Text Available The asymmetric unit of the ionic title compound, (C6H7N2O[Bi(C7H3NO42(H2O2]·H2O or (acpyH[Bi(pydc2(H2O2]·H2O, contains an [Bi(pydc2(H2O2]− anion (where pydcH2 is pyridine-2,6-dicarboxylic acid, a protonated 3-(aminocarbonylpyridine as counter-ion, (acpyH+, and one uncoordinated water molecule. The anion is an eight-coordinate complex with a square-antiprismatic geometry around the BiIII atom. In the crystal, extensive O—H...O and N—H...O hydrogen bonds, as well as ion pairing, C=O...π interactions [O...centroid distance = 3.583 (5 Å], π–π stacking [centroid–centroid distance = 3.864 (3 Å], and C—H...π and C—H...O interactions, play an important role in the formation and stabilization of the three-dimensional supramolecular structure.
2-(4-Fluoroanilino-3-(2-hydroxyethylquinazolin-4(3H-one
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2009-03-01
Full Text Available The molecular and crystal structures of the title compound, C16H14FN3O2, are stabilized by intramolecular N—H...O and intermolecular O—H...O hydrogen bonds. The existence of non-classical intramolecular C—H...N hydrogen bonds provides a dihedral angle between the fluoro-substituted benzene and pyrimidinone rings of 7.9 (1°.
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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-Hydroxybenzoic acid–purin-6-amine (3/1
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Lian-cai Du
2009-08-01
Full Text Available In the title 3:1 adduct, 3C7H6O3·C5H5N5, an intramolecular O—H...O hydrogen bond occurs in each of the three 2-hydroxybenzoic acid molecules. In the crystal, the components are linked by N—H...O and O—H...N hydrogen bonds.
Pérez, S.; López, C.; Bosque, R.; Solans, X.; Font-Bardía, M.; Roig, A.; Molins, E.; van Leeuwen, P.W.N.M.; van Strijdonck, G.P.F.; Freixa, Z.
2008-01-01
The synthesis, X-ray crystal structures, and the study of the solution behavior of the palladium(II) allyl complexes [Pd(eta(3)-1R(1)-C3H4){FcCH=N-CH2-(CH2)(n)-NMe2}][PF6] {with Fc = (eta(5)-C5H5)Fe(eta(5)-C5H4), R-1 = H, and n = 2 (4) or 1 (5) or R-1 = Ph and n = 2 (6) or 1 (7)} are described. The
Davaasuren, Bambar; Padhy, Harihara; Rothenberger, Alexander
2015-01-01
In the title compound, [FeIr(C5H5)(C20H14N3)Cl3]·2CH3CN, the central IrIII atom is sixfold coordinated by three chloride ligands and three terpyridine N atoms in a slightly distorted octahedral fashion. The terpyridine ligand is functionalized
Energy Technology Data Exchange (ETDEWEB)
Lee, Dong Woo; Jo, Vinna [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of); Ok, Kang Min, E-mail: kmok@cau.ac.kr [Department of Chemistry, Chung-Ang University, Seoul, 156-756 (Korea, Republic of)
2012-10-15
A novel noncentrosymmetric (NCS) gallium-organic framework material, [N(C{sub 3}H{sub 7}){sub 4}]{sub 3}Ga{sub 3}[C{sub 6}H{sub 3}(CO{sub 2}){sub 3}]{sub 4} (CAUMOF-11) has been synthesized by a solvothermal reaction using Ga(NO{sub 3}){sub 3}{center_dot}xH{sub 2}O, 1,3,5-C{sub 6}H{sub 3}(CO{sub 2}H){sub 3}, N(C{sub 3}H{sub 7}){sub 4}Cl, HNO{sub 3}, and HCON(CH{sub 3}){sub 2} at 180 Degree-Sign C. The structure of the reported material has been determined by single-crystal X-ray diffraction. CAUMOF-11 has an anionic three-dimensional framework with aligned four-coordinate GaO{sub 4} tetrahedra and 1,3,5-benzenetricarboxylate groups. Tetrapropylammonim cations reside within the channel and maintain the charge balance. Detailed structural analyses with full characterization including infrared spectroscopy, thermogravimetric analysis, elemental analysis, ion-exchange reactions, topotactic decomposition, and gas adsorption experiments are reported. Powder second-harmonic generating (SHG) measurements on CAUMOF-11, using 1064 nm radiation, exhibit SHG efficiency of 15 times that of {alpha}-SiO{sub 2} and the material is phase-matchable (type-1). - Graphical Abstract: Second-order nonlinear optical measurements on CAUMOF-11 reveal that the material is phase-matchable (type-1) with SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Highlights: Black-Right-Pointing-Pointer A new NCS Ga-organic framework was solvothermally synthesized. Black-Right-Pointing-Pointer CAUMOF-11 exhibits SHG efficiency of 15 times that of {alpha}-SiO{sub 2}. Black-Right-Pointing-Pointer Thermal decomposition of CAUMOF-11 crystal maintains the original morphology.
4-Bromo-N-(di-n-propylcarbamothioylbenzamide
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2009-03-01
Full Text Available The synthesis of the title compound, C14H19BrN2OS, involves the reaction of 4-bromobenzoyl chloride with potassium thiocyanate in acetone followed by condensation of the resulting 4-bromobenzoyl isothiocyanate with di-n-propylamine. Typical thiourea carbonyl and thiocarbonyl double bonds, as well as shortened C—N bonds, are observed in the title compound. The short C—N bond lengths in the centre of the molecule reveal the effects of resonance in this part of the molecule. The asymmetric unit of the title compound contains two crystallographically independent molecules, A and B. There is very little difference between the bond lengths and angles of these molecules. In molecule B, one di-n-propyl group is twisted in a −antiperiplanar conformation with C—C—C—H = −179.1 (3° and the other adopts a −synclinal conformation with C—C—C—H = −56.7 (4°; in molecule A the two di-n-propyl groups are twisted in + and −antiperiplanar conformations, with C—C—C—H = −179.9 (3 and 178.2 (3°, respectively. In the crystal, the molecules are linked into dimeric pairs via pairs of N—H...S hydrogen bonds.
Sortais, Jean-Baptiste; Brelot, Lydia; Pfeffer, Michel; Barloy, Laurent
2008-02-15
The title compound, [Ru(3)(C(12)H(12)N)(3)(CO(3))(C(6)H(6))(3)]PF(6)·CH(2)Cl(2), was obtained unintentionally as the product of an attempted deprotonation of the monomeric parent ruthenium complex [Ru(C(12)H(12)N)(C(6)H(6))(C(2)H(3)N)]PF(6). The carbonate ligand bridges three half-sandwich cyclo-ruthenated fragments, each of them exhibiting a pseudo-tetra-hedral geometry. The configuration of the Ru atoms is S. The naphthyl groups of the enanti-opure cyclo-ruthenated benzylic amine ligands point in the same direction, adopting a propeller shape.
3-Nitro-phenol-1,3,5-triazine-2,4,6-tri-amine (2/1).
Sangeetha, V; Kanagathara, N; Chakkaravarthi, G; Marchewka, M K; Anbalagan, G
2013-06-01
The asymmetric unit of the title compound, C3H6N6·2C6H5NO3, contains one melamine and two 3-nitro-phenol mol-ecules. The mean planes of the 3-nitro-phenol mol-ecules are almost orthogonal to the plane of melamine, making dihedral angles of 82.77 (4) and 88.36 (5)°. In the crystal, mol-ecules are linked via O-H⋯N, N-H⋯N and N-H⋯O hydrogen bonds, forming a three-dimensional network. The crystal also features weak C-H⋯π and π-π inter-actions [centroid-centroid distance = 3.9823 (9) Å].
(Z-3-Benzyl-2-[(2-phenylcyclohex-2-enylimino]-1,3-thiazolidin-4-one
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Chin Wei Ooi
2012-08-01
Full Text Available The title compound, C22H22N2OS, exists in a Z configuration with respect to the N=C bond. The cyclohexene ring adopts a distorted sofa conformation. The thiazolidine ring is essentially planar, with a maximum deviation of 0.030 (2 Å, and forms dihedral angles of 76.66 (6 and 74.55 (6° with the terminal phenyl rings. The dihedral angle between the phenyl rings is 71.55 (7°. In the crystal, a C—H...π interaction is observed.
Bromidotetra?kis?(1H-2-ethyl-5-methyl?imidazole-?N 3)copper(II) bromide
Godlewska, Sylwia; Baranowska, Katarzyna; Socha, Joanna; Do??ga, Anna
2011-01-01
The CuII ion in the title compound, [CuBr(C6H10N2)4]Br, is coordinated in a square-based-pyramidal geometry by the N atoms of four imidazole ligands and a bromide anion in the apical site. Both the CuII and Br− atoms lie on a crystallographic fourfold axis. In the crystal, the [CuBr(C6H10N2)4]+ complex cations are linked to the uncoordinated Br− anions (site symmetry overline{4}) by N—H...Br hydrogen bonds, generating a three-dimensional network. The ethyl group ...
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S. Sathya
2012-02-01
Full Text Available In the title compound, C22H23N3O4, the tolyl ring is almost perpendicular [83.86 (7°] to the best plane through the eight atoms of the pyrrolizidine ring system. The molecular conformation is stabilized by an intramolecular O—H...O hydrogen bond. The crystal packing features inversion dimers with R22(8 motifs linked by pairs of N—H...O hydrogen bonds.
Tricarbonyl[tris(1-methyl-1H-imidazol-2-yl-κN3methanol]manganese(I trifluoromethanesulfonate
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Guido J. Reiss
2012-09-01
Full Text Available In the title compound, [Mn(C13H16N6O(CO3](CF3O3S, the MnI atom has a slightly distorted octahedral geometry. The three CO ligands have C—Mn—C angles in the range 89.44 (10–92.31 (9°, while the three N atoms of the tripodal ligand form significantly smaller N—Mn—N angles of 82.76 (2–85.51 (6°. The three N atoms of the tripodal ligand and the three carbonyl ligands coordinate facially. In the crystal, the trifluoromethanesulfonate counter anion is connected by a medium-strength O—H...O hydrogen bond to the hydroxyl group of the manganese complex.
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Jian-Li Zhang
2010-11-01
Full Text Available The title compound, C16H12F3N3O5S·H2O, was prepared by reaction of 4-nitrobenzaldehyde, 4,4,4-trifluoro-1-(thiophen-2-ylbutane-1,3-dione and urea. The asymmetric unit contains two independent molecules, with essentially identical geometries and conformations. The dihydropyrimidine rings adopt a half-chair conformation. The dihedral angles between the benzene ring and the thiophene ring are 54.82 (8 and 58.72 (8° in the two molecules. The molecular conformation of one of the molecules is stabilized by two intramolecular O—H...O hydrogen bonds, generating an S(6 ring. The crystal structure is stabilized by intermolecular O—H...O and N—H...O hydrogen bonds.
N,N-Diethyl-2-[5-(4-methoxybenzylidene-2,4-dioxo-1,3-thiazolidin-3-yl]acetamide
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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.
1,4-Dihydroxyquinoxaline-2,3(1H,4H-dione
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Wolfgang Frey
2008-03-01
Full Text Available The asymmetric unit of the title compound, C8H6N2O4, contains one half-molecule; a twofold rotation axis bisects the molecule. The quinoxaline ring is planar, which can be attributed to electron delocalization. In the crystal structure, intermolecular O—H...O hydrogen bonds link the molecules into R22(10 motifs, leading to layers, which interact via phenyl–phenyl interactions (C...C distances in the range 3.238–3.521 Å.
(E-4-Hydroxy-6-methyl-3-[1-(2-phenylhydrazinylideneethyl]-2H-pyran-2-one
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Samra Rahmouni
2016-05-01
Full Text Available The title compound, C14H14N2O3, crystallized with three crystallographically independent molecules (A, B and C in the asymmetric unit. The three molecules each have an E conformation about the C=N bond but differ in the orientation of the phenyl and pyran rings. The dihedral angles between the phenyl and pyran ring planes are 14.30 (1, 28.38 (1 and 25.58 (1° in molecules A, B and C, respectively. There is an intramolecular O—H...N hydrogen bond in each molecule with an S(6 ring motif. In the crystal, molecules are linked by N—H...O and C—H...O hydrogen bonds, forming layers parallel to (001, enclosing R22(8 and R33(21 ring motifs. The layers are linked via C—H...π interactions, forming bilayers, which are joined by a further C—H...π interaction, forming a three-dimensional structure.
3-[(R-3,3-Dichloro-2-hydroxypropyl]-8-hydroxy-6-methoxy-1H-isochromen-1-one
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Yong-Cheng Lin
2008-09-01
Full Text Available The title compound, C13H12Cl2O5, is an isocoumarin compound which has been isolated from the ethyl acetate extract of the fermentation broth of actinomycete Streptomyces sp. (V4 from the South China Sea. There are intra- and intermolecular hydrogen bonds and halogen bonds [Cl...Cl = 3.434 (2 Å; C—Cl...Cl = 121.6°]. The intermolecular O—H...O hydrogen bonds link molecules into chains along the b axis.
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Sergey Malinkin
2011-09-01
Full Text Available The title compound, [Cu4(C7H6N2O34(H2O4]·14H2O, a tetranuclear [2 × 2] grid-type complex with S4 symmetry, contains four CuII atoms which are bridged by four pyrazolecarboxylate ligand anions and are additionally bonded to a water molecule. Each CuII atom is coordinated by two O atoms of the carboxylate and acetyl groups, two pyrazole N atoms of doubly deprotonated 3-acetyl-4-methyl-1H-pyrazole-5-carboxylic acid and one O atom of a water molecule. The geometry at each CuII atom is distorted square-pyramidal, with the two N and two O atoms in the equatorial plane and O atoms in the axial positions. O—H...O hydrogen-bonding interactions additionally stabilize the structure. One of the uncoordinated water molecules shows half-occupancy.
4-Bromoanilinium perchlorate 18-crown-6 clathrate
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Min Guo
2010-11-01
Full Text Available The reaction of 4-bromoaniline, 18-crown-6, and perchloric acid in methanol yields the title compound, C6H7BrN+·ClO4−·C12H24O6, in which the protonated –NH3+ group forms three bifurcated N—H...O hydrogen bonds to the O atoms of the crown ether.
International Nuclear Information System (INIS)
Fernandez-Armas, Sergio; Mesa, Jose L.; Pizarro, Jose L.; Chung, U-Chan; Arriortua, Maria I.; Rojo, Teofilo
2005-01-01
The organically templated (C 6 H 16 N 2 ) 0.5 [M(HPO 3 )F] [M(II)=Fe (1) and Co (2)] compounds have been synthesized by using mild hydrothermal conditions under autogeneous pressure. The crystal structures have been determined from X-ray single-crystal diffraction data. The compounds are isostructural and crystallize in the C2/c monoclinic space group. The unit-cell parameters are a=5.607(1), b=21.276(4), c=11.652(1)A, β=93.74(1) deg. for the iron phase and a=5.5822(7), b=21.325(3), c=11.4910(1)A, β=93.464(9) o for the cobalt compound with Z=4. The crystal structure of these compounds consists of [M(HPO 3 )F] - anionic sheets. The layers are constructed from chains which contain [M 2 O 6 F 3 ] dimeric units linked by fluoride ions. The trans-1,4-diaminocyclohexane cations are placed in the interlayer space. The IR and Raman spectra show the bands corresponding to the phosphite oxoanion and organic dication. The Dq and Racah (B and C) parameters have been calculated from the diffuse reflectance spectra in the visible region. Dq parameter is 790cm -1 for compound (1). For phase (2) the Dq value is 725cm -1 and B and C are 930 and 4100cm -1 , respectively. The thermal evolution of the molar magnetic susceptibilities of these compounds show maxima at 20.0 and 6.0K for the iron(II) and cobalt(II) phases, respectively. These results indicate the existence of antiferromagnetic interactions in both compounds
International Nuclear Information System (INIS)
Boyter, H.A. Jr.; Grimes, R.N.
1988-01-01
The preparation and chemistry of nido-2,3-R 2 C 2 C 2 B 4 H 6 carboranes in which R is n-butyl, isopentyl, n-hexyl, and phenyl was investigated in order to further assess the steric and electronic influence of the R groups on the properties of the nido-C 2 B 4 cage, especially with respect to metal complexation at the C 2 B 3 face and metal-promoted oxidative fusion. The three dialkyl derivatives were prepared from the corresponding dialkylacetylenes via reaction with B 5 H 9 and triethylamine, but the diphenyl compound could not be prepared in this manner and was obtained instead in a thermal reaction of B 5 H 9 with diphenylacetylene in the absence of amine. All four carboranes are readily bridge-deprotonated by NaH in THF, and the anions of the dialkyl species, on treatment with FeCl 2 and air oxidation, generate the respective R 4 C 4 B 8 H 8 carborane fusion products were R = n-C 4 H 9 , i-C 5 H 11 or n-C 6 H 13 . The diphenylcarborane anion Ph 2 C 2 B 4 H 5 - did not form detectable metal complexes with Fe 2+ , Co 2+ , or Ni 2+ , and no evidence of a Ph 4 C 4 B 8 H 8 fusion product has been found. Treatment of Ph 2 C 2 B 4 H 6 with Cr(CO) 6 did not lead to metal coordination of the phenyl rings, unlike (PhCH 2 ) 2 C 2 B 4 H 6 , which had previously been shown to form mono- and bis(tricarbonylchromium) complexes. However, the reaction of Ph 2 C 2 B 4 H 5 - , CoCl 2 , and (PhPCH 2 ) 2 did give 1,1-(Ph 2 PCH 2 ) 2 -1-Cl-1,2,3-Co(Ph 2 C 2 B 4 H 4 ), the only case in which metal complexation of the diphenylcarborane was observed. 14 references, 3 figures, 3 tables
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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].
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Augusto Rivera
2011-08-01
Full Text Available In the title compound, C25H32Cl2N2O2, there are two intramolecular O—H... N hydrogen-bonding interactions between the hydroxy groups on the aromatic rings and the two N atoms of the heterocyclic group. The cyclohexane ring adopts a chair conformation and the imidazolidine unit to which it is fused has a twisted envelope conformation. The asymmetric unit comprises one half-molecule which is completed by a twofold rotation axis. A C—H...O interaction is observed in the crystal structure.
catena-Poly[[bis[2-(2,3-dimethylanilinobenzoato-κO]cadmium(II]-di-μ-3-pyridylmethanol-κ2N:O;κ2O:N
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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.
(1S,3R,8S,9R,10S-2,2-Dichloro-3,7,7,10-tetramethyl-9,10-epoxytricyclo[6.4.0.01,3]dodecane
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Moha Berraho
2010-12-01
Full Text Available The title compound, C16H24Cl2O, was synthesized from β-himachalene (3,5,5,9-tetramethyl-2,4a,5,6,7,8-hexahydro-1H-benzocycloheptene, which was isolated from the essential oil of the Atlas cedar (cedrus atlantica. The molecule forms an extended sheet of two fused rings which exhibit different conformations. The six-membered ring has a half-chair conformation, while the seven-membered ring displays a chair conformation; the dihedral angle between the two rings is 38.2 (1°.
Nqrs Data for C3H2Cl10N2PSb[C3HCl4N2P·Cl6HSb](Subst. No. 0601)
Chihara, H.; Nakamura, N.
This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C3H2Cl10N2PSb [C3HCl4N2P·Cl6HSb] (Subst. No. 0601)
4-[(3-Hydroxyanilino(phenylmethylidene]-3-methyl-1-phenyl-1H-pyrazol-5(4H-one
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Keraghel Saida
2012-06-01
Full Text Available In the title compound, C23H19N3O2, the dihedral angles formed by the pyrazolone ring with the three benzene rings are 30.91 (6, 60.96 (4 and 57.01 (4°. The ligand is in the enamine–keto form and its structure is stabilized by an intramolecular N—H...O hydrogen bond. In the crystal, O—H...N hydrogen bonds link molecules into chains parallel to [01-1].
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Shi-Chao Wang
2014-10-01
Full Text Available In the title compound, [Zn(NCS2(C24H22N4O]·C3H7NO, the ZnII cation is N,N′,N′′-chelated by one 2-({4-[2,6-bis(pyridin-2-ylpyridin-4-yl]phenyl}(methylaminoethanol ligand and coordinated by two thiocyanate anions in a distorted N5 trigonal–bipyramidal geometry. In the molecule, the three pyridine rings are approximately coplanar [maximum deviation = 0.026 (5 Å], and the mean plane of the three pyridine rings is twisted to the benzene ring with a small dihedral angle of 5.9 (2°. In the crystal, complex molecules are linked by weak C—H...O hydrogen bonds into supramolecular chains propagated along [110]; π–π stacking is observed between adjacent chains [centroid–centroid distance = 3.678 (4 Å]. The dimethylformamide solvent molecules are linked with the complex chains via weak C—H...O hydrogen bonds.
4-(2,3-Dihydroxybenzylideneamino-3-methyl-1H-1,2,4-triazol-5(4H-one
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Şamil Işık
2009-12-01
Full Text Available All the non-H atoms of the title compound, C10H10N4O3, are almost coplanar, the maximum deviation from planarity being 0.065 (3 Å. The dihedral angle between the aromatic rings is 1.66 (6°. The molecule adopts the enol–imine tautomeric form with an intramolecular hydrogen-bonding interaction between the Schiff base N atom and the hydroxy group. In the crystal, intermolecular N—H...O and O—H...O hydrogen bonds link the molecules into a three-dimensional network.
Mei, Chong-Zhen; Shan, Wen-Wen; Liu, Bing-Tao
2011-10-15
A new 3D metal-organic coordination polymer [Cd(H(3)BPTC)(2)(bpy)](n) (1) (H(4)BPTC = 1,1'-biphenyl-2,2',6,6'-tetracarboxylic acid, bpy =4,4'-bipyridine) has been synthesized and characterized by single X-ray diffraction and IR spectroscopy. The one-dimensional metal-organic chains of the title complex, namely [Cd(H(3)BPTC)(2)](n), are held together through hydrogen bonding and bridging "second" ligand 4,4'-bpy to give a three-dimensional metal-organic network. The thermal stability of complex 1 was studied by thermal gravimetric (TG) and differential thermal analysis (DTA). Compound 1 exhibits photoluminescence with an emission maximum at ca. 380 nm upon excitation at ca. 251 nm. Copyright © 2011 Elsevier B.V. All rights reserved.
Methyl 5,7-dihydroxy-2,2,9-trimethyl-6,11-dioxo-6,11-dihydro-2H-anthra[2,3-b]pyran-8-carboxylate
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Annelise Lobstein
2008-12-01
Full Text Available The title compound, C22H18O7, also known as laurentiquinone B, is a new anthraquinone which was isolated from Vismia laurentii, a Cameroonian medicinal plant. The asymmetric unit contains two independent molecules. Each of them contains four fused rings, three of which are coplanar and typical of anthracene, while the heterocyclic rings adopt envelope conformations. Intramolecular O—H...O hydrogen bonds result in the formation of two planar rings, which are also almost coplanar with the adjacent rings. In the crystal structure, intermolecular O—H...O and C—H...O hydrogen bonds link the molecules and a π–π contact is also present [centroid-centroid distance = 3.967 (3 Å].
4-(2,4-Dichlorophenyl-6-(1H-indol-3-yl-2,2′-bipyridine-5-carbonitrile
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M. N. Ponnuswamy
2009-05-01
Full Text Available The title compound, C25H14Cl2N4, crystallizes with two independent molecules in the asymmetric unit. The two pyridine rings are almost coplanar, making dihedral angles of 3.2 (1 and 8.6 (1° in the two independent molecules. The dichlorophenyl and indole rings are twisted away from the bipyridine ring by 64.32 (5 and 18.46 (4°, respectively in the first molecule and by 51.0 (1 and 27.99 (5°, respectively in the second molecule. The crystal packing is stabilized by C—H...N, C—H...Cl, N—H...N and C—H...π interactions.
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U. H. Patel
2013-06-01
Full Text Available In the title compound, C28H24F6N2O3, the mean plane of the central pyrazoline ring forms dihedral angles of 2.08 (9 and 69.02 (16° with the 2-benzyloxy-6-hydroxy-4-methylphenyl and 3,5-bis(trifluoromethylphenyl rings, respectively. The dihedral angle between the mean planes of the pyrazoline and 3,5-bis(trifluoromethylphenyl rings is 68.97 (9°. An intramolecular O—H...N hydrogen bond is observed, which forms an S(6 graph-set motif. In the crystal, pairs of weak C—H...F halogen interactions link the molecules into inversion dimers while molecular chains along [100] are formed by C—H...O contacts.
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P. L. Nilantha Lakshman
2013-08-01
Full Text Available The title compound, C35H28N4O6S, crystallizes with two molecules in the asymmetric unit. In both molecules, the piperidine ring adopts a shallow-chair conformation, the thiazole ring adopts a twisted conformation about the Cm—N bond (m = methine and the pyrrole ring adopts an envelope conformation with the C atom shared with the thiazole ring as the flap. In the crystal, inversion dimers linked by pairs of C—H...O interactions generate R22(34 loops for one of the asymmetric molecules. Further C—H...O links also involving the other molecule lead to a three-dimesional network. The contribution of the highly disordered solvent to the scattering was removed with SQUEEZE option of PLATON [Spek (2009. Acta Cryst. D65, 148–155]. The solvent contribution is not included in the reported molecular weight and density.
Structuring effects of [Ln6O(OH)8(NO3)6(H2O)12]2+ entities
International Nuclear Information System (INIS)
Guillou, O.; Daiguebonne, C.; Calvez, G.; Le Dret, F.; Car, P.-E.
2008-01-01
In order to obtain highly porous lanthanide-based coordination polymers we are currently investigating reactions between [Ln 6 O(OH) 8 (NO 3 ) 6 (H 2 O) 12 ] 2+ di-cationic hexanuclear entities and sodium salts of benzene-poly-carboxylic acids. Two new coordination polymers obtained during this study are reported here. In both cases, the hexanuclear entity has been destroyed during the reaction. However the resulting compounds are original thanks to a structuring effect of the poly-metallic complex. The first compound of chemical formula [Y 2 (C 8 H 4 O 4 ) 3 (DMF)(H 2 O)],2DMF crystallizes in the monoclinic system, space group P121/n (n o 14) with a = 16.0975(3) A, b = 14.4605(3) A, c = 17.7197(4) A, β = 92.8504(9) o and Z = 4. The second compound of chemical formula Y 2 (NO 3 ) 2 (C 10 H 2 O 8 )(DMF) 4 crystallizes in the triclinic system, space group P-1 (n o 2) with a = 7.5312(3) A, b = 9.0288(3) A, c = 13.1144(6) A, α = 92.6008(14) o , β = 94.9180(14) o , γ = 112.1824(16) o and Z = 2. Both crystal structures are 2D. Both crystal structures are described and the original structural features are highlighted and related to a potential structuring effect of the hexanuclear precursor
International Nuclear Information System (INIS)
Krivovichev, S.V.; Tananaev, I.G.; Myasoedov, B.F.; Kalenberg, V.
2006-01-01
Crystals of new uranyl selenite(IV)-selenate(VI) [C 5 H 14 N][(UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)](H 2 SeO 3 )(HSeO 4 ) are obtained by the method of evaporation from aqueous solutions. Compound has triclinic lattice, space group P1-bar, a=11.7068(9), b=14.8165(12), c=16.9766(15), α=73.899(6), β=76.221(7), γ=89.361(6) Deg, V=2743.0(4) A 3 , Z=2. Laminated complexes (UO 2 ) 3 (SeO 4 ) 4 (HSeO 3 )(H 2 O)] 3- are the basis of the structure. [HSe(VI)O 4 ] - , [H 2 Se(IV)O 3 ] complexes and protonated methylbutylamine cations are disposed between layers [ru
Diaquabis[2,6-bis(4H-1,2,4-triazol-4-ylpyridine-κN2]bis(selenocyanato-κNcobalt(II
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Yuan-Yuan Liu
2012-08-01
Full Text Available In the title compound, [Co(NCSe2(C9H7N72(H2O2], the Co2+ cation is coordinated by two selenocyanate anions, two 2,6-bis(4H-1,2,4-triazol-4-ylpyridine ligands and two water molecules within a slightly distorted N4O2 octahedron. The asymmetric unit consists of one Co2+ cation, which is located on a center of inversion, as well as one selenocyanate anion, one 2,6-bis(4H-1,2,4-triazol-4-ylpyridine ligand and one water molecule in general positions. Intermolecular O—H...N hydrogen bonds join the complex molecules into layers parallel to the bc plane. The layers are linked by C—H...N and C—H...Se hydrogen bonds into a three-dimensional supramolecular architecture.
tert-Butyl 3-(8-bromo-4H,10H-1,2-oxazolo[4,3-c][1]benzoxepin-10-yl-2-methyl-1H-indole-1-carboxylate
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Ankur Trigunait
2010-08-01
Full Text Available In the title compound, C25H23BrN2O4, the seven-membered ring adopts a twisted-boat conformation. The indole ring system is planar within 0.021 (2 Å and the ester group [–C(=O—O—C–] is almost coplanar with it [dihedral angle = 3.0 (2°]. The conformation of the ester group is influenced by intramolecular C—H...O interactions. In the crystal structure, molecules are linked into chains along the b axis by C—H...N hydrogen bonds.
2,4,6-Triamino-1,3,5-triazine-1,3-diium aquapentafluoridoaluminate
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V. Maisonneuve
2008-04-01
Full Text Available The title compound, (C3H8N6[AlF5(H2O], was obtained by solvothermal synthesis from the reaction of aluminium hydroxide, 1,3,5-triazine-2,4,6-triamine (melamine, aqueous HF and water at 323 K for 48 h. The structure consists of [AlF5(H2O]2− octahedra and diprotonated melaminium cations. Cohesion is ensured by a three-dimensional network of hydrogen bonds.
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Yun Wei
2012-04-01
Full Text Available In the title compound, [Co(C18H18N2O4Cl(H2O]·C3H7NO, the CoIII ion is six-coordinated by a tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolate ligand, with a chloride ion and an aqua ligand in the apical positions. The compound crystallized as a dimethylformamide (DMF monosolvate. In the crystal, complex molecules are linked via O—Hwater...O hydrogen bonds to form a dimer-like arrangement. These dimers are linked via a C—H...Cl interaction, and the DMF molecule is linked to the complex molecule by C—H...O interactions.
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Kaijun Luo
2011-11-01
Full Text Available The title compound, [Ir(C11H8N2(C17H19O2], has an octahedral coordination geometry around the IrIII atom, retaining the cis-C,C,trans–N,N chelate disposition of the two 2-phenylpyridine ligands. The chelate rings are nearly mutually perpendicular [the interplanar angles range from 85.48 (17 to 89.17 (19°]. The two 2-(2-pyridylphenyl ligands are approximately planar, with the plane of the phenyl ring being inclined to that of the pyridine ring by 2.3 (3 and 5.1 (3° in the two ligands. The interplanar angle between the phenyl ring in 3-benzoyl-camphor and the IrO2C3 chelate ring is 35.5 (2°.
Energy Technology Data Exchange (ETDEWEB)
Zhang, Li; Li, Chao-Jie; He, Jia-En; Chen, Yin-Yu [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Zheng, Sheng-Run, E-mail: zhengsr@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, Guangzhou, 510006 (China); Fan, Jun [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Zhang, Wei-Guang, E-mail: wgzhang@scnu.edu.cn [School of Chemistry and Environment, South China Normal University, Guangzhou 510006 (China); Guangzhou Key Laboratory of Materials for Energy Conversion and Storage, Guangzhou, 510006 (China)
2016-01-15
Nine new coordination compounds, namely, [Co(HDSPTP){sub 2}(H{sub 2}O){sub 4}]·4H{sub 2}O (H{sub 2}DSPTP=4’-(2,4-disulfophenyl)-3,2’:6’3”-terpyridine, 1 and 2), {[Ni(DSPTP)(H_2O)_4]·3H_2O}{sub n} (3), {[Cu(HDSPTP)_2(H_2O)_3]·8H_2O}{sub n} (4), {[Cu(HDSPTP)_2(H_2O)_3]·6H_2O}{sub n} (5), {[Cu(DSPTP)(H_2O)_2]·H_2O}{sub n} (6), {[Zn(DSPTP)(H_2O)_2]·2H_2O}{sub n} (7), {[Cd(DSPTP)(H_2O)_2]·2H_2O}{sub n} (8), and [Ag{sub 2}(DSPTP)(H{sub 2}O)]{sub n} (9), were constructed based on a new ligand containing both terpyridyl and sulfo groups. The reactions of H{sub 2}DSPTP with Co(NO{sub 3}){sub 2}.6H{sub 2}O resulted in two mononuclear complexes (compounds 1 and 2). They are polymorphisms that display different hydrogen bonding networks. They are selectively synthesized by altering the added alkalis. The reaction of H{sub 2}DSPTP with Ni(NO{sub 3}){sub 2}·6H{sub 2}O resulted in a 1D “S-shaped” coordination chain (compound 3). The reactions of Cu(II) with H{sub 2}DSPTP at different pH value resulted in the following three compounds: two kinds of 1D chains obtained at pH 3.0 and 4.0 for compounds 4 and 5, respectively, and a 3D framework based on binuclear ring units with 4-connected sra topology (Compound 6). The reactions of H{sub 2}DSPTP with ds-block ions resulted in the following three compounds: a Zn(II) (compound 7) and a Cd(II) (compound 8) 3D frameworks with structures similar to that in compound 6, and a 3D framework based on tetranuclear Ag(I) SBUs with binodal (4,8)-connected flu type 3D framework topology. The structural diversity is mainly attributed to the rich coordination modes (from monodentate to µ{sub 7}-mode) and conformations (cis–cis and cis–trans) of HDSPTP{sup −}/DSPTP{sup 2−} ligands and the metal center and can be controllable synthesized by altering the alkalis, and pH value. Thermal stability of all compounds was performed, and the thermal behaviors of compounds 6 and 8 were further explored by PXRD. Compound 6 exhibits
Propane-1,2-diammonium bis(pyridine-2,6-dicarboxylato-κ3O,N,O′nickelate(II tetrahydrate
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Mohammad Ghadermazi
2008-07-01
Full Text Available The reaction of nickel(II nitrate hexahydrate, propane-1,2-diamine and pyridine-2,6-dicarboxylic acid in a 1:2:2 molar ratio in aqueous solution resulted in the formation of the title compound, (C3H12N2[Ni(C7H3NO42]·4H2O or (p-1,2-daH2[Ni(pydc2]·4H2O (where p-1,2-da is propane-1,2-diamine and pydcH2 is pyridine-2,6-dicarboxylic acid. The geometry of the resulting NiN2O4 coordination can be described as distorted octahedral. Considerable C=O...π stacking interactions are observed between the carboxylate C=O groups and the pyridine rings of the (pydc2− fragments, with O...π distances of 3.1563 (12 and 3.2523 (12 Å and C=O...π angles of 95.14 (8 and 94.64 (8°. In the crystal structure, a wide range of non-covalent interactions, consisting of hydrogen bonding [O—H...O, N—H...O and C—H...O, with D...A distances ranging from 2.712 (2 to 3.484 (2 Å], ion pairing, π–π [centroid-to-centroid distance = 3.4825 (8 Å] and C=O...π stacking, connect the various components to form a supramolecular structure.
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Qi Xu
Full Text Available Live attenuated influenza vaccine (LAIV candidates of the H7 subtype, A/Netherlands/219/03 (H7N7, NL03 ca and A/chicken/British Columbia/CN-6/2004 (H7N3, BC04 ca, were evaluated for their receptor binding specificity and immunogenicity in ferrets. The BC04 ca virus exhibited α2,3-SA and α2,6-SA dual receptor binding preference while the NL03 ca virus preferentially bound to α2,3-SA. Substitution of the Q226 and G228 (Q-G by the L226 and S228 (L-S residues in the HA improved binding to α2,6-SA for NL03 ca. The vaccine viruses with L-S retained the attenuation phenotype. NL03 L-S ca replicated more efficiently than the original NL03 ca virus in the upper respiratory tract of ferrets, and induced higher levels of humoral and cellular immune responses. Prior vaccination with seasonal LAIV reduced H7-specific antibody responses, but did not reduce the H7N7 vaccine mediated protection against a heterologous H7N3 BC04 wt virus infection in ferrets. In addition, the H7N3 and H7N7 vaccine immunized ferret sera cross reacted with the newly emerged H7N9 virus. These data, in combination with the safety data from previously conducted Phase 1 studies, suggest that these vaccines may have a role in responding to the threat posed by the H7N9 virus.
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Xuan Liu
2011-08-01
Full Text Available In the title compound, C21H21N3OS·C3H7NO, the carbonitrile molecule is built up of two fused six-membered rings and one six-membered ring linked through a spiro C atom. The 1,3-diaza ring adopts an envelope conformation and the cyclohexane ring adopts a chair conformation. The dihedral angle between the aromatic rings is 46.7 (3°. In the crystal, the components are linked by N—H...O hydrogen bonds.
2-Hydroxy-1,6,7,8-tetramethoxy-3-methylanthraquinone
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Shu-Juan Yu
2008-02-01
Full Text Available The title compound, C19H18O7, also known as chrysoobtusin, was isolated from Cassia tora L. (Leguminosae. The anthraquinone ring system is almost planar, the dihedral angle between the two benzene rings being 4.27 (4°. The structure is stabilized by intra- and intermolecular O—H...O and C—H...O hydrogen bonds, and by weak π–π stacking interactions along the b axis, with a centroid–centroid distance between related benzene rings of 3.800 (4 Å.
(N,N,N′,N′-Tetramethylethylenediamine-κNbis(2,4,6-trimethylphenolato-κOgermanium(II
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Eduard Rusanov
2012-03-01
Full Text Available In the title compound, [Ge(C9H11O2(C6H16N2], the GeII atom is coordinated in a distorted trigonal–pyramidal geometry by two O atoms belonging to two 2,4,6-trimethylphenolate ligands and one N atom of a tetramethylethylenediamine ligand. Comparing the structure with published data of similar compounds shows that the Ge—O bonds are covalent and the Ge—N bond is coordinated.
Dipropyl 3,6-diphenyl-1,2-dihydro-1,2,4,5-tetrazine-1,2-dicarboxylate.
Rao, Guo-Wu; Hu, Wei-Xiao
2003-05-01
The title compound, C(22)H(24)N(4)O(4), was prepared from propyl chloroformate and 3,6-diphenyl-1,2-dihydro-s-tetrazine. This reaction yields the title compound rather than dipropyl 3,6-diphenyl-1,4-dihydro-s-tetrazine-1,4-dicarboxylate. The 2,3-diazabutadiene group in the central six-membered ring is not planar; the C=N double-bond length is 1.285 (2) A, and the average N-N single-bond length is 1.401 (3) A, indicating a lack of conjugation. The ring has a twist conformation, in which adjacent N atoms lie +/- 0.3268 (17) A from the plane of the ring. The molecule has twofold crystallographic symmetry.
International Nuclear Information System (INIS)
Wang Yu; Yu Jihong; Li Yi; Du Yu; Xu Ruren; Ye Ling
2003-01-01
Employing trans-1,4-diaminocyclohexane (trans-1,4-DACH) as a template, a new two-dimensional layered zinc phosphite (C 6 H 16 N 2 )Zn 3 (HPO 3 ) 4 H 2 O (1) has been prepared hydrothermally. Single-crystal X-ray diffraction analysis shows that it crystallizes in the monoclinic space group P2 1 /n with a=10.458(2) A, b=14.720(3) A, c=13.079(3) A, β=97.93(3) deg. , V=1994.1(7) A 3 , Z=4, R 1 =0.0349 (I>2σ(I)) and wR 2 =0.0605 (all data). The inorganic layer is built up by alternation of ZnO 4 tetrahedra and HPO 3 pseudo pyramids forming a 4.6.8-net. The sheet is featured by a series of capped six-membered rings. The diprotonated trans-1,4-DACH molecules reside in the interlayer region and interact with the inorganic network through H-bonds
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Hoong-Kun Fun
2009-11-01
Full Text Available In the title compound, C36H29ClN4O, the dihydropyrazole ring adopts an envelope conformation. The two quinoline ring systems (r.m.s. deviations = 0.029 and 0.018 Å are oriented at a dihedral angle of 71.43 (4°. One of the quinoline rings makes a dihedral angle of 65.40 (7° with the phenyl substituent. In the crystal, molecules are linked into chains along the b axis by intermolecular C—H...N hydrogen bonds. In addition, C—H...π and π–π [centroid–centroid distance = 3.7325 (8 Å] interactions are observed.
N-(2,6-Dimethylphenylsuccinamic acid
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2009-03-01
Full Text Available In the amide segment of the title compound, C12H15NO3 {systematic name: 3-[(2,6-dimethylphenylaminocarbonyl]propionic acid}, the N—H and C=O bonds are anti to each other. The molecules are packed into a two-dimensional array via N—H...O and O—H...O hydrogen bonds.
5,7,12,14-Tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-diol dimethylformamide disolvate
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Mohammad Nozari
2016-07-01
Full Text Available The crystal lattice of the title compound, C34H22O2·2C3H7NO, at 173 K has monoclinic (P21/n symmetry. Molecules are located on crystallographic centers of symmetry and have approximate non-crystallographic mmm symmetry, indicating that in solution the chemical and spectroscopic behavior would be that of a D2h molecule. The compound has applications in gas-separation membranes fabricated from polymers of intrinsic microporosity (PIM. The compound is the product of reduction of the corresponding quinone by Na2S2O4 in DMF/NaHCO3.
5-(2,5-Dioxooxolan-3-yl-8-methyl-3,3a,4,5-tetrahydro-1H-naphtho[1,2-c]furan-1,3-dione
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Y. Z. Guo
2013-02-01
Full Text Available In the title compound, C17H14O6, the dihedral angle between the two anhydride rings is 76.01 (8°while the dihedral angles between the benzene and anhydride rings are 42.60 (7 and 68.94 (7°. The cyclohexene ring of the tetrahydronaphthalene unit exhibits an envelope conformation.
Crystal structure of 1,3-bis(2,3-dimethylquinoxalin-6-ylbenzene
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Charles E. Diesendruck
2015-12-01
Full Text Available The title compound, C26H22N4 (I, was synthesized by C—H iridium-catalyzed borylation followed by Suzuki coupling. The molecular structure of (I consists of a central benzene ring with 3-dimethylquinoxalin-6-yl groups at the 1 and 3 positions. These 2,3-dimethylquinoxalin-6-yl groups twist significantly out of the plane of the benzene ring. There are intermolecular π–π interactions which result in a two-dimensional extended structure. The layers extend parallel to the ab plane and stack along the c axis.
2-Methyl-3-(2-methylphenyl-7-nitroquinazolin-4(3H-one
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Edward R. T. Tiekink
2012-03-01
Full Text Available In the title methaqualone analogue, C16H13N3O3, the 2-tolyl group is almost orthogonal [dihedral angle = 85.20 (5°] to the fused ring system (r.m.s. deviation of fitted non-H atoms = 0.029 Å. In the crystal, twofold symmetry generates two-molecule aggregates linked by C—H...O and π–π interactions [ring centroid–centroid distance = 3.4967 (6 Å].
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Shan Gao
2012-12-01
Full Text Available In the centrosymmetric dinuclear title AgI compound, [Ag2(C6H6N2O4](NO32, the aromatic amine-coordinated AgI atom is further bridged by two hydroxylamine molecules that use aromatic and oxime N atoms for bridging, and it exists in a distorted trigonal-planar geometry. In the crystal, the nitrate anions link to the dinuclear compound molecules via O—H...O hydrogen bonds, generating a chain running along the a-axis direction.
Bis(1H-imidazole-κN3bis(1-naphthaleneacetato-κ2O,O′cadmium(II
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Hong-Mian Wu
2008-05-01
Full Text Available In the mononuclear title compound, [Cd(C12H9O22(C3H4N22], the CdII centre has a distorted octahedral coordination geometry defined by four O atoms from two naphthaleneacetate ligands and two N atoms from two imidazole ligands. The molecules are linked by N—H...O hydrogen bonds, forming a layer network.
(E-3-[5-(Diphenylaminothiophen-2-yl]-1-(pyridin-3-ylprop-2-en-1-one
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Rui Li
2013-09-01
Full Text Available In the title compound, C24H18N2OS, the pyridine and the two phenyl rings are oriented at dihedral angles of 10.1 (5, 71.7 (6 and 68.7 (5°, respectively, to the central thiophene ring. In the crystal, pairs of weak C—H...O hydrogen bonds link inversion-related molecules, forming dimers. The dimers are linked by further weak C—H...O hydrogen bonds, forming chains running along the a-axis direction.
Study on the Alkylation Reactions of N(7)-Unsubstituted 1,3-Diazaoxindoles.
Kókai, Eszter; Halász, Judit; Dancsó, András; Nagy, József; Simig, Gyula; Volk, Balázs
2017-05-19
The chemistry of the 5,7-dihydro-6 H -pyrrolo[2,3- d ]pyrimidin-6-one (1,3-diazaoxindole) compound family, possessing a drug-like scaffold, is unexplored. In this study, the alkylation reactions of N (7)-unsubstituted 5-isopropyl-1,3-diazaoxindoles bearing various substituents at the C (2) position have been investigated. The starting compounds were synthesized from the C (5)-unsubstituted parent compounds by condensation with acetone and subsequent catalytic reduction of the 5-isopropylidene moiety. Alkylation of the thus obtained 5-isopropyl derivatives with methyl iodide or benzyl bromide in the presence of a large excess of sodium hydroxide led to 5,7-disubstituted derivatives. Use of butyllithium as the base rendered alkylation in the C (5) position possible with reasonable selectivity, without affecting the N (7) atom. During the study on the alkylation reactions, some interesting by-products were also isolated and characterized.
Synthesis and reactions of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one
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NAGWA M.S. EL-DIN HARB
1999-11-01
Full Text Available The condensation of 4-(p-methoxybenzyl-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazin-3(2H-one (3, prepared by the reaction of 6-[5,6,7,8-tetrahydro-2-naphthyl]-4,5-dihydropyridazin-3(2H-one (1 and anisaldehyde, with dimethyl sulphate, formaldehyde and acrylonitrile, and also the formation of the Mannich base, proceeded smoothly at the 2-position to give compounds 4,5,6,7, respectively. 4-p-Methoxybenzyl-3-chloro-6-[5,6,7,8-tetrahydro-2-naphthyl]-pyridazine (9 was prepared in law yield by the action of phosphorus oxychloride on 3. The reaction of 9 with benzylamine, aniline and piperidine gave 10a,b,c, respectively. 4-p-Methoxybenzyl-6-[5,6,7,8-tetrahydro-2-napthyl]pyridazine-3(2H-thione (12 was prepared either by the action of thiourea on 9, or by the reaction of 3 with phosphorus pentasulphide. The reaction of these thiones with acrylonitrile, morpholine and piperidine to give 13 and 14 a,b, respectively, were also investigated.
Arslan, N. Burcu; Kazak, Canan; Aydın, Fatma
2012-04-01
The title molecule (C19H17N5O4S·H2O) was synthesized and characterized by IR-NMR spectroscopy, MS and single-crystal X-ray diffraction. The molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the compound in the ground state have been calculated by using the density functional theory (DFT) method with 6-31G(d) basis set, and compared with the experimental data. All the assignments of the theoretical frequencies were performed by potential energy distributions using VEDA 4 program. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and 1H and 13C NMR chemical shift values show good agreement with experimental data. To determine conformational flexibility, the molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which was varied from -180° to +180° in steps of 10°. Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and thermodynamic properties of the compound were investigated by theoretical calculations.
Energy Technology Data Exchange (ETDEWEB)
Iwakiri, Takeharu; Ishihara, Hideta [Saga Univ. (Japan). Faculty of Culture and Education; Terao, Hiromitsu [Tokushima Univ. (Japan). Faculty of Integrated Arts and Sciences; Lork, Enno; Gesing, Thorsten M. [Bremen Univ. (Germany). Inst. of Inorganic Chemistry and Crystallography
2017-03-01
The crystal structures of [C{sub 2}H{sub 5}NH{sub 3}]{sub 4}InBr{sub 7}(1), [C(NH{sub 2}){sub 3}]{sub 3}InBr{sub 6}(2), and [H{sub 3}NCH{sub 2}C(CH{sub 3}){sub 2}CH{sub 2}NH{sub 3}]InBr{sub 5}(3) were determined at 100(2) K: monoclinic, P2{sub 1}/n, a=1061.94(3), b=1186.40(4), c=2007.88(7) pm, β= 104.575(1) , Z=4 for 1; monoclinic, C2/c, a=3128.81(12), b=878.42(3), c=2816.50(10) pm, β=92.1320(10) , Z=16 for 2; orthorhombic, P2{sub 1}2{sub 1}2{sub 1}, a=1250.33(5), b=1391.46(6), c=2503.22(9) pm, Z=4 for 3. The structure of 1 contains an isolated octahedral [InBr{sub 6}]{sup 3-} ion and a Br{sup -} ion. The structure of 2 contains three different isolated octahedral [InBr{sub 6}]{sup 3-} ions. The structure of 3 has a corner-shared double-octahedral [In{sub 2}Br{sub 11}]{sup 5-} ion and an isolated tetrahedral [InBr{sub 4}]{sup -} ion. The {sup 81}Br nuclear quadrupole resonance (NQR) lines of the terminal Br atoms of the compounds are widely spread in frequency, and some of them show unusual positive temperature dependence. These observations manifest the N-H..Br-In hydrogen bond networks developed between the cations and anions to stabilize the crystal structures. The {sup 81}Br NQR and differential thermal analysis (DTA) measurements have revealed the occurrence of unique phase transitions in 1 and 3. When the bond angles were estimated from the electric field gradient (EFG) directions calculated by the molecular orbital (MO) methods, accurate values were obtained for [InBr{sub 6}]{sup 3-} of 1 and for [In{sub 2}Br{sub 11}]{sup 5-} and [InBr{sub 4}]{sup -} of 3, except for several exceptions in those for the latter two ions. On the other hand, the calculations of {sup 81}Br NQR frequencies have produced up to 1.4 times higher values than the observed ones.
6-Bromo-2-(4-chlorophenyl-3-methyl-3H-imidazo[4,5-b]pyridine
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Selma Bourichi
2016-05-01
Full Text Available In the title compound, C13H9BrClN3, the imidazopyridine fused-ring system is almost planar, with r.m.s. deviation of 0.006 (19 Å, and makes a dihedral angle of 29.32 (8° with the mean plane of the 4-chlorophenyl group. In the crystal, C—H...N hydrogen bonds link the molecules into chains propagating in the [100] direction. Weak intermolecular π–π interactions between the five- and six-membered rings of the 3H-imidazo[4,5-b]pyridine moieties of neighbouring molecules [centroid–centroid distance = 3.8648 (12 Å] further consolidate the packing into layers parallel to the ab plane.
Hexakis(1-methyl-1H-imidazole-κN3cobalt(II dibromide dihydrate
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Rufu Yao
2009-02-01
Full Text Available The asymmetric unit of the title compound, [Co(C4H6N26]Br2·2H2O, contains one-half of the centrosymmetric cation, one Br atom and one water molecule. The CoII atom, lying on an inversion center, has a distorted octahedral geometry, defined by six N atoms from six 1-methylimidazole ligands. In the crystal structure, intra- and intermolecular O—H...Br hydrogen bonds link pairs of uncoordinated water molecules and bromide anions.
Systems Li2B4O7 (Na2B4O7, K2B4O7)-N2H3H4OH-H2O at 25 deg C
International Nuclear Information System (INIS)
Skvortsov, V.G.; Sadetdinov, Sh.V.; Akimov, V.M.; Mitrasov, Yu.N.; Petrova, O.V.; Klopov, Yu.N.
1994-01-01
Phase equilibriums in the Li 2 B 4 O 7 (Na 2 B 4 O 7 , K 2 B 4 O 7 )-N 2 H 3 H 4 OH-H 2 O systems were investigated by methods of isothermal solubility, refractometry and PH-metry at 25 deg C for the first time. Lithium and sodium tetraborates was established to form phases of changed composition mM 2 B 4 O 7 ·nN 2 H 3 C 2 H 4 OH·XH 2 O, where M=Li, Na with hydrazine ethanol. K 2 B 4 O 7 ·4H 2 O precipitates in solid phase in the case of potassium salt. Formation of isomorphous mixtures was supported by X-ray diffraction and IR spectroscopy methods
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Maxim V. Borzov
2009-05-01
Full Text Available In the title compound, [Li(C27H23N2(C4H10O], the Li atom possesses a nearly planar trigonal coordination environment (assuming the cyclopentadienyl ring of the indenyl group occupies one coordination place. The diethyl ether ligand adopts a nearly planar W-type conformation.
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Goverdhan Mehta
2012-12-01
Full Text Available The title compound, C17H24O5, featuring a 2-carbethoxy-3-oxepanone unit in its intramolecularly O—H...O hydrogen-bonded enol form, was obtained via [(CF3CO22Rh]2-catalysed intramolecular O—H bond insertion in the α-diazo-ω-hydroxy-β-ketoester, ethyl 4-[(1S,3aS,6R,6aS-6-hydroxy-2,2,3a-trimethyl-3-oxo-octahydropentalen-1-yl]-2-diazo-3-oxobutanoate. The seven-membered oxacyclic ring, thus constructed on a cis-fused diquinane platform, was found to adopt a distorted boat–sofa conformation.
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Concepción López
2014-11-01
Full Text Available The study of the reactivity of the enantiopure ferrocenyl Schiff base (SC-[FcCH=N–CH(Me(C6H5] (1 (Fc = (η5-C5H5Fe(η5-C5H4 with cis-[PtCl2(dmso2] under different experimental conditions is reported. Four different types of chiral Pt(II have been isolated and characterized. One of them is the enantiomerically pure trans-(SC-[Pt{κ1-N[FcCH=N–CH(Me(C6H5]}Cl2(dmso] (2a in which the imine acts as a neutral N-donor ligand; while the other three are the cycloplatinated complexes: [Pt{κ2-C,N [(C6H4–N=CHFc]}Cl(dmso] (7a and the two diastereomers {(Sp,SC and (Rp,SC} of [Pt{κ2-C,N[(η5-C5H3–CH=N–{CH(Me(C6H5}]Fe(η5-C5H5}Cl(dmso] (8a and 9a, respectively. Isomers 7a-9a, differ in the nature of the metallated carbon atom [CPh (in 7a or CFc (in 8a and 9a] or the planar chirality of the 1,2-disubstituted ferrocenyl unit (8a and 9a. Reactions of 7a–9a with PPh3 gave [Pt{κ2-C,N[(C6H4–N=CHFc]}Cl(PPh3] (in 7b and the diastereomers (Sp,SC and (Rp,SC of [Pt{κ2-C,N[(η5-C5H3–CH=N–{CH(Me(C6H5}] Fe(η5-C5H5}Cl(PPh3] (8b and 9b, respectively. Comparative studies of the electrochemical properties and cytotoxic activities on MCF7 and MDA-MB231 breast cancer cell lines of 2a and cycloplatinated complexes 7b-9b are also reported. Theoretical studies based on DFT calculations have also been carried out in order to rationalize the results obtained from the cycloplatination of 1, the stability of the Pt(II complexes and their electrochemical properties.
Cocrystals of 6-propyl-2-thiouracil: N-H···O versus N-H···S hydrogen bonds.
Tutughamiarso, Maya; Egert, Ernst
2011-11-01
In order to investigate the relative stability of N-H···O and N-H···S hydrogen bonds, we cocrystallized the antithyroid drug 6-propyl-2-thiouracil with two complementary heterocycles. In the cocrystal pyrimidin-2-amine-6-propyl-2-thiouracil (1/2), C(4)H(5)N(3)·2C(7)H(10)N(2)OS, (I), the `base pair' is connected by one N-H···S and one N-H···N hydrogen bond. Homodimers of 6-propyl-2-thiouracil linked by two N-H···S hydrogen bonds are observed in the cocrystal N-(6-acetamidopyridin-2-yl)acetamide-6-propyl-2-thiouracil (1/2), C(9)H(11)N(3)O(2)·2C(7)H(10)N(2)OS, (II). The crystal structure of 6-propyl-2-thiouracil itself, C(7)H(10)N(2)OS, (III), is stabilized by pairwise N-H···O and N-H···S hydrogen bonds. In all three structures, N-H···S hydrogen bonds occur only within R(2)(2)(8) patterns, whereas N-H···O hydrogen bonds tend to connect the homo- and heterodimers into extended networks. In agreement with related structures, the hydrogen-bonding capability of C=O and C=S groups seems to be comparable.
(Z-Ethyl 3-(4-chlorophenyl-2-cyano-3-(2,6-difluorobenzamidoacrylate
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Zhang Xiaoyan
2008-12-01
Full Text Available The title compound, C19H13ClF2N2O3, was prepared by the reaction of (Z-ethyl 3-amino-3-(4-chlorophenyl-2-cyanoacrylate and 2,6-difluorobenzoyl chloride. The dihedral angle between the chlorobenzene and fluorobenzene rings is 37.0 (1°. The ethyl group is disordered over two positions [occupancies = 0.52 (2:0.48 (2]. In addition to intramolecular N—H...O and N—H...F hydrogen bonds, the crystal packing shows the molecules to be connected by intermolecular C—H...O and C—H...N hydrogen bonds.
5-(4-Ethoxyphenyl-3-(pyridin-2-yl-4,5-dihydro-1H-pyrazole-1-carbothioamide
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Hoong-Kun Fun
2012-03-01
Full Text Available In the title compound, C17H18N4OS, a pyrazoline derivative, the pyrazoline ring adopts an envelope conformation with the C atom bonded to the benzene ring as the flap atom. The dihedral angle between the pyridine and benzene rings is 80.50 (6°. The ethoxyphenyl group is approximately planar, with an r.m.s. deviation of 0.0238 (1 Å for the nine non-H atoms. In the crystal, molecules are linked by N—H...O and N—H...S hydrogen bonds into a tape along the b axis. Weak C—H...N and C—H...π interactions are also observed.
Xu, Zhengtao; Mitzi, David B; Dimitrakopoulos, Christos D; Maxcy, Karen R
2003-03-24
Two new semiconducting hybrid perovskites based on 2-substituted phenethylammonium cations, (2-XC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) (X = Br, Cl), are characterized and compared with the previously reported X = F compound, with a focus on the steric interaction between the organic and inorganic components. The crystal structure of (2-ClC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) is solved in a disordered subcell [C2/m, a = 33.781(7) A, b = 6.178(1) A, c = 6.190(1) A, beta = 90.42(3)(o), and Z = 2]. The structure is similar to the known (2-FC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) structure with regard to both the conformation of the organic cations and the bonding features of the inorganic sheet. The (2-BrC(6)H(4)C(2)H(4)NH(3))(2)SnI(4) system adopts a fully ordered monoclinic cell [P2(1)/c, a = 18.540(2) A, b = 8.3443(7) A, c = 8.7795(7) A, beta = 93.039(1)(o), and Z = 2]. The organic cation adopts the anti conformation, instead of the gauche conformation observed in the X = F and Cl compounds, apparently because of the need to accommodate the additional volume of the bromo group. The steric effect of the bromo group also impacts the perovskite sheet, causing notable distortions, such as a compressed Sn-I-Sn bond angle (148.7(o), as compared with the average values of 153.3 and 154.8(o) for the fluoro and chloro compounds, respectively). The optical absorption features a substantial blue shift (lowest exciton peak: 557 nm, 2.23 eV) relative to the spectra of the fluoro and chloro compounds (588 and 586 nm, respectively). Also presented are transport properties for thin-film field-effect transistors (TFTs) based on spin-coated films of the two hybrid semiconductors.
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Nico Fleck
2018-04-01
Full Text Available The title compound, a triarylmethanol, C46H64OS12Si3 1, was synthesized via lithiation of tris-2,2,6,6-tetramethylbenzo[1,2-d;4,5-d′]bis[1,3]dithiol-4-yl-methanol, 2, and electrophilic quenching with trimethylsilyl chloride. The current crystal structure reveals information about the reactivity of this compound and compares well with the structure reported for the unsubstituted parent compound 2 [Driesschaert et al. (2012. Eur. J. Org. Chem. 33, 6517–6525]. The title compound 1 forms molecular propellers and crystallizes in P\\overline{1}, featuring an unusually long Si—Car bond of 1.910 (3 Å. Moreover, the geometry at the central quaternary carbon is rather trigonal-pyramidal than tetrahedral due to vast intramolecular stress. One trimethylsilyl group is disordered over two positions in a 0.504 (4:0.496 (4 ratio and one S atom is disordered over two positions in a 0.509 (7:0.491 (7 ratio. The contribution of disordered diethyl ether solvent molecule(s was removed using the PLATON SQUEEZE (Spek, 2015 solvent masking procedure. These solvent molecules are not considered in the given chemical formula and other crystal data.
1-(4-Methylphenylsulfonyl-5,6-dinitro-1H-indazole
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Bassou Oulemda
2014-01-01
Full Text Available In the title compound, C14H10N4O6S, the indazole ring system is almost perpendicular to the tosyl ring, as indicated by the dihedral angle of 89.40 (9° between their planes. The dihedral angles between the indazole system and the nitro groups are 57.0 (3 and 31.9 (3°. In the crystal, molecules are linked by C—H...O interactions, forming chains running along [100].
Shao, Ze-Huai; Luo, Jun; Cai, Rui-Fang; Zhou, Xi-Geng; Weng, Lin-Hong; Chen, Zhen-Xia
2004-06-01
Two new one-dimensional coordination polymers, viz. the title compounds, [Co[C(CN)(3)](2)(C(6)H(5)N(3))(2)](n), (I), and [Mn[C(CN)(3)](2)(C(5)H(8)N(2))(2)](n), (II), have been synthesized and characterized by X-ray diffraction. Both complexes consist of linear chains with double 1,5-tricyanomethanide bridges between neighbouring divalent metal ions. The Co and Mn atoms are located on centres of inversion. In (I), the coordination environment of the Co(II) atom is that of an elongated octahedron. The Co(II) atom is coordinated in the equatorial plane by four nitrile N atoms of four bridging tricyanomethanide ions, with Co-N distances of 2.106 (2) and 2.110 (2) A, and in the apical positions by two N atoms from the benzotriazole ligands, with a Co-N distance of 2.149 (2) A. The [Co[C(CN)(3)](2)(C(6)H(5)N(3))(2)] units form infinite chains extending along the a axis. These chains are crosslinked via a hydrogen bond between the uncoordinated nitrile N atom of a tricyanomethanide anion and the H atom on the uncoordinated N atom of a benzotriazole ligand from an adjacent chain, thus forming a three-dimensional network structure. In (II), the Mn(II) atom also adopts a slightly distorted octahedral geometry, with four nitrile N atoms of tricyanomethanide ligands [Mn-N = 2.226 (2) and 2.227 (2) A] in equatorial positions and two N atoms of the monodentate 3,5-dimethylpyrazole ligands [Mn-N = 2.231 (2) A] in the axial sites. In (II), one-dimensional polymeric chains extending along the b axis are formed, with tricyanomethanide anions acting as bidentate bridging ligands. A hydrogen bond between the uncoordinated nitrile N atom of the tricyanomethanide ligand and the H atom on the uncoordinated N atom of a 3,5-dimethylpyrazole group from a neighbouring chain links the molecule into a two-dimensional layered structure.
Synthesis of new dithiacobaltaborane clusters derived from arachno-6,8-S2B7H9
International Nuclear Information System (INIS)
Kang, S.O.; Sneddon, L.G.
1988-01-01
A series of air-stable dithiacobaltaborane clusters has been isolated from either the reaction of the arachno-S 2 B 7 H 8 - anion with cobalt chloride and pentamethylcyclopentadienide or the reaction of neutral arachno-6,8-S 2 B 7 H 9 with cobalt atoms and pentamethylcyclopentadiene. Thus, the reaction of arachno-S 2 B 7 H 8 - with CoCl 2 and C 5 (CH 3 ) 5 - in THF gave, as the major products, the triple-decker compound nido-4,6-η-C 5 (CH 3 ) 52 Co 2 -3,5-S 2 B 2 H 2 (I) and the 11-vertex cluster nido-8,10(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (III). Also isolated in smaller amounts were a chloride derivative of I, nido-1-Cl-4,6-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -3,5-S 2 B 2 H (II), two isomers of III, nido-3,10-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (IV) and nido-3,5-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -7,9-S 2 B 7 H 7 (V), and the eight-boron cluster nido-8-(η-C 5 (CH 3 ) 5 )Co-7,9-S 2 B 8 H 8 (VI). Other trace products of the reaction included the six-boron clusters nido-5,8-(η-C 5 (CH 3 ) 5 ) 2 Co 2 -6,9-S 2 B 6 H 6 (VII) and arachno-7-(η-C 5 (CH 3 ) 5 )Co-6,8-S 2 B 6 H 8 (VIII). Compound III was found to isomerize at 250 degree C to IV, which could then be converted to V at 300 degree C. The reaction of cobalt atoms with arachno-6,8-S 2 B 7 H 9 in the presence of pentamethylcyclopentadiene gave VIII as the major product; however, a number of other clusters including I, V, VI, and [(η-C 5 (CH 3 ) 5 ) 2 Co] + [(SB 10 H 10 ) 2 Co] - were isolated in trace amounts. 16 references, 6 figures, 3 tables
N,N',N"-Tris[(5-methoxy-1H-indol-3-ylethyl]benzene-1,3,5-tricarboxamide
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Ute Schmidt
2015-03-01
Full Text Available The title indole-based compound that enforces tripodal topology and is potential applicable for the use as artificial receptor, was prepared by a simple reaction of 1,3,5-benzenetricarbonyl trichloride with 5-methoxytryptamine. The compound was characterized by elemental analysis, 1H-NMR, 13C-NMR and mass spectrometry.
Ethyl (E)-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylidene)acetate
Oulemda Bassou; Hakima Chicha; Latifa Bouissane; El Mostapha Rakib; Mohamed Saadi; Lahcen El Ammari
2017-01-01
In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å), with the largest deviation from the mean plane being 0.012 (1) Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7)° between them. Two intramolecular hydrogen bonds, completing S(6) ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hy...
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Niklas Koch
2014-04-01
Full Text Available In the title compound, C36H24Br3N3O6·C7H8, the toluene solvent molecule is associated with the receptor molecule via C—H...π bonding. The planes of the phthalimido groups are inclined at 77.0 (1, 63.0 (1 and 77.8 (1° with respect to the benzene ring. The molecular conformation is stabilized by C—H...O and C—H...Br hydrogen bonds. The crystal structure features non-classical hydrogen bonds of the C—H...N, C—H...O and C—H...Br type, leading to a three-dimensional cross-linking of molecules. The pattern of non-covalent intermolecular bonding is completed by O...Br halogen bonds [3.306 (3 Å], which link the receptor molecules into infinite strands extending along the a-axis direction.
2,2,7-Trichloro-3,4-dihydronaphthalen-1(2H-one
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Ben Capuano
2009-09-01
Full Text Available The title compound, C10H7Cl3O, obtained as a major byproduct from a classical Schmidt reaction. The cyclohexyl ring is distorted from a classical chair conformation, as observed for monocyclic analogues, presumably due to conjugation of the planar annulated benzo ring and the ketone group (r.m.s. deviation 0.024 Å. There are no significant intermolecular interactions.
7-Chloro-4-oxo-4H-chromene-3-carbaldehyde
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Yoshinobu Ishikawa
2014-08-01
Full Text Available In the title compound, C10H5ClO3, a chlorinated 3-formylchromone derivative, all atoms are essentially coplanar (r.m.s. deviation = 0.0592 Å for all non-H atoms, with the largest deviation from the least-squares plane [0.1792 (19 Å] being for the chromone-ring carbonyl O atom. In the crystal, molecules are linked through C—H...O hydrogen bonds to form tetrads, which are assembled by stacking interactions [centroid–centroid distance between the pyran rings = 3.823 (3 Å] and van der Waals contacts between the Cl atoms [Cl...Cl = 3.4483 (16 Å and C—Cl...Cl = 171.73 (7°] into a three-dimensional architecture.
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Sergey Malinkin
2009-10-01
Full Text Available The title compound, [Cu2(C7H6N2O3Cl2(C5H5N4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octahedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H...O hydrogen bond connects the complex molecules and propan-2-ol solvent molecules into pairs. These pairs form columns along the a axis.
(3-Methylbenzonitrile-1κN-cis-tetrakis(μ-N-phenylacetamidato-1:2κ4N:O;1:2κ4O:N-dirhodium(II(Rh—Rh
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Cassandra T. Eagle
2014-08-01
Full Text Available The complex molecule of the title compound, [Rh2{N(C6H5COCH3}4(NCC7H7], has crystallographically-imposed mirror symmetry. The four acetamide ligands bridging the dirhodium core are arranged in a 2,2-cis manner with two N atoms and two O atoms coordinating to the unique RhII atom cis to one another. The Neq—Rh—Rh—Oeq torsion angles on the acetamide bridge are 0.75 (7 and 1.99 (9°. The axial nitrile ligand completes the distorted octahedral coordination sphere of one RhII atom and shows a nonlinear coordination, with an Rh—N—C bond angle of 162.8 (5°; the N—C bond length is 1.154 (7 Å.
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Teng Zhao
2016-11-01
Full Text Available In 2014, surveillance of sentinel chicken for avian influenza virus was conducted in aquatic bird habitat near Wuxi City, Jiangsu Province, China. Two H7N2, one H5N6, and two H9N2 viruses were isolated. Sequence analysis revealed that the H7N2 virus is a novel reassortant of H7N9 and H9N2 viruses and H5N6 virus is a reassortant of H5N1 clade 2.3.4 and H6N6 viruses. Substitutions V186 and L226 (H3 numbering in the hemagglutinin (HA gene protein was found in two H7N2 viruses but not in the H5N6 virus. Two A138 and A160 mutations were identified in the HA gene protein of all three viruses but a P128 mutation was only in the H5N6 virus. A deletion of three and eleven amino acids in the neuraminidase stalk region was found in two H7N2 and H5N6 viruses, respectively. Moreover, a mutation of N31 in M2 protein was observed in both two H7N2 viruses. High similarity of these isolated viruses to viruses previously identified among poultry and humans, suggests that peridomestic aquatic birds may play a role in sustaining novel virus transmission. Therefore, continued surveillance is needed to monitor these avian influenza viruses in wild bird and domestic poultry that may pose a threat to poultry and human health.
International Nuclear Information System (INIS)
Holzapfel, C.W.; Koekemoer, J.M.; Kruger, G.J.; Van Dyk, M.S.
1985-01-01
The structure and stereochemistry of the title compound, a 11-deoxy-11-azaprostaglandin synthon, has been determined by single-crystal X-ray diffraction methods. The dioxolane and aza-rings are cis-fused on the same side to the central furanose ring. Both the ethoxycarbonyl group on C(5) and the acetoxy-group on C(6) have a β-configuration. The conformation of the solid state structure is compared with that in chloroform solution, as evidenced by 1 H n.m.r. studies
Crystal structure of strontium osmate (8) Sr[OsO5(H2O)]x3H2O
International Nuclear Information System (INIS)
Nevskij, N.N; Ivanov-Ehmin, B.N.; Nevskaya, N.A.; Belov, N.V.; AN SSSR, Moscow. Inst. Kristallografii)
1982-01-01
Crystal structure of the Sr[OsO 5 (H 2 O)]x3H 2 O complex is studied. Rhombic P-cell has the parameters: a=6.426(1), b=7.888(1), c=14.377(5) A, Vsub(c)=729 A 3 . The R-factor equals 0.034. The coordinates of the basis atoms and isotropic temperature corrections, as well as basic interatomic distances, are determined
{1-[(3,5-Dimethyl-4H-1,2,4-triazol-4-ylimino]ethyl}ferrocene
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Mao-Ping Song
2008-10-01
Full Text Available In the title compound, [Fe(C5H5(C11H13N4], the triazolyl and Cp ring form a dihedral angle of 76.6 (3°. In the crystal structure, there are both intra- and intermolecular C—H...π interactions, forming a one-dimensional chain structure along [010].
cis-Dichlorido(dimethyl sulfoxide-κS(N,N,N′,N′-tetramethylguanidine-κN′′platinum(II
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Ivan I. Eliseev
2013-02-01
Full Text Available In the title compound, cis-[PtCl2(C5H13N3(C2H6OS], the four-coordinate PtII atom is bonded to one N atom of the N,N,N′,N′-tetramethylguanidine ligand, one dimethyl sulfoxide S atom and two chloride ligands, forming a cis-square-planar geometry. The bond lengths and angles of the N—Pt—Cl functionality are typical for imine dichloridoplatinum(II complexes. The H atom of the imino group is oriented towards the O atom of the sulfoxide group of a neighboring molecule and forms an N—H...O hydrogen bond.
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S. Sriman Narayanan
2008-09-01
Full Text Available In the title compound, C29H24F2N2O2, one of the pyrrolidine rings of the pyrrolizine system is disordered over two sites, with occupancy factors 0.734:0.266 (12. Both components of the disordered pyrrolidine ring adopt envelope conformations, whereas the other pyrrolidine ring adopts a twist conformation. The molecules are linked into centrosymmetric dimers by N—H...O hydrogen bonds and the dimers are connected via C—H...π interactions. The crystal structure is also stabilized by intermolecular C—H...F hydrogen bonds.
Propane-1,3-diaminium–2-carboxypyridine-6-carboxylate–pyridine-2,6-dicarboxylic acid–water (1/2/2/8
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Hossein Aghabozorg
2008-01-01
Full Text Available The title proton-transfer compound, C3H12N22+·2C7H4NO4−·2C7H5NO4·8H2O or (pnH2(pydcH2.2(pydcH2·8H2O, was obtained by the reaction of pyridine-2,6-dicarboxylic acid (pydcH2 and propane-1,3-diamine (pn in aqueous solution. Both neutral and monoanionic forms of the diacid are observed in the crystal structure. The negative charge of two monoanions is balanced by the dicationic propane-1,3-diaminium species. In addition, considerable π–π stacking interactions between the aromatic rings of the (pydcH− and (pydcH2 fragments [with centroid–centroid distances of 3.5108 (11–3.5949 (11 Å] are observed. The most important feature of this crystal structure is the presence of a large number of O—H...O, O—H...N, N—H...O, N—H...N, C—H...O and C—H...N hydrogen bonds, with D...A ranging from 2.445 (2 to 3.485 (3 Å. These interactions as well as ion pairing and π–π stacking connect the various fragments into a supramolecular structure.
Bis(O-ethyl dithio-carbonato-κS,S')bis-(pyridine-3-carbonitrile-κN)nickel(II).
Kapoor, Sanjay; Kour, Ramandeep; Sachar, Renu; Kant, Rajni; Gupta, Vivek K; Kapoor, Kamini
2012-01-01
The Ni(2+) ion in the title complex, [Ni(C(3)H(5)OS(2))(2)(C(6)H(4)N(2))(2)], is in a strongly distorted octa-hedral coordination environment formed by an N(2)S(4) donor set, with the Ni(2+) ion located on a centre of inversion. In the crystal, weak C-H⋯S and C-H⋯N inter-actions are observed.
(3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione
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Garima Sharma
2012-09-01
Full Text Available In the title compound, C26H18N2O3, the maximum deviations from planarity for the tetrahydro-1H-naphtho[2,3-c]pyrrole and indoline rings systems are 0.091 (1 and 0.012 (2 Å, respectively. These ring systems make a dihedral angle of 89.95 (6° with each other and they make dihedral angles of 73.42 (8 and 71.28 (9°, respectively, with the benzene ring. In the crystal, inversion dimers linked by pairs of N—H...O hydrogen bonds generate R22(8 loops and C—H...O interactions connect the dimers into corrugated sheets lying parallel to the bc plane.
2-(4-Methoxy-1H-indol-3-ylacetonitrile
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Yong-Hong Lu
2012-01-01
Full Text Available In the title compound, C11H10N2O, the cyanide group is twisted away from the indole-ring plane [Ccy—Cme—Car—Car = 70.7 (2°; cy = cyanide, me = methylene, ar = aromatic], whereas the methoxy C atom is almost coplanar with the ring system [displacement = 0.014 (5 Å]. In the crystal, N—H...N hydrogen bonds link the molecules into C(7 chains propagating in [100].
2,6-Bis(9-ethyl-9H-carbazolylmethylenecyclohexanone
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Abdullah M. Asiri
2009-10-01
Full Text Available The title compound, 2,6-bis(ethyl-9-ethyl-9H-carbazolylmethylenecyclohexanone has been synthesized by condensation of 9-ethylcarbazole-3-aldehyde and cyclohexanone in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H NMR, 13C NMR and EI-MS spectral analysis.
International Nuclear Information System (INIS)
Borel, A.G.; Abbott, F.S.
1990-01-01
Pentadeuteriophenyl clobazam was synthesized in essentially quantitative isotopic purity, and characterized by 1 H-NMR and mass spectroscopy. The title compound was found to be >98% pure by HPLC, and its retention time (t R 6.17 min) was less than that of an authentic clobazam standard (t R 6.32 min). Of the five steps in the synthesis of clobazam, the most susceptible to deuterium exchange was the nucleophilic substitution of 2,4-dichloronitrobenzene by aniline-d 7 to form N-(5-chloro-2-nitrophenyl)penta-deuteriophenylamine. In this step, the isotopic impurity aniline-2,3,4,5-d 5 introduced protons from nitrogen into the ortho and para positions of the deuteriophenyl ring of N-(5-chloro-2-nitrophenyl)pentadeuteriophenylamine. (author)
N-[7-Ethoxy-1-(prop-2-en-1-yl-1H-indazol-4-yl]-4-methylbenzenesulfonamide
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Najat Abbassi
2011-07-01
Full Text Available In the title compound, C19H21N3O3S, the C—SO2—NH—C torsion angle is 103.72 (11°. The almost planar indazole ring [r.m.s. deviation = 0.0202 (14 Å] is twisted away from the methylbenzene ring by 76.87 (7°. The vinyl group is disordered over two orientations with site occupancies of 0.622 (10 and 0.378 (10. The S atom has a distorted tetrahedral geometry [maximum deviation: O—S—O = 119.18 (11°]. An intramolecular C—H...O hydrogen bond occurs. In the crystal, two molecules are linked about a center of inversion by pairs of N—H...O hydrogen bonds, generating a dimer. C—H...π interactions are also observed.
Murugan, R.; Gunasekaran, B.; Narayanan, S. Sriman; Manivannan, V.
2008-01-01
In the title compound, C37H27Cl2NO2, the 3,4-dichloro?phenyl ring makes a dihedral angle of 46.66?(6)? with the phenyl ring. The mol?ecular structure is stabilized by weak intra?molecular C?H?O inter?actions and the crystal structure is stabilized by weak inter?molecular C?H?O inter?actions. The C?C?C?C?C five-membered ring is planar, while the C?C?C?C?N five-membered ring adopts a half-chair conformation.
International Nuclear Information System (INIS)
McMahon, M.M.; Schwenk, W.F.; Haymond, M.W.; Rizza, R.A.
1989-01-01
Recent studies indicate that hydrogen-labeled glucose tracers underestimate glucose turnover in humans under conditions of high flux. The cause of this underestimation is unknown. To determine whether the error is time-, pool-, model-, or insulin-dependent, glucose turnover was measured simultaneously with [6-3H]-, [6,6-2H2]-, and [6-14C]glucose during a 7-h infusion of either insulin (1 mU.kg-1.min-1) or saline. During the insulin infusion, steady-state glucose turnover measured with both [6-3H]glucose (8.0 +/- 0.5 mg.kg-1.min-1) and [6,6-2H2]glucose (7.6 +/- 0.5 mg.kg-1.min-1) was lower (P less than .01) than either the glucose infusion rate required to maintain euglycemia (9.8 +/- 0.7 mg.kg-1.min-1) or glucose turnover determined with [6-14C]glucose and corrected for Cori cycle activity (9.8 +/- 0.7 mg.kg-1.min-1). Consequently negative glucose production rates (P less than .01) were obtained with either [6-3H]- or [6,6-2H2]- but not [6-14C]glucose. The difference between turnover estimated with [6-3H]glucose and actual glucose disposal (or 14C glucose flux) did not decrease with time and was not dependent on duration of isotope infusion. During saline infusion, estimates of glucose turnover were similar regardless of the glucose tracer used. High-performance liquid chromatography of the radioactive glucose tracer and plasma revealed the presence of a tritiated nonglucose contaminant. Although the contaminant represented only 1.5% of the radioactivity in the [6-3H]glucose infusate, its clearance was 10-fold less (P less than .001) than that of [6-3H]glucose. This resulted in accumulation in plasma, with the contaminant accounting for 16.6 +/- 2.09 and 10.8 +/- 0.9% of what customarily is assumed to be plasma glucose radioactivity during the insulin or saline infusion, respectively (P less than .01)
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M. J. Piltan
2016-08-01
Full Text Available In the present paper, an efficient one-pot synthesis of 7-alkyl-6H,7H-naphtho[1',2':5,6]pyrano[3,2-c]chromen-6-ones is described by three-component reaction of β-naphthol, aromatic aldehydes and 4-hydroxycoumarin using ZnO nanoparticles under solvent-free conditions. The present method provides a novel and efficient procedure for the synthesis of chromene derivatives with some advantageous such as short reaction times, easy workup, high yields, wide range of products, reusability of the catalyst, little catalyst loading and green conditions in the presence of ZnO nanoparticles (7 mol% at 110 ºC.
(7aR-1-[(2R,5S,E-6-Hydroxy-5,6-dimethylhept-3-en-2-yl]-7a-methylhexahydro-1H-inden-4(2H-one
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Marcos L. Rivadulla
2013-02-01
Full Text Available The chiral title compound, C19H32O2, contains a [4.3.0]-bicyclic moiety in which the shared C—C bond presents a trans configuration and a side chain in which the C=C double bond shows an E conformation. The conformations of five- and six-membered rings are envelope (with the bridgehead atom bearing the methyl substituent as the flap and chair, respectively, with a dihedral angle of 4.08 (17° between the idealized planes of the rings. In the crystal, the molecules are self-assembled via classical O—H...O hydrogen bonds, forming chains along [112]; these chains are linked by weak non-classical C—H...O hydrogen bonds, giving a two-dimensional supramolecular structure parallel to (010. The absolute configuration was established according to the configuration of the starting material.
μ-Adipato-κ2O1:O4-bis{[2,6-bis(1H-benzimidazol-2-yl-κN3pyridine-κN](nitrato-κOlead(II}
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Lian-Qiang Wei
2010-01-01
Full Text Available The dinuclear title compound, [Pb2(C6H8O4(NO32(C19H13N52], lies with the mid-point of the butyl chain of the bridging adipate unit on a center of inversion. The PbII ion is covalently bonded to the nitrate anion and is bonded to a carboxylate group of the adipate unit by another covalent bond. The N-heterocycle functions in a chelating tridentate mode. The metal atom exists in a Ψ-octahedral coordination environment. When weaker Pb...O interactions are also considered, the geometry is a Ψ-tricapped trigonal prism in which the lone-pair electrons occupy one face of the trigonal prism. Adjacent molecules are linked into a layer structure by N—H...O hydrogen bonds.
6-Chloro-N′-(2-hydroxy-1-naphthylmethylenenicotinohydrazide
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Feng Zhi
2008-01-01
Full Text Available The title compound, C17H12ClN3O2, was synthesized by the Schiff base condensation reaction of 2-hydroxy-1-naphthaldehyde with 6-chloronicotinic acid hydrazide in a methanol solution. The molecule displays a trans configuration with respect to the C=N and C—N bonds. The dihedral angle between the naphthyl ring system and the pyridine ring is 7.6 (4°. There is an intramolecular O—H...N hydrogen bond. The crystal structure is stabilized by intermolecular N—H...O and C—H...O hydrogen bonds, forming chains running along the b axis.
Poly[di-μ2-aqua-μ5-(pyridine-2,6-dicarboxylato-μ3-(pyridine-2,6-dicarboxylato-cobalt(IIdisodium
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Alexander N. Boyko
2011-12-01
Full Text Available In the title compound, [CoNa2(C7H3NO42(H2O2]n, the CoII atom is coordinated by two pyridine N atoms and four carboxylate O atoms from two doubly deprotonated pyridine-2,6-dicarboxylate ligands in a distorted octahedral geometry. One Na+ cation is coordinated by three carboxylate O atoms and two water molecules and the other is coordinated by five carboxylate O atoms and two water molecules in an irregular geometry. The bis(pyridine-2,6-dicarboxylatocobalt complex units are connected by Na+ cations and bridging water molecules into a three-dimensional coordination network. O—H...O hydrogen bonds are formed between the water molecules and the carboxylate O atoms.
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Sushil K. Gupta
2011-10-01
Full Text Available The title compound, C46H40N4O2·0.33C6H12, was obtained unintentionally as a product of an attempted synthesis of a cadmium(II complex of the [2,6-{PhSe(CH22N=CPh}2C6H2(4-Me(OH] ligand. The full tetraiminodiphenol macrocyclic ligand is generated by the application of an inversion centre. The macrocyclic ligand features strong intramolecular O—H...N hydrogen bonds. The dihedral angles formed between the phenyl ring incorporated within the macrocycle and the peripheral phenyl rings are 82.99 (8 and 88.20 (8°. The cyclohexane solvent molecule lies about a site of overline{3} symmetry. Other solvent within the lattice was disordered and was treated with the SQUEEZE routine [Spek (2009. Acta Cryst. D65, 148–155].
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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.
N-(3-{[(Z-(3-Hydroxy-4-methylphenylimino]methyl}pyridin-2-ylpivalamide
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Şehriman Atalay
2016-03-01
Full Text Available The molecular structure of the title compound, C18H21N3O2, contains pivalamide, pyridin and hydroxy-methylphenyl moieties. The whole molecule is not planar, the dihedral angle between the benzene rings being 34.84 (7°. The molecular conformation is stabilized by an intramolecular N—H...N hydrogen bond. In the crystal, molecules are linked by O—H...O, O—H...N and C—H...O hydrogen bonds. The C and H atoms of the tert-butyl group disordered over two sets of sites with an occupancy ratio of 0.692 (5:0.308 (5.
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Mehmet Akkurt
2014-06-01
Full Text Available In the title compound, C33H27BrClNO4, the dihydropyridine ring adopts a flattened boat conformation. The molecular conformation is stabilized by an intramolecular O—H...O hydrogen bond, with an S(8 ring motif. In the crystal, O—H...O, C—H...O and C—H...Cl hydrogen bonds, and C—H...π interactions link the molecules, forming a three-dimensional network. In the acridinedione ring system, the two ring C atoms at the 2- and 3-positions, and the C atom at the 6-position and the atoms of the phenyl ring attached to the C atom at the 6-position are disordered over two sets of sites with occupancy ratios of 0.783 (5:0.217 (5 and 0.526 (18:0.474 (18, respectively.
Poly[[diaqua-μ4-pyrazine-2,3-dicarboxylato-κ6N,O2:O2′:O3,O3′:O3-strontium(II] monohydrate
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Vahid Amani
2008-07-01
Full Text Available In the title compound, {[Sr(C6H2N2O4(H2O2]·H2O}n, the SrII ions are bridged by the pyrazine-2,3-dicarboxylate ligands with the formation of two-dimensional polymeric layers parallel to the ac plane. Each SrII ion is eight-coordinated by one N and five O atoms from the four ligands and two water molecules. The coordination polyhedron is derived from a pentagonal bipyramid with an O atom at the apex on one side of the equatorial plane and two O atoms sharing the apical site on the other side. The coordinated and uncoordinated water molecules are involved in O—H...O and O—H...N hydrogen bonds, which consolidate the crystal structure.
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Ackland, M.J.; Dring, L.G.; Jones, J.R.
1991-01-01
The title compounds were synthesised in 7 steps from 1,7-dihydroxynaphthalene as follows: 1,7-dihydroxynaphthalene was methylated and subjected to a Birch reduction to yield 8-methoxy-2-tetralone. Reductive amination with sodium cyanoboro[ 3 H]hydride and n-propylamine gave 8-methoxy-2-(n-propylamino)-[2- 3 H]tetralin which was acylated and reduced to give (±)8-methoxy-2-(N,N-dipropylamino)-[2 3 H]tetralin. Treatment with conc.HC1 gave (±)-8-hydroxy-2-(N,N-dipropylamino)-[2- 3 H]tetralin. The racemate was then resolved by chiral mobile phase chromatography. (author)
N6-Benzyladenosine Derivatives as Novel N-Donor Ligands of Platinum(II Dichlorido Complexes
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Ján Vančo
2013-06-01
Full Text Available The platinum(II complexes trans-[PtCl2(Ln2]∙xSolv 1–13 (Solv = H2O or CH3OH, involving N6-benzyladenosine-based N-donor ligands, were synthesized; Ln stands for N6-(2-methoxybenzyladenosine (L1, involved in complex 1, N6-(4-methoxy-benzyladenosine (L2, 2, N6-(2-chlorobenzyladenosine (L3, 3, N6-(4-chlorobenzyl-adenosine (L4, 4, N6-(2-hydroxybenzyladenosine (L5, 5, N6-(3-hydroxybenzyl-adenosine (L6, 6, N6-(2-hydroxy-3-methoxybenzyladenosine (L7, 7, N6-(4-fluoro-benzyladenosine (L8, 8, N6-(4-methylbenzyladenosine (L9, 9, 2-chloro-N6-(3-hydroxy-benzyladenosine (L10, 10, 2-chloro-N6-(4-hydroxybenzyladenosine (L11, 11, 2-chloro-N6-(2-hydroxy-3-methoxybenzyladenosine (L12, 12 and 2-chloro-N6-(2-hydroxy-5-methylbenzyladenosine (L13, 13. The compounds were characterized by elemental analysis, mass spectrometry, IR and multinuclear (1H-, 13C-, 195Pt- and 15N- and two-dimensional NMR spectroscopy, which proved the N7-coordination mode of the appropriate N6-benzyladenosine derivative and trans-geometry of the title complexes. The complexes 1–13 were found to be non-toxic in vitro against two selected human cancer cell lines (HOS and MCF7; with IC50 > 50.0 µM. However, they were found (by ESI-MS study to be able to interact with the physiological levels of the sulfur-containing biogenic biomolecule L-methionine by a relatively simple 1:1 exchange mechanism (one Ln molecule was replaced by one L-methionine molecule, thus forming a mixed-nitrogen/sulfur-ligand dichlorido-platinum(II coordination species.
4,10-Diallyloxy-1,2,3,6b,7,8,9,12b-octahydroperylene
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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.
7α-Methoxycarbonyl-6,7,8,14-tetrahydro-6,14-endo-ethenothebaine
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Mustafa Odabaşoğlu
2009-04-01
Full Text Available In the molecule of the title compound, C23H27NO5, the furan ring adopts an envelope conformation. Intramolecular C—H...O interactions result in the formation of S(5 and S(6 motifs. In the crystal structure, weak intermolecular C—H...O hydrogen bonds link the molecules through C(6 and C(8 chains along the [100] and [010] directions, generating a two-dimensional network.
trans-(1,8-Dibenzyl-1,3,6,8,10,13-hexaazacyclotetradecanediisonicotinatonickel(II
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Kil Sik Min
2008-02-01
Full Text Available In the centrosymmetric title compound, [Ni(C6H4NO22(C22H34N6], the NiII ion is bonded to the four secondary N atoms of the macrocyclic ligand in a square-planar fashion and two carboxylate O atoms of the isonicotinate ions in axial positions, resulting in a tetragonally distorted octahedron. An offset face-to-face π–π stacking interaction [centroid–centroid distance = 3.674(4 Å] and N—H...N and N—H...O hydrogen-bonding interactions give rise to a one-dimensional supramolecular structure in the solid state.
Ethyl (E-2-(2,7-dimethyl-5-oxo-4H,5H-pyrano[4,3-b]pyran-4-ylideneacetate
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Oulemda Bassou
2017-02-01
Full Text Available In the title compound, C14H14O5, the two heterocyclic rings are coplanar (r.m.s. deviation = 0.008 Å, with the largest deviation from the mean plane being 0.012 (1 Å. The mean plane through the acetate group is inclined slightly with respect to the oxopyrano[4,3-b]pyran-4-yl system, as indicated by the dihedral angle of 1.70 (7° between them. Two intramolecular hydrogen bonds, completing S(6 ring motifs, are observed in the molecule. In the crystal, molecules are linked by weak C—H...O hydrogen bonds involving the same acceptor atom, forming chains propagating along the c-axis direction and enclosing R21(6 ring motifs. The chains are linked via offset π–π interactions [intercentroid distance = 3.622 (1 Å], involving inversion-related oxopyrano[4,3-b]pyran-4-yl ring systems, forming slabs parallel to the bc plane.
9-Furfurylidene-2,3-dimethyl-6,7,8,9-tetrahydro-4H-thieno[2′,3′:4,5]pyrimidino[1,2-a]pyridin-4-one
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Khusnutdin M. Shakhidoyatov
2010-03-01
Full Text Available The title compound, C17H16N2O2S, was obtained by condensation of 2,3-dimethylthieno[2′,3′:4,5]pyrimidino[1,2-a]pyridin-4-one with furfural in the presence of sodium hydroxide. One of the methylene groups of the tetrahydropyrido ring is disordered over two positions in a 0.87 (1:0.13 (1 ratio. The thieno[2,3-d]pyrimidin-4-one unit and the furan ring are both planar (r.m.s. deviation = 0.535 Å, and coplanar with each other, forming a dihedral angle of 5.4 (1°. Four weak intermolecular hydrogen bonds (C—H...O and C—H...N are observed in the structure, which join molecules into a network parallel to (101.
2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide
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B. Narayana
2013-01-01
Full Text Available In the crystal structure of the title compound, C19H17Cl2N3O2, the molecules form dimers of the R22(10 type through N—H...O hydrogen bonding. As a result of steric repulsion, the amide group is rotated with respect to both the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 80.70 (13 and 64.82 (12°, respectively. The dihedral angle between the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings is 48.45 (5° while that between the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings is 56.33 (6°.
(E-2-(5-Chloro-2-hydroxybenzylidene-N-cyclohexylhydrazine-1-carbothioamide
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Md. Azharul Arafath
2017-01-01
Full Text Available In the title compound, C14H18ClN3OS, the phenol ring is almost coplanar with the hydrazinecarbothioamide moiety, making a dihedral angle of 6.92 (8°. The cyclohexane ring has a chair conformation and the conformation about the C=N bond is E. In the crystal, molecules are linked by N—H...O and O—H...S hydrogen bonds, forming inversion dimers with an R22(14 ring motif flanked by two R22(6 ring motifs. The dimers are linked by short Cl...Cl interactions, forming layers parallel to the ab plane.
Energy Technology Data Exchange (ETDEWEB)
Dammak, T., E-mail: thameurlpa@yahoo.f [Laboratoire de Physique appliquee (LPA), Faculte des Sciences de Sfax, 3018, BP 802 (Tunisia); Elleuch, S. [Laboratoire de Physique appliquee (LPA), Faculte des Sciences de Sfax, 3018, BP 802 (Tunisia); Bougzhala, H. [Laboratoire de cristallochimie et des materiaux, Faculte des Sciences de Tunis (Tunisia); Mlayah, A. [Centre d' Elaboration de Materiaux et d' Etudes Structurales, CNRS-Universite Paul Sabatier, 29 rue Jeanne Marvig, 31055 Toulouse, Cedex 4 (France); Chtourou, R. [Centre de Recherche et des Technologies de l' Energie CRTEn BP. 95, Hammam-Lif 2050, Laboratoire de Photovoltaique et de Semiconducteur (Tunisia); Abid, Y. [Laboratoire de Physique appliquee (LPA), Faculte des Sciences de Sfax, 3018, BP 802 (Tunisia)
2009-09-15
An organic-inorganic hybrid perovskite (C{sub 4}H{sub 9}NH{sub 3}){sub 4}Pb{sub 3}I{sub 4}Br{sub 6} was synthesized and studied by X-ray diffraction, Raman and infrared spectroscopies, optical transmission and photoluminescence. The title compound, abbreviated (C{sub 4}){sub 4}Pb{sub 3}I{sub 4}Br{sub 6}, crystallises in a periodic two-dimensional multilayer structure with P2{sub 1}/a space group. The structure is built up from alternating inorganic and organic layers. Each inorganic layer consists of three sheets of PbX{sub 6} (X=I, Br) octahedra. Raman and infrared spectra of the title compound were recorded in the 100-3500 and 400-4000 cm{sup -1} frequency ranges, respectively. An assignment of the observed vibration modes is reported. Optical transmission measurements, performed on thin films of (C{sub 4}){sub 4}Pb{sub 3}I{sub 4}Br{sub 6}, revealed two absorption bands at 474 and 508 nm. Photoluminescence measurements have shown a green emission peak at 519 nm.
Crystal structure of 1-isopropyl-4,7-dimethyl-3-nitronaphthalene
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Ahmed Benharref
2015-09-01
Full Text Available The title compound, C15H17NO2, was synthesized from a mixture of α-himachalene (2-methylene-6,6,9-trimethylbicyclo[5.4.01,7]undec-8-ene and β-himachalene (2,6,6,9-tetramethylbicyclo[5.4.01,7]undeca-1,8-diene, which were isolated from an oil of the Atlas cedar (Cedrus Atlantica. The naphthalene ring system makes dihedral angles of 68.6 (2 and 44.3 (2°, respectively, with its attached isopropyl C/C/C plane and the nitro group. In the crystal, molecules held together by a C—H...O interaction, forming a chain along [-101].
Crystal structure of 3-methyl-2,6-bis(4-methyl-1,3-thiazol-5-ylpiperidin-4-one
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A. Manimaran
2014-09-01
Full Text Available In the title compound, C14H17N3OS2, the central piperidinone ring adopts a chair conformation and the thiazole rings are inclined to its mean plane by 80.16 (12 and 67.15 (12°. The O atom and methyl group C atom deviate significantly from the mean plane of the central piperidinone ring, by 0.8138 (2 and 0.3175 (2 Å, respectively. The dihedral angle between the thiazole rings is 51.88 (13°. In the crystal, molecules are linked via C—H...O hydrogen bonds, forming zigzag C(10 chains running parallel to [001].
A comparative study of the progression of radiation pulmonary injury in C57BL/6J and C3H/HeN mice
International Nuclear Information System (INIS)
Liu Ying; Li Yang; Peng Ruiyun; Wang Shuming; Gao Yabing; Ma Junjie; Song Liangwen
2007-01-01
Objective: To compare the course of radiation pulmonary injury in C57BL/6J and C3H/HeN mice. Methods: C57BL/6J and C3H/HeN mice irradiated with 20 Gy 60 Co gamma rays were used as animal models. Sirius red staining and hydroxyproline measurement were used to detect the distribution of type I and III collagens and the content of pulmonary hydroxyproline. Immunohistochemistry was used to observe the changes of the expressions of fibronectin (FN) and laminin (LN) and alpha-smooth muscle actin (α-SMA) in the lung. Results: The changes in the lungs in C57BL/6J mice were as follows: the pathological changes undergone interstitial pneumonia, proliferation and fibrosis; significant increase of collagen deposition; FN increased rapidly to a significantly higher level at 1 and 3 months after irradiation than that in the control (P<0.01), and then decreased gradually to a normal level at 6 month after irradiation; LN elevated gradually after irradiation; the expressions of α-SMA were more intense than that in C3H/HeN mice. The changes in the lungs in C3H/HeN mice were as follows: the pathological changes mainly developed institial pneumonitis; no significant changes of FN expression was observed after irradiation compared to that in the control; LN increased significantly at 1 and 3 months after irradiation, and then decreased gradually. Conclusions: The models of radiation pulmonary fibrosis-sensitive and-resistant were established by irradiation with gamma rays, C57BL/6J mice developed late radiation pulmonary fibrosis, and were characterized by the significant accumulation of collagen. C3H/HeN mice did not develop radiation pulmonary fibrosis. (authors)
Bayar, I.; Khedhiri, L.; Soudani, S.; Lefebvre, F.; Pereira da Silva, P. S.; Ben Nasr, C.
2018-06-01
Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C8H12NO)·[NO3] (I), and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C8H14N4)·[ClO4]2(II), have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a = 15.7908 (7), b = 6.8032 (3), c = 8.7091 (4) Å, V = 935.60 (7) Å3 with Z = 4. Full-matrix least-squares refinement converged at R = 0.038 and wR(F2) = 0.115. Compound (II) belongs to the monoclinic system, space group P21/c with the following parameters: a = 10.798(2), b = 7.330(1), c = 21.186(2) Å, β = 120.641 (4)°, V = 1442.7 (3) Å3and Z = 4. The structure was refined to R = 0.044, wR(F2) = 0.132. In the structures of (I) and (II), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13C, 35Cl and 15N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands.
4-(1,3-Diphenyl-4,5-dihydro-1H-pyrazol-5-yl-1,3-diphenyl-1H-pyrazole
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Hoong-Kun Fun
2011-11-01
Full Text Available The title compound, C30H24N4, contains two pyrazole rings and four phenyl rings. The pyrazole rings are essentially planar, with maximum deviations of 0.003 (1 and 0.066 (1 Å and make a dihedral angle of 73.43 (6°. The two pyrazole rings make dihedral angles of 40.08 (6, 9.28 (6, 15.78 (8 and 17.25 (7° with their attached phenyl rings. In the crystal, there are no significant intermolecular hydrogen-bonding interactions. The crystal structure is stabilized by C—H...π interactions.
Dell'Amico, Daniela Belli; Calderazzo, Fausto; Marchetti, Fabio; Ramello, Stefano; Samaritani, Simona
2008-02-04
The hexanuclear Pd6Cl12, i.e., the crystal phase classified as beta-PdCl2, was obtained by reacting [TBA]2[Pd2Cl6] with AlCl3 (or FeCl3) in CH2Cl2. The action of AlCl3 on PtCl42-, followed by digestion of the resulting solid in 1,2-C2H4Cl2 (DCE), CHCl3, or benzene, produced Pt6Cl12.DCE, Pt6Cl12.CHCl3, or Pt6Cl12.C6H6, respectively. Treating [TBA]2[PtCl6] with a slight excess of AlCl3 afforded [TBA][Pt2Cl9], whose anion was established crystallographically to be constituted by two "PtCl6" octahedra sharing a face. Dehydration of H2PtCl6.nH2O with SOCl2 gave an amorphous compound closely analyzing as PtCl4, reactive with [Q]Cl in SOCl2 to yield [Q][Pt2Cl9] or [Q]2[Pt2Cl10], depending on the [Q]Cl/Pt molar ratio (Q=TBA+, PPN+). A single-crystal X-ray diffraction study has shown [PPN]2[Pt2Cl10].C7H8 to contain dinuclear anions formed by two edge-sharing PtCl6 octahedra.
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
3,5-Dimethyl-4-nitroso-1H-pyrazole
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Inna Safyanova
2011-09-01
Full Text Available In the unit cell of the title compound, C5H7N3O, there are two conformers (A and B which differ in the position of the oxime group with respect to the protonated pyrazole nitrogen (trans in the A conformer and cis in the B conformer and in the geometric parameters. The oxime group exists in the nitroso form in both conformers. In the crystal, molecules are linked by intermolecular N—H...O and N—H...N hydrogen bonds into zigzag-like chains along the b axis.
9-Benzyl-6-benzylsulfanyl-9H-purin-2-amine
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Maywan Hariono
2014-03-01
Full Text Available In the title compound, C19H17N5S, the dihedral angles between the purine ring system (r.m.s. deviation = 0.009 Å and the S-bound and methylene-bound phenyl rings are 74.67 (8 and 71.28 (7°, respectively. In the crystal, inversion dimers linked by pairs of N—H...N hydrogen bonds generate R22(8 loops. C—H...N interactions link the dimers into (100 sheets.
4-Phenethylthio-2-phenylpyrazolo[1,5-a][1,3,5]triazin-7(6H-one
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Sergey A. Smolnikov
2017-12-01
Full Text Available Exploring the pharmacologically important pyrazolo[1,5-a][1,3,5]triazin-7(6H-one scaffold for the construction of new bioactive compounds, we developed a synthesis of 4-phenethylthio-2-phenylpyrazolo[1,5-a][1,3,5]triazin-7(6H-one (4 via S-alkylation of 2-phenyl-4-thioxopyrazolo[1,5-a][1,3,5]triazine-7(6H-one (3, prepared by the double ring closure of pyrazole and triazine rings upon the treatment of 1-cyanoacetyl-4-benzoylthiosemicarbazide (2 with alkali. The antiproliferative activity of 4 against human lung cancer (A549 and human breast cancer (MDA-MB231 cell lines was investigated. Compound 4 was found to be more active against lung cancer cells than breast cancer cells.
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Palanikumar Maniam
2011-06-01
Full Text Available Hydrothermal reaction involving zinc nitrate hexahydrate, trisodium benzene-1,3,5-tricarboxylate (Na3BTC and 2-methylimidazole (2-MeImH yielded the title compound, [Zn2(C9H3O6(C4H5N2(C4H6N23]. In this mixed-ligand metal-organic compound, Zn2+ ions are coordinated by N atoms from 2-MeImH molecules and (2-MeIm− ions, as well as by O atoms from (BTC3− ions. This results in two different distorted tetrahedra, viz. ZnN3O and ZnN2O2. These tetrahedra are interconnected via (BTC3− ions and N:N′-bridging (2-MeIm− ions, thus forming a layered structure in the bc plane. Hydrogen bonds between the O atoms of carboxylate ions and NH groups of 2-MeImH ligands link the layers into a three-dimensional structure.
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Fatih Şen
2017-05-01
Full Text Available In the present study, a combined experimental and computational study on molecular structure and spectroscopic characterization on the title compound has been reported. The crystal was synthesized and its molecular structure brought to light by X-ray single crystal structure determination. The spectroscopic properties of the compound were examined by FT-IR and NMR (1H and 13C techniques. FT-IR spectra of the target compound in solid state were observed in the region 4000–400 cm−1. The 1H and 13C NMR spectra were recorded in CDCl3 solution. The molecular geometries were those obtained from the X-ray structure determination optimized using the density functional theory (DFT/B3LYP method with the 6-31G(d, p and 6-31G+(d, p basis set in ground state. From the optimized geometry of the molecule, geometric parameters (bond lengths, bond angles and torsion angles, vibrational assignments and chemical shifts of the title compound have been calculated theoretically and compared with those of experimental data. Besides, molecular electrostatic potential (MEP, frontier molecular orbitals (FMOs, Mulliken population analysis, Thermodynamic properties and non-linear optical (NLO properties of the title molecule were investigated by theoretical calculations.
International Nuclear Information System (INIS)
Gao, Zhen-Fei; Di, You-Ying; Liu, Su-Zhou; Lu, Dong-Fei; Dou, Jian-Min
2014-01-01
Graphical abstract: A novel coordination compound sodium pyruvate C 3 H 3 O 3 Na(s) is synthesised. Elemental analysis and X-ray crystallography are used to characterise the composition and crystal structure of the compound. The lattice potential energy and ionic volume of the anion are obtained from crystallographic data. The standard molar enthalpy of formation of the compound is calculated by an isoperibol solution-reaction calorimeter. Molar enthalpies of dissolution of the compound at various molalities are measured at T = 298.15 K. According to Pitzer’s theory, molar enthalpy of dissolution of the title compound at infinite dilution is calculated. The values of relative apparent molar enthalpies and relative partial molar enthalpies of the solvent and the compound at different concentrations m/(mol · kg −1 ) are derived. - Highlights: • The sodium pyruvate was synthesised and crystal structure was determined. • The enthalpy change of the synthesis reaction was obtained. • Standard molar enthalpy of formation was obtained. • Molar enthalpy of dissolution at infinite dilution was calculated. - Abstract: A novel coordination compound sodium pyruvate C 3 H 3 O 3 Na(s) is synthesised by a liquid phase reaction. The compound has an obvious bioactivity and can be used as the biological carbon source and the chemical identification of primary and secondary alcohols. It can be also used to determinate transaminase. Elemental analysis and X-ray crystallography are used to characterise the composition and crystal structure of the compound. Single crystal X-ray analysis reveals that the compound is formed by one CH 3 COCOO − anion and one Na + cation. An obvious feature of the crystal structure is the formation of the five-membered chelate ring by the coordination of O1 of carboxylate and O3 of keto form with Na + cation, and it is good for the stability of the compound in structure. The lattice potential energy and ionic volume of the anion are obtained
Design, synthesis and molecular docking study of thienopyrimidin-4(3H-thiones as antifungal agents
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Sanjay B. Bari
2017-01-01
Full Text Available In an attempt to find a new class of antimicrobial agents, a series of thienopyrimidin-4(3H-thiones 4(H1–H36 were synthesized and evaluated for in vitro antifungal activity against Candida albicans (NCIM 3471, Aspergillus niger (NCIM 545, and Penicillium chrysogenum (NCIM 709. The title compounds were synthesized by thionation of thienopyrimidin-4(3H-ones 3(H1–H36 using Lawesson’s reagent. All the compounds were characterized using elemental analytical (C, H, and N and spectral (FT-IR, 1H NMR, 13C NMR and MS data. Among the tested compounds, 5-(4-chlorophenyl-2-(pyridin-3-ylthieno[2,3-d]pyrimidine-4(3H-thione 4(H11, 2-sulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H18, and 2-(butylsulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H32 were identified as potentially excellent antifungal agents. They exhibited potent antifungal activity against C. albicans (MIC; 4 μg/mL, A. niger (MIC; 2 μg/mL, and P. chrysogenum (MIC; 2 μg/mL comparable with that of ketoconazole. The binding mode of compounds by SP docking studies shows that it fits well into the active site cavity of DHFR. Lipinski’s rule and in silico ADME pharmacokinetic parameters are within the acceptable range defined for human use thereby indicating their potential as drug-like molecules.
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S. Sriman Narayanan
2008-09-01
Full Text Available In the title compound, C29H26N2O2, one of the pyrrolidine rings in the pyrrolizine system is disordered, with site occupancies of ca 0.55 and 0.45. Both components of the disordered pyrrolidine ring adopt envelope conformations, whereas the other pyrrolidine ring adopts a twist conformation. The molecules are linked into centrosymmetric dimers by N—H...O hydrogen bonds and the dimers are connected via C—H...π interactions.
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Guozheng Zhao
2013-01-01
Full Text Available The B3LYP/6-31G (d density functional theory (DFT method was used to study molecular geometry, electronic structure, infrared spectrum (IR and thermodynamic properties. Heat of formation (HOF and calculated density were estimated to evaluate detonation properties using Kamlet-Jacobs equations. Thermal stability of 3,6,7,8-tetranitro-3,6,7,8-tetraaza-tricyclo [3.1.1.1(2,4]octane (TTTO was investigated by calculating bond dissociation energy (BDE at the unrestricted B3LYP/6-31G(d level. Results showed the N-NO2 bond is a trigger bond during the thermolysis initiation process. The crystal structure obtained by molecular mechanics (MM methods belongs to P2(1/C space group, with cell parameters a = 8.239 Å, b = 8.079 Å, c = 16.860 Å, Z = 4 and r = 1.922 g cm-3. Both detonation velocity of 9.79 km s-1 and detonation pressure of 44.22 GPa performed similarly to CL-20. According to the quantitative standards of energetics and stability, TTTO essentially satisfies this requirement as a high energy density compound (HEDC.
Dibromido(6-methyl-2,2′-bipyridine-κ2N,N′zinc(II
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Vahid Amani
2010-10-01
Full Text Available In the title compound, [ZnBr2(C11H10N2], the ZnII atom is four-coordinated in a distorted tetrahedral configuration by two N atoms from a 6-methyl-2,2′-bipyridine ligand and two terminal Br atoms. Weak intermolecular C—H...Br hydrogen bonds and π–π stacking interactions between the pyridine rings [centroid–centroid distances = 3.763 (5 and 3.835 (6 Å] contribute to crystal-packing effects.
International Nuclear Information System (INIS)
Mandal, Sukhendu; Natarajan, Srinivasan
2005-01-01
A hydrothermal reaction of a mixture of cobalt (II) oxalate, phosphorous acid, piperazine and water at 150 o C for 96h followed by heating at 180 o C for 24h gave rise to a new inorganic-organic hybrid solid, [C 4 N 2 H 12 ][Co 4 (HPO 3 ) 2 (C 2 O 4 ) 3 ], I. The structure consists of edge-shared CoO 6 octahedra forming a [Co 2 O 10 ] dimers that are connected by HPO 3 and C 2 O 4 units forming a three-dimensional structure with one-dimensional channels. The amine molecules are positioned within these channels. The oxalate units have a dual role of connecting within the plane of the layer as well as out of the plane. Magnetic susceptibility measurement shows the compound orders antiferromagnetically at low temperature (T N =22K). Crystal data: I, monoclinic, space group=P2 1 /c (No. 14). a=7.614(15), b=7.514(14), c=17.750(3)A, β=97.351(3) o , V=1007.30(3)A 3 , Z=2, ρ calc =2.466g/cm 3 , μ (MoKα) =3.496mm -1 , R 1 =0.0310 and wR 2 =0.0807 data [I>2σ(I)
Kumar, Praveen; Tripathi, Laxmi
2012-05-01
A series of 2-(1H-Benzotriazol-1-yl)-N'-[substituted]acetohydrazides were designed & synthesized keeping in view the structural requirement of pharmacophore and evaluated for anticonvulsant activity and neurotoxicity. The new compounds were characterized using FT-IR, 1H NMR, mass spectral data and elemental analysis. The anticonvulsant activity of the titled compounds was assessed using the 6 Hz psychomotor seizure test. The neurotoxicity was assessed using the rotorod method. The most active compound of the series was N'-[4-(1,3-Benzodioxol-5-yloxy)benzylidene]-2-(1H-benzotriazol-1-yl)acetohydrazide (BTA 9), which showed good activity with 75 % protection (3/4, 0.5 h) at a dose of 100 mg/kg in mice. All the compounds exhibited no neurotoxicity. A computational study was carried out for calculation of pharmacophore pattern and prediction of pharmacokinetic properties. Titled compounds have also exhibited good binding properties with epilepsy molecular targets such as glutamate, GABA (A) delta, GABA (A) alpha-1 receptors and Na/H exchanger, in Lamarckian genetic algorithm based flexible docking studies.
4-Chloroselanyl-3,5-diethyl-1H-pyrazol-2-ium chloride
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Maksym Seredyuk
2011-11-01
Full Text Available In the cation of the title compound, C7H12ClN2Se+·Cl−, the ethylene groups and the Se–Cl fragment adopt a cis configuration with a C—Se—Cl angle of 96.09 (6°. In the crystal, intermolecular N—H...Cl hydrogen bonds link two cations and two chlorine anions into centrosymmetric clusters. π–π interactions between the pyrazole rings [centroid–centroid distance of 3.530 (2 Å] link these clusters into columns along [001] with short intermolecular Se...Cl− contacts of 2.995 (1 Å.
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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
Experimental and theoretical studies of the C{sub 6}H{sub 5} + C{sub 6}H{sub 6} reaction
Energy Technology Data Exchange (ETDEWEB)
Park, J.; Burova, S.; Rodgers, A.S.; Lin, M.C.
1999-11-11
The absolute rate constants for the C{sub 6}H{sub 5} + C{sub 6}H{sub 6} and C{sub 6}D{sub 6} reactions have been measured by cavity ringdown spectrometry at temperatures between 298 and 495 K at a constant 40 Torr Ar pressure. The new results, which reveal no detectable kinetic isotopic effect, can be represented by the Arrhenius equation, {kappa}{sub 1} = 10{sup (11.91{+-}0.13)} exp[{minus}(2,102 {+-} 106)/T] cm{sup 3}/(mol s). Low-temperature data for the addition/stabilization process, C{sub 6}H{sub 5} + C{sub 6}H{sub 6} {r{underscore}arrow} C{sub 12}H{sub 11}, can be correlated with those obtained in a low-pressure, high-temperature Knudsen cell study for the addition/displacement reaction, C{sub 6}H{sub 5} + C{sub 6}H{sub 6} {r{underscore}arrow} C{sub 12}H{sub 10} + H, by the RRKM theory using the molecular and transition-state parameters computed at the B3LYP/6-311G(d,p) level of theory. Combination of these two sets of data gives {kappa}{sub 1} = 10{sup (11.98{+-}0.03)} exp[{minus}(2168 {+-} 34)/T] cm{sup 3}/(mol s) covering the temperature range 298--1,330 K. The RRKM theory also correlates satisfactorily the forward reaction data with the high-temperature shock-tube result for the reverse H-for-C{sub 6}H{sub 5} substitution process with 2.7 and 4.7 kcal/mol barriers for the entrance (C{sub 6}H{sub 5} + C{sub 6}H{sub 6}) and reverse (H + C{sub 12}H{sub 10}) reactions, respectively. For modeling applications, the authors have calculated the forward reaction rate constants for the formation of the two competing products, H + C{sub 12}H{sub 10} and C{sub 12}H{sub 11}, at several pressures covering 300 K {lt} T {lt} 2,500 K.
2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate
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Guoquan Zhou
2012-04-01
Full Text Available The title compound, C6H7O2S3+·BF4−, consists of a planar 2-thioxo-1,3-dithiol-4,5-yl unit [maximum deviation from the ring plane = 0.020 (3 Å], with an ethylenedioxy group fused at the 4,5-positions; the ethylenedioxy C atoms are disordered over two positions with site-occupancy factors of 0.5. The 1,4-dioxine ring has a twist-chair conformation. Weak cation–anion S...F interactions [3.022 (4–3.095 (4 Å] and an S...O [3.247 (4 Å] interaction are present.
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Mohammad Hossein Mosslemin
2009-06-01
Full Text Available The asymmetric unit of the title compound, C16H12ClF3N2O3S·H2O, contains two crystallographically independent organic molecules and two water molecules. The organic species are linked by an intermolecular O—H...O hydrogen bond, while the water molecules are connected to them through intermolecular O—H...N hydrogen bonds. The thiophene and phenyl rings are oriented at dihedral angles of 62.35 (4 in the first independent molecule and 60.74 (5° in the second, while the pyrimidine rings adopt twisted conformations in both molecules. Intramolecular N—H...F interactions result in the formation of two five-membered rings having envelope conformations. In the crystal structure, further intermolecular O—H...O and N—H...O hydrogen bonds link the molecules into chains.
International Nuclear Information System (INIS)
Parker, R.F.
1987-01-01
The studies reported here used genetic differences in susceptibility of C57BL/6N and C3H/HeN mice and exacerbation of the disease by nitrogen dioxide (NO 2 ) as tools in assessing the role of early host responses in the pathogenesis of MRM. The two strains did not differ in susceptibility to infection, but C3H/HeN mice were more susceptible to and had increased severity of lung lesions 14 days after intranasal inoculation as determined by 50% biological endpoints and morphometric analysis of tissues. Exposure to NO 2 for 4 hours prior to exposure to infectious aerosols exacerbated murine respiratory mycoplasmosis (MRM) by 7 days after exposure in both mouse strains. NO 2 appeared to affect host lung defense mechanisms responsible for limiting mycoplasmal growth in the lungs. The NO 2 exposure concentration required for this effect varied with the genetic background of the host, the dose of mycoplasmas administered, and the endpoint measured. Pulmonary clearance of radiolabeled M. pulmonis was determined in both mouse strains, and in C57BL/6N mice exposed to NO 2
Ahmed, Houssem Eddine; Kamoun, Slaheddine
2017-09-01
The crystal structure of (C6H20N3)SbCl5·Cl·H2O is built up of [NH3(CH2)3NH2(CH2)3NH3]3 + cations, [SbCl5]2 - anions, free Cl- anions and neutral water molecules connected together by Nsbnd H ⋯ Cl, Nsbnd H ⋯ O and Osbnd H ⋯ Cl hydrogen bonds. The optical band gap determined by diffuse reflection spectroscopy (DRS) is 3.78 eV for a direct allowed transition. Optimized molecular geometry, atomic Mulliken charges, harmonic vibrational frequencies, HOMO-LUMO and related molecular properties of the (C6H20N3)SbCl5·Cl·H2O compound were calculated by Density functional theory (DFT) using B3LYP method with GenECP sets. The calculated structural parameters (bond lengths and angles) are in good agreement with the experimental XRD data. The vibrational unscaled wavenumbers were calculated and scaled by a proper scaling factor of 0.984. Acceptable consistency was observed between calculated and experimental results. The assignments of wavenumbers were made on the basis of potential energy distribution (PED) using Vibrational Energy Distribution Analysis (VEDA) software. The HOMO-LUMO study was extended to calculate various molecular parameters like ionization potential, electron affinity, global hardness, electro-chemical potential, electronegativity and global electrophilicity of the given molecule.
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S. Subasri
2017-02-01
Full Text Available The title compounds, C16H15N5OS, (I, and C12H12FN5OS, (II, are [(diaminopyrimidinesulfanyl]acetamide derivatives. In (I, the pyrimidine ring is inclined to the naphthalene ring system by 55.5 (1°, while in (II, the pyrimidine ring is inclined to the benzene ring by 58.93 (8°. In (II, there is an intramolecular N—H...N hydrogen bond and a short C—H...O contact. In the crystals of (I and (II, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with R22(8 ring motifs. In the crystal of (I, the dimers are linked by bifurcated N—H...(O,O and C—H...O hydrogen bonds, forming layers parallel to (100. In the crystal of (II, the dimers are linked by N—H...O hydrogen bonds, also forming layers parallel to (100. The layers are linked by C—H...F hydrogen bonds, forming a three-dimensional architecture.
International Nuclear Information System (INIS)
Safronov, A.V.; Sokolova, M.N.; Vorontsov, E.V.; Petrovskij, P.V.; Barakovskaya, I.G.; Chizhevskij, I.T.
2004-01-01
New closo-(η 2 ,η 3 -(4-vinylcyclopentene-3-yl)rhodacarboranes were prepared by reaction of the complex [(η 4 -C 7 H 8 )RhCl] 2 (C 7 H 8 -norbornadiene) with salts of substituted nido-dicarbaundecaborates [K][nido-7-R 1 -8-R 2 -7,8-C 2 B 9 H 10 ] (R 1 =R 2 =H (a); R = R 2 =Me (b); R 1 , R 2 =1',2'-(CH 2 ) 2 C 6 H 4 (c); R 1 =Me, R 2 =Ph (d) in CH 2 Cl 2 . The structure of the compounds prepared in solution was studied by the method of multinuclear NMR spectroscopy. A probable mechanism of the norbornadiene ligand regrouping was suggested [ru
(E-5,6-Dimethoxy-2-(pyridin-4-ylmethylidene-2,3-dihydro-1H-inden-1-one
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Mohamed Ashraf Ali
2010-11-01
Full Text Available The molecule of the title compound, C17H15NO3, is slightly twisted, with a dihedral angle of 12.12 (3° between the dihydroindenone group and the pyridine ring. In the crystal, molecules are connected into layers parallel to the ab plane via intermolecular C—H...O hydrogen bonds. Weak π–π [centroid–centroid distance = 3.5680 (6 Å] interactions are also observed.
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Xin-Ping Kang
2010-11-01
Full Text Available In the title layered coordination polymer, {[Cd(C17H18F2N3O3(C8H4O4]·3H2O}n, the CdII atom exhibits a very distorted CdO6 octahedral geometry defined by one O3,O4-bidentate 1-ethyl-6,8-difluoro-7-(3-methylpiperazin-1-yl-4-oxo-1,4-dihydroquinoline-3-carboxylate (lome ligand, one O,O′-bidentate benzene-1,4-dicarboxylate (bdc dianion and two O-monodentate bdc dianions. Both the bdc species in the asymmetric unit are completed by crystallographic inversion symmetry. The bridging bdc dianions link the cadmium nodes into a rectangular grid lying parallel to (01overline{1}. A network of N—H...O and O—H...O hydrogen bonds helps to establish the packing.
N,N′-Bis(3β-acetoxy-5α-cholest-6-ylidenehydrazine
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Zishan Tabassum
2011-02-01
Full Text Available The asymmetric unit of the title compound, C58H96N2O4, contains two crystallographically independent molecules. All cyclohexane rings are in chair conformations, while the furan ring is in an envelope conformation in one molecule and a twist conformation in the other. Two acetaldehyde and one isobutane groups are disordered over two orientations with refined site occupancies of 0.940 (4:0.060 (4 and 0.791 (7:0.209 (7, respectively. In the crystal, molecules are stacked along the a axis through van der Waals interactions.
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Alain Igau
2013-12-01
Full Text Available In the cation of the title complex, [Ru(C31H32N3P2(C10H8N22](PF6(Br2·2CH2Cl2·H2O, the ruthenium ion is coordinated in a distorted octahedral geometry by two 2,2′-bipyridine (bpy ligands and a chelating cationic N-diphenylphosphino-1,3,4,6,7,8-hexahydro-2-pyrimido[1,2-a]pyrimidine [(PPh22-hpp] ligand. The tricationic charge of the complex is balanced by two bromide and one hexafluoridophosphate counter-anions. The compound crystallized with two molecules of dichloromethane (one of which is equally disordered about a Cl atom and a water molecule. In the crystal, one of the Br anions bridges two water molecules via O—H...Br hydrogen bonds, forming a centrosymmetric diamond-shaped R42(8 motif. The cation and anions and the solvent molecules are linked via C—H...F, C—H...Br, C—H...Cl and C—H...O hydrogen bonds, forming a three-dimensional network.
Crystal structure of 1-methyl-4-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine
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Mohammed El Fal
2014-12-01
Full Text Available In the title compound, C7H8N4S, the non-H atoms of the pyrazolo[3,4-d]pyrimidine ring system and the methylsulfanyl group lie on a crystallographic mirror plane. In the crystal, molecules are linked via a number of π–π interactions [centroid–centroid distances vary from 3.452 (7 to 3.6062 (8 Å], forming a three-dimensional structure.
Hughes, Michael J; Gerken, Michael; Mercier, Hélène P A; Schrobilgen, Gary J
2010-06-07
Dissolution of the infinite chain polymer, (OsO(3)F(2))(infinity), in CH(3)CN solvent at -40 degrees C followed by solvent removal under vacuum at -40 degrees C yielded fac-OsO(3)F(2)(NCCH(3)).nCH(3)CN (n >/= 2). Continued pumping at -40 degrees C with removal of uncoordinated CH(3)CN yielded fac-OsO(3)F(2)(NCCH(3)). Both fac-OsO(3)F(2)(NCCH(3)).nCH(3)CN and fac-OsO(3)F(2)(NCCH(3)) are yellow-brown solids and were characterized by low-temperature (-150 degrees C) Raman spectroscopy. The crystal structure (-173 degrees C) of fac-OsO(3)F(2)(NCCH(3)).2CH(3)CN consists of two co-crystallized CH(3)CN molecules and a pseudo-octahedral OsO(3)F(2).NCCH(3) molecule in which three oxygen atoms are in a facial arrangement and CH(3)CN is coordinated trans to an oxygen atom in an end-on fashion. The Os---N bond length (2.205(3) A) is among the shortest M---N adduct bonds observed for a d(0) transition metal oxide fluoride. The (19)F NMR spectrum of (OsO(3)F(2))(infinity) in CH(3)CN solvent (-40 degrees C) is a singlet (-99.6 ppm) corresponding to fac-OsO(3)F(2)(NCCH(3)). The (1)H, (15)N, (13)C, and (19)F NMR spectra of (15)N-enriched OsO(3)F(2)(NCCH(3)) were recorded in SO(2)ClF solvent (-84 degrees C). Nitrogen-15 enrichment resulted in splitting of the (19)F resonance of fac-OsO(3)F(2)((15)NCCH(3)) into a doublet ((2)J((15)N-(19)F), 21 Hz). In addition, a doublet of doublets ((2)J((19)F(ax)-(19)F(eq)), 134 Hz; (2)J((15)N-(19)F(eq)), 18 Hz) and a doublet ((2)J((19)F(ax)-(19)F(eq)), 134 Hz) were observed in the (19)F NMR spectrum that have been assigned to mer-OsO(3)F(2)((15)NCCH(3)); however, coupling of (15)N to the axial fluorine-on-osmium environment could not be resolved. The nitrogen atom of CH(3)CN is coordinated trans to a fluorine ligand in the mer-isomer. Quantum-chemical calculations at the SVWN and B3LYP levels of theory were used to calculate the energy-minimized gas-phase geometries, vibrational frequencies of fac- and mer-OsO(3)F(2)(NCCH(3)) and of CH(3)CN. The
1-(4,5-Dinitro-10-azatricyclo[6.3.1.02,7]dodeca-2,4,6-trien-10-yl-2,2,2-trifluoroethanone
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Jin-Tang Wang
2008-12-01
Full Text Available In the title compound, C13H10F3N3O5, a derivative of andrographolide, the five-membered ring adopts an envelope conformation, while the non-planar six-membered ring has a chair conformation. An intramolecular C—H...F hydrogen bond results in the formation of a non-planar six-membered ring adopting a twisted conformation. In the crystal structure, intermolecular C—H...O hydrogen bonds link the molecules into centrosymmetric dimers.
Synthesis and structure of [(NH2)2CSSC(NH2)2]2[OsBr6]Br2 . 3H2O
International Nuclear Information System (INIS)
Rudnitskaya, O. V.; Kultyshkina, E. K.; Stash, A. I.; Glukhova, A. A.; Venskovskii, N. U.
2008-01-01
The complex [(NH 2 ) 2 CSSC(NH 2 ) 2 ] 2 [OsBr 6 ]Br 2 . 3H 2 O is synthesized by the reaction of K 2 OsBr 6 with thiocarbamide in concentrated HBr and characterized using electronic absorption and IR absorption spectroscopy. Its crystal structure is determined by X-ray diffraction. The crystals are orthorhombic, a = 11.730(2) A, b = 14.052(3) A, c = 16.994(3) A, space group Cmcm, and Z = 4. The [OsBr 6 ] 2- anionic complex has an octahedral structure. The Os-Br distances fall in the range 2.483-2.490 A. The α,α'-dithiobisformamidinium cation is a product of the oxidation of thiocarbamide. The S-S and C-S distances are 2.016 and 1.784 A, respectively. The H 2 O molecules, Br - ions, and NH 2 groups of the cation are linked by hydrogen bonds.
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Jin-Xia Mu
2015-12-01
Full Text Available The title compound 4-(5-((4-bromobenzylthio-4-phenyl-4H-1,2,4-triazol-3-ylpyridine (C20H15BrN4S was synthesized, and its structure was confirmed by 1H NMR, MS and elemental analyses and single-crystal X-ray structure determination. It crystallizes in the triclinic space group P-1 with a = 7.717(3, b = 9.210(3, c = 13.370(5 Å, α = 80.347(13, β = 77.471(13, γ = 89.899(16°, V = 913.9(6 Å3, Z = 2 and R = 0.0260 for 3145 observed reflections with I > 2σ(I. A Density functional theory (DFT (B3LYP/6-31G calculation of the title molecule was carried out. The full geometry optimization was carried out using a 6-31G basis set, and the frontier orbital energy. Atomic net charges are discussed. Calculated bond lengths and bond angles were found to differ from experimental values, and the compound exhibits moderate antifungal activity.
International Nuclear Information System (INIS)
Polyanskaya, T.M.
2006-01-01
A monocrystal X-ray diffraction study of a new iodine-containing cluster compound 9-(pyridine)-11-iodo-decahydro-7,8-dicarba-nido-undecaborane [9-C 5 H 5 N-11-I-7,8-C 2 B 9 H 10 ] has been performed. Crystal data: C 7 H 15 B 9 NI, M = 337.39, monoclinic, space group P2 1 /c, unit cell parameters: a=9.348(1) A, b=11.159(1) A, c=13.442(2) A, β=98.13(1) deg, V=1388.1(5) A 3 , Z=4, d calc = 1.614 g/cm 3 , T = 295 K, F(000)=648, μ=2.276 mm -1 . The structure was solved by a direct method and refined in the full-matrix anisotropic approximation (isotropic for hydrogen atoms) to final agreement factors R 1 = 0.0254, wR 2 = 0.0454 for 2437 I hkl >2σ I from 3590 measured I hkl (an Enraf-Nonius CAD-4 diffractometer, λMoK α , graphite monochromator, θ/2θ-scanning). The molecules are joined into a supramolecular assembly by hydrogen bonds X-H...I (X = B, C) [ru
Crystal structure of 4-allylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine
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Mohammed El Fal
2014-09-01
Full Text Available In the title compound, C8H8N4S, the pyrazolo[3,4-d]pyrimidine ring system is essentially planar, with a maximum deviation from the mean plane of 0.025 (3 Å. The allyl group is disordered over two sites in a 0.512 (6:0.488 (6 ratio. In the crystal, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(8 graph-set motif.
Monegan, Jessie D; Bunge, Scott D
2009-04-06
The synthesis and structural characterization of several 1,1,3,3-tetramethylguanidine (H-TMG) solvated magnesium aryloxide complexes are reported. Bu(2)Mg was successfully reacted with H-TMG, HOC(6)H(3)(CMe(3))(2)-2,6 (H-DBP), and either ethanol, a carboxylic acid, or diphenyl phosphate in a 1:1 ratio to yield the corresponding [Mg(mu-L)(DBP)(H-TMG)](2) where L = OCH(2)CH(3) (OEt, 1), O(2)CC(CH(3))(3) (OBc, 2), O(2)C(C(6)H(2)-2,4,6-(CH(3))(3)) (TMBA, 3), or O(2)P(OC(6)H(5))(2) (DPP, 4). Bu(2)Mg was also reacted with two equivalents of H-TMG and HOC(6)H(3)(CMe(3))-2-(CH(3))-6 (BMP) or HO-2,6-Ph(2)C(6)H(3) to yield [Mg(BMP)(2)(H-TMG)(2)] (5) and [Mg(O-2,6-Ph(2)C(6)H(3))(2)(H-TMG)(2)] (6). Compounds 1-6 were characterized by single-crystal X-ray diffraction. Polymerization of l- and rac-lactide with 1 was found to generate polylactide (PLA). A discussion concerning the relevance of compounds 2 - 4 to the structure of Mg-activated phosphatase enzymes is also provided. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, FT-IR spectroscopy, and (1)H, (13)C and (31)P NMR studies.
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R. A. Nagalakshmi
2015-01-01
Full Text Available In the title compounds, C24H22BrN3, (I, and C24H22ClN3, (II, the 2-aminopyridine ring is fused with a cycloheptane ring, which adopts a half-chair conformation. The planes of the phenyl and benzene rings are inclined to that of the central pyridine ring [r.m.s. deviations = 0.0083 (1 and 0.0093 (1 Å for (I and (II, respectively] by 62.47 (17 and 72.51 (14°, respectively, in (I, and by 71.44 (9 and 54.90 (8°, respectively, in (II. The planes of the aromatic rings are inclined to one another by 53.82 (17° in (I and by 58.04 (9° in (II. In the crystals of both (I and (II, pairs of N—H...Nnitrile hydrogen bonds link the molecules, forming inversion dimers with R22(12 ring motifs. In (I, the resulting dimers are connected through C—H...Br hydrogen bonds, forming sheets parallel to (10-1, and π–π interactions [inter-centroid distance = 3.7821 (16 Å] involving inversion-related pyridine rings, forming a three-dimensional network. In (II, the resulting dimers are connected through π–π interactions [inter-centroid distance = 3.771 (2 Å] involving inversion-related pyridine rings, forming a two-dimensional network lying parallel to (001.
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Svitlana V. Shishkina
2014-07-01
Full Text Available The title solvate, C20H14N4O4S·C3H7NO, comprises a stereogenic centre but the centrosymmetric space group causes the presence of the racemate in the crystal. The spiro-joined fragments are almost orthogonal, with a dihedral angle of 86.8 (2° between the mean planes of the pyrane ring and the dihydroindolone ring system. The atoms of the indolinone bicycle are coplanar, with an r.m.s. deviation of 0.005 Å. In the crystal, pairs of N—H...O hydrogen bonds link the molecules into centrosymmetric dimers which are linked to the dimethylformamide solvent molecules by further N—H...O hydrogen bonds. N—H...N hydrogen bonds link neighbouring dimers into [010] chains.
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Mohamed I. Attia
2013-12-01
Full Text Available 5-Alkyl-6-(substituted benzyl-2-thiouracils 3a,c were reacted with (2-chloroethyl diethylamine hydrochloride to afford the corresponding 2-(2-diethylaminoethylthiopyrimidin- 4(3H-ones 4a,b. Reaction of 3a–c with N-(2-chloroethylpyrrolidine hydrochloride and/or N-(2-chloroethylpiperidine hydrochloride gave the corresponding 2-[2-(pyrrolidin-1-ylethyl]-thiopyrimidin-4(3H-ones 5a–c and 2-[2-(piperidin-1-ylethyl]thiopyrimidin-4(3H-ones 6a,b, respectively. Treatment of 3a–d with N-(2-chloroethylmorpholine hydrochloride under the same reaction conditions formed the corresponding 2-[2-(morpholin-4-ylethyl]thiopyrimidines 6c–f. On the other hand, 3a,b were reacted with N-(2-bromoethylphthalimide and/or N-(3-bromopropylphthalimide to furnish the corresponding 2-[2-(N-phthalimidoethyl]-pyrimidines 7a,b and 2-[3-(N-phthalimido-propyl]pyrimidines 7c,d, respectively. Compounds 3a–d, 4a,b, 5a–c, 6a–f and 7a–d were screened against Gram-positive bacteria (Staphylococcus aureus ATCC 29213, Bacillus subtilis NRRL 4219 and Bacillus cereus, yeast-like pathogenic fungus (Candida albicans ATCC 10231 and a fungus (Aspergillusniger NRRL 599. The best antibacterial activity was displayed by compounds 3a, 3b, 4a, 5a, 5b, 6d, 6f, 7b and 7d, whereas compounds 4b, 5b, 5c, 6a, 6b and 6f exhibited the best antifungal activity.
Ethyl 2-(6-bromo-2-phenyl-1H-imidazo[4,5-b]pyridin-1-ylacetate
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Mohammed Yassin Hjouji
2016-05-01
Full Text Available In the title compound, C16H14BrN3O2, the fused-ring system is essentially planar, with the largest deviation from the mean plane being 0.0216 (15 Å for the substituted N atom of the five-membered ring, the plane of which makes dihedral angles of 28.50 (7 and 77.48 (7° with the terminal phenyl ring and the ethoxycarbonylmethyl group mean planes, respectively. In the crystal, C—H...N hydrogen bonds link the molecules into inversion dimers. These combine with weak C—H...N contacts to stack the molecules into columns along the b-axis direction.
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Fortune Ezemobi
2014-12-01
Full Text Available The title compounds, C9H7NO3, (1, C10H7NO5, (2, and C14H9NO5, (3, are three potentially anticonvulsant compounds. Compounds (1 and (2 are isoindoline derivatives and (3 is an isoquinoline derivative. Compounds (2 and (3 crystallize with two independent molecules (A and B in their asymmetric units. In all three cases, the isoindoline and benzoisoquinoline moieties are planar [r.m.s. deviations are 0.021 Å for (1, 0.04 and 0.018 Å for (2, and 0.033 and 0.041 Å for (3]. The substituents attached to the N atom are almost perpendicular to the mean planes of the heterocycles, with dihedral angles of 89.7 (3° for the N—O—Cmethyl group in (1, 71.01 (4 and 80.00 (4° for the N—O—C(=OO—Cmethyl groups in (2, and 75.62 (14 and 74.13 (4° for the same groups in (3. In the crystal of (1, there are unusual intermolecular C=O...C contacts of 2.794 (1 and 2.873 (1 Å present in molecules A and B, respectively. There are also C—H...O hydrogen bonds and π–π interactions [inter-centroid distance = 3.407 (3 Å] present, forming slabs lying parallel to (001. In the crystal of (2, the A and B molecules are linked by C—H...O hydrogen bonds, forming slabs parallel to (10-1, which are in turn linked via a number of π–π interactions [the most significant centroid–centroid distances are 3.4202 (7 and 3.5445 (7 Å], forming a three-dimensional structure. In the crystal of (3, the A and B molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure, which is consolidated by π–π interactions [the most significant inter-centroid distances are 3.575 (3 and 3.578 (3 Å].
Bis(3-acetyl-6-methyl-2-oxo-2H-pyran-4-olatobis(dimethyl sulfoxidenickel(II
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Amel Djedouani
2009-10-01
Full Text Available In the title compound, [Ni(C8H7O42{(CH32SO}2], the NiII atom is located on a crystallographic centre of symmetry and has a distorted octahedral coordination geometry of type MO6. The bidentate dehydroacetic acid (DHA ligands occupy the equatorial plane of the complex in a trans configuration, and the dimethyl sulfoxide (DMSO ligands are weakly coordinated through their O atoms in the axial positions.
{2-[(4-Nitrobenzylideneamino]-4,5,6,7-tetrahydro-1-benzothiophen-3-yl}(phenylmethanone
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Manpreet Kaur
2014-06-01
Full Text Available In the title compound, C22H18N2O3S, disorder is found in the benzoyl group (A and B, as well as for four C atoms of the cyclohexene ring. Two orientations were modeled in a 0.583 (5:0.417 (5 ratio. The cyclohexene ring is in a distorted chair conformation. The dihedral angles between the mean plane of the thiophene ring and the 4-nitrobenzene and phenyl rings are 30.9 (8 and 64.8 (3 (A and 62.4 (7° (B. The mean planes of the 4-nitrobenzene and the phenyl rings are almost perpendicular to each other, with dihedral angles of 85.4 (1 (A and 83.9 (8° (B. An extensive array of weak C—H...O interactions consolidate molecules into a three-dimensional architecture, forming chains along [001] and [010] and layers parallel to (011.
Synthesis and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).
Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B
2016-08-01
Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms.
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Krystal R. Fontenot
2013-09-01
Full Text Available The title compound, C26H22N5O4P3·C3H6O, has been achieved in a two-step synthesis that does not require chromatography. This molecule contains a seven-membered spirocyclic ring at two P-atom positions and a five-membered ring containing new P—N bonds at the other P-atom position. Endocyclic torsion angles about the central biphenyl C—C bonds are −41.5 (3 and −44.4 (3°, and P—N bonds of the central P3N3 ring are within the range 1.5665 (17–1.6171 (17 Å, while the P—O distances are in the range 1.5940 (14–1.6041 (14 Å. One N—H group makes an intermolecular N—H...N hydrogen bond, forming centrosymmetric dimers, while the other N—H group makes an N—H...O hydrogen bond to the acetone solvent molecule. The crystal was a two-component non-merohedral twin with ratio 0.811/0.189.
2-Ethoxy-4-[2-(3-nitrophenylhydrazonomethyl]phenol
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Jun-Qiang Chen
2009-10-01
Full Text Available The title Schiff base compound, C15H15N3O4, was prepared from a condensation reaction of 3-ethoxy-4-hydroxybenzaldehyde and 3-nitrophenylhydrazine. The molecule is nearly planar; the dihedral angle between the hydroxybenzene ring and the nitrobenzene ring is 6.57 (7°. O—H...O, O—H...N and C—H...O hydrogen bonding helps to stabilize the crystal structure.
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Hai Le Thi Hong
2015-09-01
Full Text Available The asymmetric unit of the title compound, [Ni(H2O6](C11H8NO8S2·2H2O, features a half-hexaaquanickel(II complex cation with the NiII ion on an inversion center, one deprotonated 5,6-dihydroxy-3-sulfoquinolin-7-yloxyacetic acid (QOH molecule appearing in its zwitterionic form and one lattice water molecule. The sulfonate group is disordered over two positions with occupancy factors of 0.655 (5 and 0.345 (5. The hexaaquanickel(II cation interacts through hydrogen bonding with eight QOH molecules and two water molecules. The six-membered rings of quinoline show π–π stacking [centroid-to-centroid distances of 3.679 (2 Å and 3.714 (2 Å].
H-D exchange in metal carbene complexes: Structure of cluster (μ-H)(μ-OCD3)Os3(CO)9{:C(CD3)NC2H8O}
Savkov, Boris; Maksakov, Vladimir; Kuratieva, Natalia
2015-10-01
X-ray and spectroscopic data for the new complex (μ-H)(μ-OCH3)Os3(CO)9{:C(CD3)NC2H8O} (2) obtained in the reaction of the (μ-H)(μ-Cl)Os3(CO)9{:C(CH3)NC2H8O} (1) with NaOCD3 in CD3OD solution are reported. It is shown that cluster 1 has the property of CH-acidity inherent of Fisher type carbenes. This had demonstrated using hydrogen deuterium exchange reaction in the presence of a strong base. Bridging chlorine to metoxide ligand substitution takes place during the reaction. The molecular structure of 2 is compared with known analogues.
Takahashi, S; Kakinuma, N; Iwai, H; Yanagisawa, T; Nagai, K; Suzuki, K; Tokunaga, T; Nakagawa, A
2000-11-01
Three novel quinolone compounds, quinolactacins A (1), B (2) and C (3), have been found from the fermentation broth of Penicillium sp. EPF-6, a fungus isolated from the larvae of mulberry pyralid (Margaronia pyloalis Welker). The molecular formulas of 1, 2 and 3 were determined to be C16H18N2O2, C15H16N2O2 and C16H18N2O3, respectively by FAB-MS and NMR spectral analyses. The structures of these compounds have a novel quinolone skeleton with a gamma-lactam ring consisting of C12H8N2O2 as the common chromophore.
Energy Technology Data Exchange (ETDEWEB)
Borel, A.G.; Abbott, F.S. (British Columbia Univ., Vancouver, BC (Canada). Dept. of Pharmaceutical Sciences)
1990-07-01
Pentadeuteriophenyl clobazam was synthesized in essentially quantitative isotopic purity, and characterized by {sup 1}H-NMR and mass spectroscopy. The title compound was found to be >98% pure by HPLC, and its retention time (t{sub R} 6.17 min) was less than that of an authentic clobazam standard (t{sub R} 6.32 min). Of the five steps in the synthesis of clobazam, the most susceptible to deuterium exchange was the nucleophilic substitution of 2,4-dichloronitrobenzene by aniline-d{sub 7} to form N-(5-chloro-2-nitrophenyl)penta-deuteriophenylamine. In this step, the isotopic impurity aniline-2,3,4,5-d{sub 5} introduced protons from nitrogen into the ortho and para positions of the deuteriophenyl ring of N-(5-chloro-2-nitrophenyl)pentadeuteriophenylamine. (author).
2,2′-Bis{8-[(benzylaminomethylidene]-1,6-dihydroxy-5-isopropyl-3-methylnaphthalen-7(8H-one}
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Shukhrat M. Hakberdiev
2013-11-01
Full Text Available The asymmetric unit of the title compound, C44H44N2O6, contains two independent molecules with similar conformations. The dihydronaphthalene ring systems are approximately planar [maximum deviations = 0.036 (2, 0.128 (2, 0.0.24 (2 and 0.075 (2 Å]. The dihedral angle between two dihydronaphthalene ring systems is 83.37 (4° in one molecule and 88.99 (4° in the other. The carbonyl O atom is linked with the adjacent hydroxy and imino groups via intramolecular O—H...O and N—H...O hydrogen bonds. In the crystal, molecules are linked through O—H...O hydrogen bonds into layers parallel to (001, and adjacent layers are further stacked by π–π interactions between dihydronaphthalene and phenyl rings into a three-dimensional supramolecular architecture. In the crystal, one of the isopropyl groups is disordered over two positions with an occupancy ratio of 0.684 (8:0.316 (8.
Thermal decomposition of heavy rare-earth butanoates, Ln(C3H7CO2)3 (Ln = Er, Tm, Yb and Lu) in argon
DEFF Research Database (Denmark)
Grivel, Jean-Claude; Yue, Zhao; Tang, Xiao
2016-01-01
was observed in all four compounds, but its course depends on the rare-earth element. Decomposition to sesquioxides proceeds via the formation of dioxymonocarbonates (Ln2O2CO3) and release of 4-heptanone (C3H7COC3H7) as well as carbon dioxide (CO2) without evidence for an intermediate oxobutanoate stage...... of Ln2O2CO3 and Ln2O3. The stability of this intermediate state seems to decrease with the mass of the rare-earth elements. Complete conversion to Ln2O3 is reached at about 1100 °C. The overall thermal decomposition behaviour of the title compounds is different from previous reports for other rare....... During the decomposition of Ln2O2CO3 into the respective sesquioxides (Ln2O3), an intermediate plateau extending from approximately 550 to 850 °C appears in the TG traces. The overall composition during this stage corresponds approximately to Ln2O2.8(CO3)0.2, but the state is more probably a mixture...
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Richard Betz
2011-10-01
Full Text Available The title compound, C30H28N6O2, is a symmetric diimine derived from ortho-dibenzaldehyde. Both C=N bonds are (E-configured. The terminal N-bonded phenyl groups adopt staggered conformations relative to their respective parent heterocycles, the relevant least-squares planes intersect at angles of 32.35 (11 and 38.59 (10°. In the crystal, C—H...O contacts connect the molecules into chains along the b axis and give rise to a C11(14C11(14 and a R22(12 pattern on different levels of graph-set analysis. The shortest intercentroid distance between two centroids was found at 4.2074 (11 Å between the two five-membered heterocycles.
tert-Butyl 6-bromo-1,4-dimethyl-9H-carbazole-9-carboxylate
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Jean-François Lohier
2010-08-01
Full Text Available The title compound, C19H20BrNO2, consists of a carbazole skeleton with methyl groups at positions 1 and 4, a protecting group located at the N atom and a Br atom at position 6. The pyrrole ring is oriented at dihedral angles of 1.27 (7 and 4.86 (7° with respect to the adjacent benzene rings. The dihedral angle between the benzene rings is 5.11 (7. The crystal structure is determined mainly by intramolecular C—H...O and intermolecular π–π interactions. π-stacking between adjacent molecules forms columns with a parallel arrangement of the carbazole ring systems. The presence of the tert-butoxycarbonyl group on the carbazole N atom and the intramolecular hydrogen bond induce a particular conformation of the exocyclic N—C bond within the molecule.
Halogen effect on structure and 13C NMR chemical shift of 3,6-disubstituted-N-alkyl carbazoles
DEFF Research Database (Denmark)
Radula-Janik, Klaudia; Kupka, Teobald; Ejsmont, Krzysztof
2013-01-01
Structures of selected 3,6-dihalogeno-N-alkyl carbazole derivatives were calculated at the B3LYP/6-311++G(3df,2pd) level of theory and their 13C NMR isotropic nuclear shieldings were predicted using density functional theory (DFT). The model compounds contained 9H-, N-methyl and N-ethyl derivatives...
N-(5-Benzylsulfanyl-1,3,4-thiadiazol-2-yl-2-(piperidin-1-ylacetamide
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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.
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Juan Kong
2008-01-01
Full Text Available The title complex, [Ni2(C42H46Cl2N6O2(C2H3O2]ClO4·2CH3CN, was synthesized by condensation of 2,6-diformyl-4-chlorophenol with N,N-bis(aminopropylbenzylamine in the presence of NiII ions. The ligand is a 28-membered macrocycle with two identical pendant arms. The coordination geometries of the Ni atoms are both octahedral. The two Ni atoms are bridged by two phenolate O atoms of the macrocyclic ligand and one acetate ligand, with an Ni...Ni distance of 3.147 (4 Å.
4-[(3-Phenyl-4,5-dihydroisoxazol-5-ylmethyl]-2H-benzo[b][1,4]thiazin-3(4H-one
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Nada Kheira Sebbar
2016-06-01
Full Text Available In the title compound, C18H16N2O2S, the 5-dihydroisoxazol-5-yl ring and its phenyl substituent are nearly coplanar, with the largest deviation from the mean plane being 0.0184 (16 Å. The thiomorpholin-3-one ring adopts a screw-boat conformation and the attached benzene ring makes a dihedral angle of 42.26 (7° with the mean plane through the 3-phenyl-4,5-dihydroisoxazol-5-yl ring system. In the crystal, molecules are linked by pairs of C—H...N hydrogen bonds, forming inversion dimers. These dimers are linked via C—H...O hydrogen bonds, generating a three-dimensional network.
Triaquabis(1H-imidazolebis[μ2-2-(oxaloaminobenzoato(3−]dicopper(IIcalcium(II heptahydrate
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Peng Zhang
2008-02-01
Full Text Available In the title heterotrinuclear coordination compound, [CaCu2(C9H4NO52(C3H4N22(H2O3]·7H2O, the Ca2+ cation is in a pentagonal–bipyramidal geometry and bridges two (1H-imidazole[2-(oxaloaminobenzoato(3−]copper(II units in its equatorial plane. Each CuII atom has a normal square-planar geometry. The molecule has approximate local (non-crystallographic mirror symmetry and 23 classical hydrogen bonds are found in the crystal structure.
Berkei, Michael; Bickley, Jamie F; Heaton, Brian T; Steiner, Alexander
2002-09-21
The reaction of M[PtX3(CO)] (M+ = [(C4H9)4N]+, X = Br, Cl) with an excess of Br2 gives the new platinum(IV) salts, [(C4H9)4N]2[Pt2Br10].(Br2)7, 1, and [(C4H9)4N]2[PtBr4Cl2].(Br2)6, 2, which, in the solid state, contain strong Br Br interactions resulting in the formation of polymeric networks; they could provide useful solid storage reservoirs for elemental bromine.
Sangeetha, V; Kanagathara, N; Chakkaravarthi, G; Marchewka, M K; Anbalagan, G
2013-05-01
The asymmetric unit of the title salt, C3H7N6 (+)·C6H7O4 (-)·C3H4O2·H2O, contains a 2,4,6-tri-amino-1,3,5-triazin-1-ium cation, a 3-(prop-2-eno-yloxy)propano-ate anion and acrylic acid and water solvent mol-ecules in a 1:1:1:1 ratio and with each species in a general position. In the crystal, the components are linked into a supra-molecular layer in the bc plane via a combination of O-H⋯O, N-H⋯N and N-H⋯O hydrogen bonding. The crystal studied was a non-merohedral twin, the minor component contribution being approximately 26%.
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.
(2,3,7,8,12,13,17,18-Octaethylporphyrinato-κ4Ncobalt(II–2-nitrobenzaldehyde (1/2
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Anissa Mansour
2012-09-01
Full Text Available The asymmetric unit of the title compound, [Co(C36H44N4]·2C7H5NO3, is composed of one half of the complex, arranged about an inversion center, and a complete 2-nitrobenzaldehyde (NBA molecule. The structure consists of columns that contain interleaved molecules of NBA and [CoII(OEP] (OEP is 2,3,7,8,12,13,17,18-octaethylporphyrin, which are stacked along the a axis. The CoII atom is involved in a π interaction with the ring of the NBA molecule with a centroid–metal distance of 3.508 (6 Å. There is an intramolecular C—H...O hydrogen bond in the NBA molecule.
Malinkin, Sergey; Penkova, Larisa; Pavlenko, Vadim A.; Haukka, Matti; Fritsky, Igor O.
2009-01-01
The title compound, [Cu2(C7H6N2O3)Cl2(C5H5N)4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octahedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H⋯O hydrogen bond connects the complex molecules and propan-2-ol solvent molecules into pairs. These pairs form columns along the a axis. PMID:21577764
Davaasuren, Bambar
2015-02-25
In the title compound, [FeIr(C5H5)(C20H14N3)Cl3]·2CH3CN, the central IrIII atom is sixfold coordinated by three chloride ligands and three terpyridine N atoms in a slightly distorted octahedral fashion. The terpyridine ligand is functionalized at the 4\\'-position with a ferrocenyl group, the latter being in an eclipsed conformation. In the crystal, molecules are stacked in rows parallel to [001], with the acetonitrile solvent molecules situated between the rows. An extensive network of intra- and intermolecular C-H...Cl interactions is present, stabilizing the three-dimensional structure.
(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
N-(4-Chlorophenyl-2-(hydroxyiminoacetamide
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Jie Sun
2009-09-01
Full Text Available The title compound, C8H7ClN2O2, is an intermediate in the synthesis of 5-chloroisatin, which can be further transformed to 5-chloro-2-indolinone via a Wolff–Kishne reduction. The C2N acetamide plane forms a dihedral angle of 6.3 (3° with the benzene ring. An intramolecular C—H...O interaction results in the formation of a six-membered ring. In the crystal, intermolecular N—H...O, N—H...N and O—H...O hydrogen bonds link the molecules into multimers, forming sheets.
2-[N-(3-Amino-4-nitrophenylcarboximidoyl]phenol
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Gholam Hossein Shahverdizadeh
2011-11-01
Full Text Available The title compound, C13H11N3O3, is essentially planar (r.m.s. for the 19 non-H atoms = 0.031 Å, a conformation stabilized in part by intramolecular O—H...N and N—H...O hydrogen bonds. The configuration about the imine bond [1.2919 (12 Å] is E. The presence of N—H...O(nitro hydrogen bonds leads to the formation of supramolecular tapes in the crystal structure. These are connected into layers by π–π interactions [centroid–centroid distance = 3.6046 (6 Å] occurring between the hydroxy- and amino-substituted benzene rings.
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Mingyan Yang
2015-11-01
Full Text Available In order to find new lead compounds with high fungicidal activity, (Z/E-3,7-dimethyl-2,6-octadienoic acids were synthesized via selective two-step oxidation using the commercially available geraniol/nerol as raw materials. Twenty-eight different (Z/E-3,7-dimethyl-2,6-octadienamide derivatives were prepared by reactions of (Z/E-carboxylic acid with various aromatic and aliphatic amines, followed by oxidation of peroxyacetic acid to afford their 6,7-epoxy analogues. All of the compounds were characterized by HR-ESI-MS and 1H-NMR spectral data. The preliminary bioassays showed that some of these compounds exhibited good fungicidal activities against Rhizoctonia solani (R. solani at a concentration of 50 µg/mL. For example, 5C, 5I and 6b had 94.0%, 93.4% and 91.5% inhibition rates against R. solani, respectively. Compound 5f displayed EC50 values of 4.3 and 9.7 µM against Fusahum graminearum and R. Solani, respectively.
N,N-Diethylanilinium 2,4-dioxo-5-(2,4,6-trinitrophenyl-1,2,3,4-tetrahydropyrimidin-6-olate
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Manickam Buvaneswari
2011-12-01
Full Text Available In the crystal structure of the title molecular salt, C10H16N+·C10H4N5O9−, the components are linked through a N—H...O hydrogen bonds. R22(8 ring motifs are formed between inversion-related barbiturate residues. Two intramoleculer N—H...O hydrogen bonds are observed in the anion. The dihedral angle between 2,4,6-trinitrophenyl and barbiturate rings is 53.6 (2°. The N,N-diethylamine substituent is disordered and was modeled as two geometrically equivalent conformers with occupancies of 0.737 (2 and 0.273 (2.
1,6-Bis[(2,2′:6′,2′′-terpyridin-4′-yloxy]hexane
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Varvara I. Nikolayenko
2012-07-01
Full Text Available The molecule of the title compound, C36H32N6O2, lies about an inversion center, located at the mid-point of the central C—C bond of the diether bridge. The terminal pyridine rings form dihedral angles of 4.67 (7 and 26.23 (7° with the central ring. In the crystal, weak C—H...N and C—H...O interactions link the molecules into a three-dimensional network.
N-[3-(Benzenesulfonamidopropyl]benzenesulfonamide
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Tahir Ali Sheikh
2011-07-01
Full Text Available In the title compound, C15H18N2O4S2, the dihedral angle between the aromatic rings is 71.8 (2°. The conformation of the central N—C—C—C—N fragment is gauche–gauche [torsion angles = 72.5 (5 and 65.7 (5°]. Both N atoms adopt pyramidal geometries. In the crystal, molecules are linked by N—H...O hydrogen bonds, generating (001 sheets, and weak C—H...O interactions consolidate the packing.
3-[2-(5H-Indolo[2,3-b]quinoxalin-5-ylethyl]-1,3-oxazolidin-2-one
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Abdussalam Alsubari
2010-09-01
Full Text Available The title compound, C19H16N4O2, has an almost planar fused N-heterocyclic system (r.m.s. deviation = 0.031 Å and an almost planar five-membered 1,3-oxazolidine ring (r.m.s. deviation = 0.015 Å at the ends of an ethylene chain [N—C—C—N torsion angle = −65.6 (2°]. The ring systems are inclined at 38.1 (1° to one another.
International Nuclear Information System (INIS)
Buragohain, Amlan; Couck, Sarah; Van Der Voort, Pascal; Denayer, Joeri F.M.; Biswas, Shyam
2016-01-01
Four existing and three new functionalized chromium terephthalates having MIL-101 topology and denoted as Cr-MIL-101-X (existing ones with X=–F, 1-F; –Cl, 2-Cl; –Br, 3-Br; –CH 3 , 4-CH 3 ; new ones with X=–C 6 H 4 , 5-C 6 H 4 ; –F 2 , 6-F 2 , –(CH 3 ) 2 , 7-(CH 3 ) 2 ) were synthesized under hydrothermal conditions. All the materials except 5-C 6 H 4 could be prepared by a general synthetic route, in which the mixtures of CrO 3 , H 2 BDC-X (BDC=1,4-benzenedicarboxylate) linkers, conc. HCl and water with a molar ratio of 1:1:3.9:222.2 were reacted at 180 °C for 144 h. Compared to the 144 h of synthesis time, three of the compounds, namely 1-Cl, 2-Br and 5-C 6 H 4 , could be prepared in much shorter reaction times (12–18 h at 180–210 °C). The materials possess high thermal stability up to 270–300 °C in an air atmosphere. The activated compounds exhibit significant porosity (S BET range: 1273–2135 m 2 g −1 ). At 0 °C and 1 bar, the CO 2 adsorption capacities of the compounds fall in the 1.7–2.9 mmol g −1 range. Compounds 1-F and 6-F 2 showed enhanced CO 2 uptake values compared to parent Cr-MIL-101. The benzene adsorption capacities of the compounds lie in the range of 66.2–139.5 molecules per unit cell at 50 °C and p/p 0 =0.35. The increased benzene uptake value of 1-F compared to un-functionalized Cr-MIL-101 and 4-CH 3 suggests that the fluorination has induced more hydrophobicity in Cr-MIL-101 as compared to the methylation. - Graphical abstract: Benzene adsorption by seven functionalized Cr-MIL-101-X metal-organic framework (MOF) materials Display Omitted - Highlights: • Seven functionalized Cr-MIL-101-X materials were synthesized solvothermally. • All Cr-MIL-101-X materials exhibited high thermal stability up to 270–300 °C in air. • All Cr-MIL-101-X compounds displayed considerable porosity towards N 2 , CO 2 and benzene. • Mono- and di-fluorinated Cr-MIL-101 materials showed enhanced CO 2 adsorption capacities.
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
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Raju Suresh Kumar
2010-08-01
Full Text Available In the title compound, C37H32N2O3, an intramolecular O—H...N hydrogen bond generates a five-membered ring, producing an S(5 motif. The piperidone ring adopts a half-chair conformation. The two fused pyrrolidine rings have similar envelope conformations. The interplanar angles between the benzene rings A/B and C/D are 75.68 (7 and 30.22 (6°, respectively. In the crystal structure, adjacent molecules are interconnected into chains propagating along the [010] direction via intermolecular C—H...O hydrogen bonds. Further stabilization is provided by weak C—H...π interactions.
3-(1H-Indol-3-yl-2-(2-nitrobenzenesulfonamidopropanoic acid including an unknown solvate
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Islam Ullah Khan
2012-07-01
Full Text Available In the title compound, C17H15N3O6S, which crystallized with highly disordered methanol and/or water solvent molecules, the dihedral angle between the the indole and benzene ring systems is 5.3 (2°, which allows for the formation of intramolecular π–π stacking interactions [centroid–centroid separations = 3.641 (3 and 3.694 (3 Å] and an approximate overall U-shape for the molecule. In the crystal, dimers linked by pairs of Ns—H...Oc (s = sulfonamide and c = carboxylate hydrogen bonds generate R22(10 loops, whereas Ni—H...π (i = indole interactions lead to chains propagating in [100] or [010]. Together, these lead to a three-dimensional network in which the solvent voids are present as intersecting (two-dimensional systems of [100] and [010] channels. The title compound was found to contain a heavily disordered solvent molecule, which could be methanol or water or a mixture of the two. Due to its uncertain nature and the unresolvable disorder, the data were processed with the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155], which revealed 877.8 Å3 of solvent-accessible volume per unit cell and 126 electron-units of scattering density or 109.7 Å3 (16 electron units per organic molecule.. This was not included in the calculations of overall formula weight, density and absorption coefficient.
2-Oxo-2H-chromen-7-yl 4-tert-butylbenzoate
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Mohammad Ouédraogo
2018-04-01
Full Text Available In the title compound, C20H18O4, the benzoate ring is oriented at an acute angle of 33.10 (12° with respect to the planar (r.m.s deviation = 0.016 Å coumarin ring system. An intramolecular C—H...O hydrogen bond closes an S(6 ring motif. In the crystal, C—H...O contacts generate infinite C(6 chains along the b-axis direction. Also present are π–π stacking interactions between neighbouring pyrone and benzene rings [centroid–centroid distance = 3.7034 (18 Å] and C=O...π interactions [O...centroid = 3.760 (3 Å]. The data obtained from quantum chemical calculations performed on the title compound are in good agreement with the observed structure, although the calculated C—O—C—C torsion angle between the coumarin ring system and the benzoate ring (129.1° is somewhat lower than the observed value [141.3 (3°]. Hirshfeld surface analysis has been used to confirm and quantify the supramolecular interactions.
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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.
Duchateau, R; Meetsma, A; Teuben, JH
1996-01-01
AlCl3 reacts with [PhC(NSiMe(3))(2)]Li(OEt(2)) to afford the bis(N,N'-bis(trimethylsilyl)benzamidinato)aluminium chloro compound which, on treatment with KBEt(3)H, yields the structurally characterized monomeric hydride derivative, [PhC(NSiMe(3))(2)]2AlH, whose reactivity towards unsaturated
Bis(2-amino-1,3-benzothiazole-κN3dichloridozinc(II ethanol hemisolvate
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Young-Inn Kim
2012-02-01
Full Text Available In the title compound, [ZnCl2(C7H6N2S2]·0.5CH3CH2OH, the ZnII atom is coordinated by two N atoms of two 2-aminobenzothiazole ligands and two Cl atoms within a distorted tetrahedral geometry. The dihedral angle between the N/Zn/N and Cl/Zn/Cl planes is 86.22 (7°. The benzothiazole molecules are almost perpendicular to each other, forming a dihedral angle of 80.20 (8°. The molecular structure is stabilized by intramolecular N—H...Cl hydrogen bonds. In the crystal, intermolecular N—H...Cl hydrogen bonds link the molecules into a three-dimensional network. The SQUEEZE procedure in PLATON [Spek (2009. Acta Cryst. D65, 148–155] was used to model a disordered ethanol solvent molecule; the calculated unit-cell data allow for the presence of half of this molecule in the asymmetric unit.
Shibuya, K; Takeoka, Y; Asai, K
2002-01-01
We report a new type of scintillator especially suitable for pulse-radiation detection. Thin films of organic/inorganic perovskite compound (n-C sub 6 H sub 1 sub 3 NH sub 3) sub 2 PbI sub 4 , which is characterized by a multiple quantum well structure, were bombarded by 2.0 MeV protons, and their radiation-induced emission spectra were obtained. A single and sharp emission peak due to an exciton was observed at the wavelength of 524 nm. This emission was clearly detected even at room temperature, and its quantum efficiency was very high. The line shape of this emission did not change, retaining its sharpness, and no other emissions appeared throughout the irradiation. The optical response of (n-C sub 6 H sub 1 sub 3 NH sub 3) sub 2 PbI sub 4 is very fast. (n-C sub 6 H sub 1 sub 3 NH sub 3) sub 2 PbI sub 4 is a promising scintillator material, meeting requirements not satisfied by conventional scintillators.
Ethyl 2-amino-4-(4-bromophenyl-6-methoxy-4H-benzo[h]chromene-3-carboxylate
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Seik Weng Ng
2013-03-01
Full Text Available In the title compound, C23H20BrNO4, the pyran ring has a flattened boat conformation with the O and methine C atoms lying to one side of the plane [0.160 (5 and 0.256 (6 Å, respectively] defined by the remaining atoms. Nevertheless, the 4H-benzo[h]chromene ring system approximates a plane (r.m.s. deviation = 0.116 Å with the bromobenzene ring almost perpendicular [dihedral angle = 83.27 (16°] and the ester group coplanar [C—C—C—O = 3.4 (5°]; the methoxy substituent is also coplanar [C—O—C—C = 174.5 (3°]. In addition to an intramolecular N—H...O(ester carbonyl hydrogen bond, the ester carbonyl O atom also forms an intermolecular N—H...O hydrogen bond with the second amine H atom, generating a zigzag supramolecular chain along the c axis in the crystal packing. The chains are linked into layers in the bc plane by N—H...Br hydrogen bonds, and these layers are consolidated into a three-dimensional architecture by C—H...π interactions.
NMR study of distinct phase transitional behaviors in (CnH2n+1NH3)2SnCl6
International Nuclear Information System (INIS)
Lee, K. W.; Lee, C. E.; Choi, J. Y.; Kim, J.
2005-01-01
Phase transitions in bis-(n-C n H 2n+1 NH 3 ) 2 SnCl 6 , where the hydrocarbon part is analogous to lipid membrane, were investigated by means of 200-MHz 1 H nuclear magnetic resonance. As a result, critical fluctuations and molecular dynamics associated with the phase transitions, an order-disorder and a conformational phase transition, were distinguished in a wide temperature range. The critical dynamics, observed in the long-chain compounds but not in the short-chain compounds by laboratory frame spin-lattice relaxation measurements, is discussed in view of the chain length dependence of molecular dynamics.
Cluster-enhanced X-O-2 photochemistry (X=CH3I, C3H6, C6H12, and Xe)
Baklanov, A.V.; Bogdanchikov, G.A.; Vidma, K.V.; Chestakov, D.A.; Parker, D.H.
2007-01-01
The effect of a local environment on the photodissociation of molecular oxygen is investigated in the van der Waals complex X-O-2 (X=CH3I, C3H6, C6H12, and Xe). A single laser operating at wavelengths around 226 nm is used for both photodissociation of the van der Waals complex and simultaneous
2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate
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YuanQi Yu
2011-10-01
Full Text Available The asymmetric unit of the title compound, C8H9N2+·C8H5O4−, contains two independent ion pairs. In each 2-methyl-1H-benzimidazolium ion, an intramolecular O—H...O bond forms an S(7 graph-set motif. In the crystal, the components are linked by N—H...O hydrogen bonds, forming chains along [210]. Further stabilization is provided by weak C—H...O hydrogen bonds.
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Thomas Lanyon-Hogg
2016-06-01
Full Text Available In this data article we describe synthetic and characterisation data for four members of the 5-acyl-6,7-dihydrothieno[3,2-c]pyridine (termed “RU-SKI” class of inhibitors of Hedgehog acyltransferase, including associated NMR spectra for final compounds. RU-SKI compounds were selected for synthesis based on their published high potencies against the enzyme target. RU-SKI 41 (9a, RU-SKI 43 (9b, RU-SKI 101 (9c, and RU-SKI 201 (9d were profiled for activity in the related article “Click chemistry armed enzyme linked immunosorbent assay to measure palmitoylation by Hedgehog acyltransferase” (Lanyon-Hogg et al., 2015 [1]. 1H NMR spectral data indicate different amide conformational ratios between the RU-SKI inhibitors, as has been observed in other 5-acyl-6,7-dihydrothieno[3,2-c]pyridines. The synthetic and characterisation data supplied in the current article provide validated access to the class of RU-SKI inhibitors.
Energy Technology Data Exchange (ETDEWEB)
Gichumbi, Joel M.; Omondi, Bernard; Friedrich, Holger B. [School of Chemistry, University of KwaZulu-Natal, Durban (South Africa); Lazarus, Geraldine; Singh, Moganavelli; Shaikh, Nazia; Chenia, Hafizah Y. [School of Life Sciences, University of KwaZulu-Natal, Durban (South Africa)
2017-06-01
New complexes [(η{sup 6}-p-cymene)Ru(C{sub 5}H{sub 4}N-2-CH=N-Ar)X]PF{sub 6} [X = Br (1), I (2); Ar = 4-fluorophenyl (a), 4-chlorophenyl (b), 4-bromophenyl (c), 4-iodophenyl (d), 2,5-dichlorophenyl (e)] were prepared, as well as 3a-3e (X = Cl) and the new complexes [(η{sup 6}-arene)RuCl(N-N)]PF{sub 6} [arene = C{sub 6}H{sub 5}OCH{sub 2}CH{sub 2}OH, N-N = 2,2{sup '}-bipyridine (4), 2,6-(dimethylphenyl)-pyridin-2-yl-methylene amine (5), 2,6-(diisopropylphenyl)-pyridin-2-yl-methylene amine (6); arene = p-cymene, N-N = 4-(aminophenyl)-pyridin-2-yl-methylene amine (7)]. X-ray diffraction studies were performed for 1a, 1b, 1c, 1d, 2b, 5, and 7. Cytotoxicities of 1a-1d and 2 were established versus human cancer cells epithelial colorectal adenocarcinoma (Caco-2) (IC{sub 50}: 35.8-631.0 μM), breast adenocarcinoma (MCF7) (IC{sub 50}: 36.3-128.8.0 μM), and hepatocellular carcinoma (HepG2) (IC{sub 50}: 60.6-439.8 μM), 3a-3e were tested against HepG2 and Caco-2, and 4-7 were tested against Caco-2. 1-7 were tested against non-cancerous human epithelial kidney cells. 1 and 2 were more selective towards tumor cells than the anticancer drug 5-fluorouracil (5-FU), but 3a-3e (X = Cl) were not selective. 1 and 2 had good activity against MCF7, some with lower IC{sub 50} than 5-FU. Complexes with X = Br or I had moderate activity against Caco-2 and HepG2, but those with Cl were inactive. Antibacterial activities of 1a, 2b, 3a, and 7 were tested against antibacterial susceptible and resistant Gram-negative and -positive bacteria. 1a, 2b, and 3a showed activity against methicillin-resistant S. aureus (MIC = 31-2000 μg.mL{sup -1}). (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)
International Nuclear Information System (INIS)
Ahmed, M.N.; Yasin, K.A.; Khan, R.A.H.; Mahmood, T.; Ayub, K.; Malik, D.
2017-01-01
Ethyl-6-(4-(ethoxycarbonyl)-1H-1,2,3-triazol-1-yl)pyridine-3-carboxylate (1), was synthesized via click reaction between ethyl tetrazolo[1,5-a]pyridine-6-carboxylate and ethyl propiolate in tetrahydrofuran (THF) in the presence of catalytic amount of a copper acetate. The structure was confirmed by single-crystal X-ray diffraction, NMR, FT-IR and MS. The compound crystallizes in the triclinic system, space group P-1 with a = 4.9122 (5), b = s9.5891 (11), c = 15.4851 (18) Å, a = 92.371 (5), beta = 90.015 (4), gamma = 101.722 (5) Z = 2 and V (Å /sup 3/) = 713.55 (14). Packing diagram indicates that there is dimeric interaction between two units via N(2)H(7). The crystal structure of the title compound 1 is stabilized by several nonboding interactions. Space filling model also revealed C-H...π and the π-π interactions in the molecule. Theoretical investigations were executed by using the Gaussian 09 software to enable comparison with X-ray structure as well as spectroscopic results, and to further probe the structural properties. The molecular electrostatic potential (MEP) analysis gave the idea about chemical reactivity and the Mulliken charge analysis gave quantitative estimate of the charges on the atoms. Frontier molecular orbitals analysis (electronic properties) was used to find the energy gap between the HOMO and the LUMO. The target compound was screened against three different bacterial strains like S. typhimurium, M. luteus and B. bronchiseptica as well as three different fungal strains i.e Aspergilus niger, Mucor specie and Aspergilus flavus. Moderate activities have been displayed by the target compound against tested strains. (author)
5-(4-Fluorophenyl-2,2,6-trimethyl-4H-1,3-dioxin-4-one
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Julio Zukerman-Schpector
2009-07-01
Full Text Available The 1,3-dioxine ring in the title compound, C13H13FO3, is in a half-boat conformation with the methyl-bonded C atom 0.612 (2 Å out of the plane defined by the remaining five atoms.
N-(2,6-Dichlorophenyl-4-methylbenzamide
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Vinola Z. Rodrigues
2011-08-01
Full Text Available In the title compound, C14H11Cl2NO, the two aromatic rings are nearly orthogonal to each other [dihedral angle 79.7 (1°], while the central amide core –NH—C(=O– is nearly coplanar with the benzoyl ring [N—C—C—C torsion angles = −5.5 (3 and 1772. (2°]. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into C(4 chains propagating in [001].
cis-Aquadichlorido[pyrimidin-2(1H-one-κN3]copper(II
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A. Guy Orpen
2008-07-01
Full Text Available In the title compound, [CuCl2(C4H4N2O(H2O], the CuII cation is coordinated by two chloride anions, one pyrimidin-2-one N atom and one water molecule, giving a slightly distorted square-planar geometry. In the crystal structure, the pyrimidin-2-one rings stack along the b axis, with an interplanar distance of 3.306 Å, as do the copper coordination planes (interplanar spacing = 2.998 Å. The coordination around the Jahn–Teller-distorted CuII ion is completed by long Cu...O [3.014 (5 Å] and Cu...Cl [3.0194 (15 Å] interactions with adjacent molecules involved in this stacking. Several N—H...Cl, O—H...Cl and O—H...O intermolecular hydrogen bonds form a polar three-dimensional network.
N-(1-Acryloyl-2,2,6,6-tetramethylpiperidin-4-ylacrylamide
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Shailesh K. Goswami
2011-11-01
Full Text Available The title compound, C15H24N2O2, crystallizes with two unique molecules, (I and (II, in the asymmetric unit, differing in the orientation of the acryloyl units with respect to the piperidine rings. The acrylamide units are essentially planar in both molecules (r.m.s. deviations = 0.042 and 0.024 Å, respectively, as are the C3N chains of the acryloyl units. The carbonyl O atoms of the acryloyl systems lie significantly out of these planes, viz. by −0.171 (9 Å for molecule (I and by 0.33 (1 Å for molecule (II. The acrylamide and acryloyl planes are inclined at 68.7 (4° and 59.8 (3° in the two molecules. The piperidine rings each adopt twist boat conformations. In the crystal, strong N—H...O hydrogen bonds link the molecules into zigzag C(4 chains along b. Additional C—H...O contacts result in the formation of stacks along a.
Jiménez-Pulido, Sonia B; Hueso-Ureña, Francisco; Fernández-Liencres, M Paz; Fernández-Gómez, Manuel; Moreno-Carretero, Miguel N
2013-01-14
The oxime derived from 6-acetyl-1,3,7-trimethyllumazine (1) ((E-6-(hydroxyimino)ethyl)-1,3,7-trimethylpteridine-2,4(1H,3H)-dione, DLMAceMox) has been prepared and its molecular and crystal structure determined from spectral and XRD data. The oxime ligand was reacted with silver nitrate, perchlorate, thiocyanate, trifluoromethylsulfonate and tetrafluoroborate to give complexes with formulas [Ag(2)(DLMAceMox)(2)(NO(3))(2)](n) (2), [Ag(2)(DLMAceMox)(2)(ClO(4))(2)](n) (3), [Ag(2)(DLMAceMox)(2)(SCN)(2)] (4), [Ag(2)(DLMAceMox)(2)(CF(3)SO(3))(2)(CH(3)CH(2)OH)]·CH(3)CH(2)OH (5) and [Ag(DLMAceMox)(2)]BF(4) (6). Single-crystal XRD studies show that the asymmetrical residual unit of complexes 2, 3 and 5 contains two quite different but connected silver centers (Ag1-Ag2, 2.9-3.2 Å). In addition to this, the Ag1 ion displays coordination with the N5 and O4 atoms from both lumazine moieties and a ligand (nitrato, perchlorato or ethanol) bridging to another disilver unit. The Ag2 ion is coordinated to the N61 oxime nitrogens, a monodentate and a (O,O)-bridging nitrato/perchlorato or two monodentate O-trifluoromethylsulfonato anions. The coordination polyhedra can be best described as a strongly distorted octahedron (around Ag1) and a square-based pyramid (around Ag2). The Ag-N and Ag-O bond lengths range between 2.22-2.41 and 2.40-2.67 Å, respectively. Although the structure of 4 cannot be resolved by XRD, it is likely to be similar to those described for 2, 3 and 5, containing Ag-Ag units with S-thiocyanato terminal ligands. Finally, the structure of the tetrafluoroborate compound 6 is mononuclear with a strongly distorted tetrahedral AgN(4) core (Ag-N, 2.27-2.43 Å). Always, the different Ag-N distances found clearly point to the more basic character of the oxime N61 nitrogen atom when compared with the pyrazine N5 one. A topological analysis of the electron density within the framework provided by the quantum theory of atoms in molecules (QTAIM) using DFT(M06L) levels of
4-(Prop-2-yn-1-ylsulfanyl-1H-pyrazolo[3,4-d]pyrimidine
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Mohamed El Hafi
2017-10-01
Full Text Available The asymmetric unit of the title compound, C8H6N4S, consists of two independent molecules differing in the orientation of the side chain. In the crystal, molecules form dimers through N—H...N hydrogen bonds. The dimers stack along the a-axis direction with weak π–π stacking interactions [centroid–centroid distances of 3.898 (2 and 3.908 (2 Å]. The crystal studied was refined as a two-component twin.
Bis(O-ethyl dithiocarbonato-κ2 S,S′)bis(pyridine-3-carbonitrile-κN 1)nickel(II)
Kapoor, Sanjay; Kour, Ramandeep; Sachar, Renu; Kant, Rajni; Gupta, Vivek K.; Kapoor, Kamini
2012-01-01
The Ni2+ ion in the title complex, [Ni(C3H5OS2)2(C6H4N2)2], is in a strongly distorted octahedral coordination environment formed by an N2S4 donor set, with the Ni2+ ion located on a centre of inversion. In the crystal, weak C—H⋯S and C—H⋯N interactions are observed. PMID:22259356
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Detlef Selent
2012-02-01
Full Text Available The reaction of (η3-allyl[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I with tris(2,4-di-tert-butylphenylphosphite in toluene produces the title compound, [Rh(C42H62O3P(C8H12]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2 and 0.190 (2.
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
Energy Technology Data Exchange (ETDEWEB)
Sharma, P. [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India); Subbulakshmi, K. N.; Narayana, B. [Mangalore University, Department of Chemistry (India); Sarojini, B. K. [Mangalore University, Industrial Chemistry Division, Department of Studies in Chemistry (India); Kant, R., E-mail: rkant.ju@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India)
2016-03-15
The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C{sub 15}H{sub 11}N{sub 3}O{sub 2}S{sub 2} · C{sub 3}H{sub 7}NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.
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Andreas Roodt
2009-12-01
Full Text Available In the title compound, [Rh(C13H16NO(C18H15P(CO]·0.5C3H6O, the Rh atom exhibits a square-planar coordination geometry, being coordinated by the N and O atoms of the bidentate β-diketonato ligand, a P atom from the triphenylphosphine unit and a C atom from the carbonyl group. The asymmetric unit also contains a disordered half-molecule, lying about an inversion center, of the acetone solvate. Intermolecular C—H...O hydrogen bonds are observed between a C—H group of the triphenylphosphine unit and a carbonyl O atom and between the methyl group of the enaminoketonato backbone and the solvent O atom. In addition, an intramolecular interaction is observed between a C—H group of the triphenylphosphine unit and the O atom of the enaminoketonato ligand.
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Lip Lin Koh
2011-01-01
Full Text Available In the title compound, C16H13N7O, the 1,2,4-triazolo[1,5-a][1,3,5]triazine heterocyclic system is essentially planar (r.m.s. deviation = 0.0375 Å. The attached benzene ring lies almost in the mean plane of 1,2,4-triazolo[1,5-a][1,3,5]triazine [dihedral angle = 1.36 (23°], while the pyridine ring is turned out of this plane by the aminomethyl bridge [dihedral angle = 69.22 (9°]. The amino group H atom is involved in intramolecular hydrogen bonding with a triazole N atom. In the crystal, molecules are connected via C(=ONH...N hydrogen bonds into C(11 chains parallel to [100]. The amino group H atom acts as a hydrogen-bond donor, forming an NH...O=C hydrogen bond with the carbonyl O atom, which links the molecules into C(6 chains running along [011] and [01overline{1}].
Experimental and computational thermochemistry of 6,7-dihydro-4(5H)-benzofuranone
International Nuclear Information System (INIS)
Sousa, Clara C.S.; Morais, Victor M.F.; Matos, M. Agostinha R.
2013-01-01
Highlights: ► Standard molar enthalpy of formation of 6,7-dihydro-4(5H)-benzofuranone was obtain. ► Computational estimative of the standard molar enthalpy of formation. ► Computational and experimental values agree. ► Estimates of the standard molar enthalpy of formation of the isomers were obtain. - Abstract: The standard (p = 0.1 MPa) molar enthalpy of formation of 6,7-dihydro-4(5H)-benzofuranone was measured, at T = 298.15 K, by static bomb calorimetry and the standard molar enthalpy of vaporization, at T = 298.15 K, was obtained using Calvet microcalorimetry. These values were combined together to derive the standard molar enthalpy of formation of the title compound in gaseous phase, at T = 298.15 K, −(226.0 ± 2.8) kJ · mol −1 . Additionally, density functional theoretical calculations using the B3LYP hybrid exchange-correlation energy functional with extended basis sets and also other higher-level ab initio quantum calculations have been performed.
2-(4-Chlorobenzoyl-3,6-dimethoxynaphthalene
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Noriyuki Yonezawa
2008-03-01
Full Text Available In the title compound, C19H15ClO3, the interplanar angle between the naphthalene and benzene ring systems is 62.67 (6°. The carbonyl group is twisted from both ring planes, with torsion angles of −44.9 (2° with respect to the naphthalene ring and −26.7 (2° with respect to the phenylene ring. There is an intermolecular hydrogen bond between an H atom of one methoxy group and the O atom of the second methoxy group, forming chains along the ac diagonal.
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Jianxin Xing
2009-04-01
Full Text Available The title compound, [Co(C18H18N2O4Cl(H2O]·H2O, contains a distorted octahedral cobalt(III complex with a 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolate ligand, a chloride and an aqua ligand, and also a disordered water solvent molecule (half-occupancy. The CoIII ion is coordinated in an N2O3Cl manner. Weak O—H...O hydrogen bonds may help to stabilize the crystal packing.
Rhodium(III)- and iridium(III)-catalyzed C7 alkylation of indolines with diazo compounds.
Ai, Wen; Yang, Xueyan; Wu, Yunxiang; Wang, Xuan; Li, Yuanchao; Yang, Yaxi; Zhou, Bing
2014-12-22
A Rh(III)-catalyzed procedure for the C7-selective C-H alkylation of various indolines with α-diazo compounds at room temperature is reported. The advantages of this process are: 1) simple, mild, and pH-neutral reaction conditions, 2) broad substrate scope, 3) complete regioselectivity, 4) no need for an external oxidant, and 5) N2 as the sole byproduct. Furthermore, alkylation and bis-alkylation of carbazoles at the C1 and C8 positions have also been developed. More significantly, for the first time, a successful Ir(III)-catalyzed intermolecular insertion of arene C-H bonds into α-diazo compounds is reported. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
3,4-Diaminopyridinium 2-carboxy-4,6-dinitrophenolate
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Madhukar Hemamalini
2010-11-01
Full Text Available In the title salt, C5H8N3+·C7H3N2O7−, the pyridine N atom of the 3,4-diaminopyridine molecule is protonated. The 3,5-dinitrosalicylate anion shows whole-molecule disorder over two orientations with a refined occupancy ratio of 0.875 (4: 0.125 (4. In the crystal, the cations and anions are connected by intermolecular N—H...O and C—H...O hydrogen bonds, forming a three-dimensional network.
Li, Yunyun; Qi, Zisong; Wang, He; Yang, Xifa; Li, Xingwei
2016-09-19
Indoles are an important structural motif that is commonly found in biologically active molecules. In this work, conditions for divergent couplings between imidamides and acceptor-acceptor diazo compounds were developed that afforded NH indoles and 3H-indoles under ruthenium catalysis. The coupling of α-diazoketoesters afforded NH indoles by cleavage of the C(N2 )-C(acyl) bond whereas α-diazomalonates gave 3H-indoles by C-N bond cleavage. This reaction constitutes the first intermolecular coupling of diazo substrates with arenes by ruthenium-catalyzed C-H activation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Energy Technology Data Exchange (ETDEWEB)
Constable, D A; Dring, L G [Upjohn Ltd., Crawley (UK); Jones, J R [Surrey Univ., Guildford (UK). Dept. of Chemistry
1990-07-01
Three radiolabelled forms of trospectomycin (6'-n-propylspectinomycin sulphate hydrate) have been synthesised, namely (8'-{sup 14}C)-, (6',7'-{sup 3}H)-, and (5',6',7'-{sup 3}H)-trospectomycin. Although all three forms of the drug are metabolically stable and therefore suitable for use in animal studies the {sup 14}C compound is produced in poor yield as is the (6',7'-{sup 3}H)trospectomycin. On the other hand, the (5',6',7'-{sup 3}H)-form is produced in good yield and appears to be the labelled form of choice. Following subcutaneous administration of any of the labelled forms to rats, more than 50% of the dose was excreted in the urine as unchanged drug during the first 6h after dosing. Approximately 80% and 10% of the dose appeared in the urine and faeces respectively after 6 days. (author).
Crystal structure of 1-[(6-chloropyridin-3-ylsulfonyl]-1,2,3,4-tetrahydroquinoline
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S. Jeyaseelan
2015-06-01
Full Text Available The tetrahydropyridine ring of the quinoline system in the title compound, C14H13ClN2O2S, adopts a half-chair conformation with the bond-angle sum at the N atom being 350.0°. The dihedral angle between the least-squares planes of the two aromatic rings is 50.13 (11°. In the crystal, inversion dimers linked by pairs of C—H...O hydrogen bonds generate R22(10 loops. Additional intermolecular C—H...O hydrogen bonds generate C(7 chains along [100].
2-Ureido-1,3-thiazol-3-ium dihydrogen phosphate
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Kateryna Gubina
2011-07-01
Full Text Available The title compound, C4H6N3OS+·H2PO4−, (I, was obtained as a result of hydrolysis of [(1,3-thiazol-2-ylaminocarbonyl]phosphoramidic acid, (II, in water. X-ray analysis has shown that the N—P bond in (II breaks, leading to the formation of the substituted carbamide (I. This compound exists as an internal salt. The unit cell consists of a urea cation and an anion of H2PO4−. Protonation of the N atom of the heterocyclic ring was confirmed by the location of the H atom in a difference Fourier map. The molecules of substituted urea are connected by O...O hydrogen bonds into unlimited planes. In turn, those planes are connected to each other via N—H...O hydrogen bonds with molecules of phosphoric acid, forming a three-dimensional polymer.
Ethyl 4,6-O-benzylidene-2-deoxy-N-phthalimido-1-thio-β-d-glucopyranoside
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Göran Widmalm
2010-12-01
Full Text Available In the title compound, C23H23NO6S, the plane of the N-phthalimido group makes a dihedral angle of 67.4 (1° with the least square plane of the sugar ring defined by the C2, C3, C5 and O5 atoms using standard glucose nomenclature. The thioethyl group has the exo-anomeric conformation. In the crystal, intermolecular hydrogen bonds involving the hydroxy groups and the carbonyl O atoms of adjacent N-phthalimido groups form chains parallel to the b axis. The chains are further stabilized by C—H...π interactions.
Crystal structure of (1R,3S,8R,11R-11-acetyl-3,7,7-trimethyl-10-oxatricyclo[6.4.0.01,3]dodecan-9-one
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Abdoullah Bismoussa
2015-12-01
Full Text Available The title compound, C16H24O3, is built up from three fused rings, a six-membered, a seven-membered and a three-membered ring. The absolute configuration of the title compound was determined as (1R,3S,8R,11R based on the synthetic pathway. The six-membered ring has an half-chair conformation whereas the seven-membered ring displays a boat conformation. In the cyrstal, C—H...O hydrogen bonds build up a two-dimensional network parallel to (0 0 1. The crystal studied was an inversion twin with a minor twin component of 34%.
2,2,3,3,5,5,6,6-Octa-p-tolyl-1,4-dioxa-2,3,5,6-tetragermacyclohexane dichloromethane disolvate
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Monika L. Amadoruge
2009-09-01
Full Text Available The title compound, C56H56Ge4O2·2CH2Cl2 or Tol8Ge4O2·2CH2Cl2 (Tol = p-CH3C6H4, was obtained serendipitously during the attempted synthesis of a branched oligogermane from Tol3GeNMe2 and PhGeH3. The molecule contains an inversion center in the middle of the Ge4O2 ring which is in a chair conformation. The Ge—Ge bond distance is 2.4418 (5 Å and the Ge—O bond distances are 1.790 (2 and 1.785 (2 Å. The torsion angles within the Ge4O2 ring are −56.7 (1 and 56.1 (1° for the Ge—Ge—O—Ge angles and −43.9 (1° for the O—Ge—Ge—O angle.
Synthesis and characterization of diphenyltin (IV) dithiocarbamate compounds
International Nuclear Information System (INIS)
Amirah Faizah Abdul Muthalib; Ibrahim Baba; Yang Farina; Mohd Wahid Samsudin
2011-01-01
Ten compounds of diphenyltin(IV) with N-dialkyl dithiocarbamate were successfully prepared using in situ methods. Elemental analysis data (C, H, N and S) showed an agreement with the general formula of (C 6 H 5 ) 2 Sn[S 2 CNR 1 R 2 ] (R 1 = CH 3 , C 2 H 5 , C 7 H 7 ; R 2 = C 2 H 5 , C 4 H 9 , C 6 H 1 1, iC 3 H 7 , C 7 H 7 ). The structures of these compounds have been examined by infrared spectroscopy, ultraviolet, 1 H, 13 C and 119 Sn NMR spectroscopy and X-ray crystallography. The infrared spectra of these compounds showed three important peaks for v(C...N), v(C...S) and v(C...S) bands that appeared in the region of 1474 -1499, 969 - 995 and 324 - 335 cm -1 respectively. Data for 13 C NMR spectroscopy showed an important peak in the region of 198 - 200 ppm that corresponded to the NCS 2 group. Single crystal X-ray diffraction studies showed (C 6 H 5 ) 2 Sn[S 2 CN(C 2 H 5 )(CH 3 )] 2 (1) is six coordinated and adopted a monoclinic system with space group C2/c, while (C 6 H 5 ) 2 SnCl[S 2 CN(C 7 H 7 )(iC 3 H 7 )] (2) is five coordinated, crystallized in monoclinic system with space group Pb 1 /n. Meanwhile, six coordinated (C 6 H 5 ) 2 Sn[S 2 CN(CH 3 )(iC 3 H 7 )] 2 (3) adopted a orthorhombic system with a space group Pbcn. (author)
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Lan-Sun Zheng
2009-12-01
Full Text Available The asymmetric unit of the title compound [Zn8(C16H12N2O44(H2O4]·6C3H7NO, consists of eight ZnII cations, four tetravalent anionic ligands, L4− (L4− = 3,3′-(1E,1′E-(ethane-1,2-diylbis(azan-1-yl-1-ylidenebis(methan-1-yl-1-ylidenedibenzene-1,2-bis(olate, four coordinated water molecules and six N,N-dimethylformamide solvate molecules. The coordination complex comprises an octanuclear ZnII unit with its ZnII centers coordinated in two discrete distorted square-pyramidal geometries. Four ZnII atoms each coordinate to two nitrogen atoms and two phenolate oxygen atoms from an individual L4− ligand and one coordinated water molecule. The other four ZnII atoms each bind to five phenolate oxygen atoms from three different L4− ligands. In the crystal structure, the ZnII complex unit, coordinated water molecules and dimethylformamide solvate molecules are linked via O—H...O and C—H...O hydrogen bonds. Molecules are connected by additional intermolecular O—H...O and C—H...O hydrogen bonds, forming an extensive three dimensional framework.
International Nuclear Information System (INIS)
Standridge, R.T.; Swigor, J.E.
1993-01-01
The title compound ([ 14 C]cefepime hydrochloride) was prepared as follows:- [ 14 C]Thiourea was condensed with ethyl 4-bromo-3-oxo-2-methoxyimino-acetate providing ethyl 2-(2-amino-4-[2- 14 C] thiazolyl)-2-methoxyi-minoacetate as the pure Z-isomer. Saponification gave the amino acid this was reacted with 1-hydroxybenzotriazole to give the activated ester. Condensation in situ with 7-amino-3-(1-methylpyrrolidinio) methyl-3-cephem-4-carboxylate yielded the product as the pure sulfate salt. Treatment of the sulfate salt with base provided the zwitterion isolated as the stable N-methyl-2-pyrrolidinone adduct. An aqueous solution of the adduct was converted to the crystalline title compound, [ 14 C]Cefepime hydrochloride hydrate, with hydrochloric acid/acetone. Radiochemical purity was 99.0% and specific activity, 34.2 μCi/mg. Overall yield from [ 14 C]thiourea was 18%. (Author)
N-{2-[2-(5-Methyl-1H-pyrazol-3-ylacetamido]phenyl}benzamide monohydrate
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Karim Chkirate
2017-02-01
Full Text Available The asymmetric unit of the title compound, C19H18N4O2·H2O, comprises the U-shaped pyrazole derivative and a solvent water molecule. The molecular conformation is partly determined by an intramolecular N—H...O hydrogen bond. The crystal packing is directed by an extensive network of O—H...O, N—H...O, N—H...N and C—H...O hydrogen bonds together with C—H...π(ring contacts that generate a three-dimensional network.
Liu, Zhaohong; Sivaguru, Paramasivam; Zanoni, Giuseppe; Anderson, Edward A; Bi, Xihe
2018-05-08
A catalyst-dependent chemoselective one-carbon insertion of diazo compounds into the C-C or C-H bonds of 1,3-dicarbonyl species is reported. In the presence of silver(I) triflate, diazo insertion into the C(=O)-C bond of the 1,3-dicarbonyl substrate leads to a 1,4-dicarbonyl product containing an all-carbon α-quaternary center. This reaction constitutes the first example of an insertion of diazo-derived carbenoids into acyclic C-C bonds. When instead scandium(III) triflate was applied as the catalyst, the reaction pathway switched to formal C-H insertion, affording 2-alkylated 1,3-dicarbonyl products. Different reaction pathways are proposed to account for this powerful catalyst-dependent chemoselectivity. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Xiao Zhen Feng
2008-05-01
Full Text Available In the title compound, [Cu(C13H13Cl2NO3(C3H7NO], the CuII atom is coordinated in a slightly distorted square-planar geometry by two O atoms and one N atom from the tridentate chiral ligand 2-[(3,5-dichloro-2-oxidobenzylideneamino]-3-methylpentanoate and by one O atom from dimethylformamide. In the crystal structure, the Cu atom forms contacts with Cl and O atoms of two units (Cu...Cl and Cu...O = 3.401 and 2.947 Å, respectively, thereby forming an approximately octahedral arrangement. A three-dimensional network is constructed through Cl...Cu, O...Cu, Cl...Cl contacts and C—H...O hydrogen bonds.
7-Chloro-11a-phenyl-2,3,5,10,11,11a-hexahydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11-dione
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Vahan Martirosyan
2008-03-01
Full Text Available The title compound, C18H15ClN2O2, is a potential human immunodeficiency virus type-1 (HIV-1 non-nucleoside reverse transcriptase inhibitor. The pyrrolidine ring adopts an envelope and the diazepine ring a boat conformation. In the crystal structure, two isomers (R and S form centrosymmetric dimers via N—H...O hydrogen bonds.
Bis[bis(3,5-diamino-1H-1,2,4-triazol-4-ium)copper(I)] tris(hexafluoridosilicate)
Marian Mys'kiv; Evgeny Goreshnik
2010-01-01
In the title compound, [Cu(C2H6N5)2]2(SiF6)3, the asymmetric unit is composed of one [Cu(HL)2]3+ cation (where L is 3,5-diamino-1,2,4-triazole) and one and a half SiF62− anions. The rather large positively charged guanazole ligand moiety promotes the low metal coordination number of 2 for the CuI atom. The compound was obtained using the electrochemical alternating-current technique starting from an ethanol–methanol solution of CuSiF6·4H2O and guanazole. In the cr...
Prakash, S. M.; Pandiarajan, K.; Kumar, S.
2013-06-01
Four new [N-methyl-3t-alkyl-2r,6c-diaryl-4-ylidine]-5'-methylthiozolidin-4-ones 9-12 have been synthesized by the condensation of N-methyl-3t-alkyl-2r,6c-diarylpiperidin-4-one thiosemicarbazones with ethyl 2-bromopropionate. These compounds have been characterized using FT-IR, 1H NMR, 13C NMR spectral techniques. HOMOCOSY, HSQC and HMBC spectral study have been done for [N-methyl-3,3-dimethyl-2r,6c-bis(p-methoxyphenyl)piperidin-4-ylidine]-5'-methylthiazolidine-4-one (12). Two geometrical isomers are formed in this reaction. In all these compounds piperidin rings adopt chair conformation. The rotation of the aryl group at C-2 is rather slow in 10-12. Antimicrobial activities have also been studied for 9-12. These compounds are active against all the tested bacterial and fungal strains.
Dichloridobis(4-methyl-3,5-diphenyl-1H-pyrazole-κN2copper(II
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Moayad Hossaini Sadr
2011-12-01
Full Text Available The asymmetric unit of the title compound, [CuCl2(C16H14N22], comprises half of the complex. The CuII atom lies on a crystallographic twofold rotation axis and shows a significantly distorted tetrahedral coordination geometry. The dihedral angle between the phenyl rings is 74.3 (2°. The crystal structure is stabilized by intermolecular π–π interactions [centroid–centroid distances = 3.635 (2–3.803 (3 Å].
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Zhensheng Li
2013-07-01
Full Text Available The title compound, C26H24BF2N3O, comprises a boron–dipyrromethene (BODIPY framework and a phenolic Schiff base substituent group. The BODIPY unit is close to planar [maximum deviation from the least-squares plane = 0.040 (3 Å], and forms a dihedral angle of 80.38 (13° with the meso-substituent phenyl ring and an angle of 56.57 (13° with the phenolic ring in the extended substituent chain. An intramolecular O—H...N hydrogen bond is formed between the phenolic hydroxyl group and the Schiff base N-atom. The crystal studied was a non-merohedral twin with a BASF factor of 0.447 (3 for the two components.
Poly[[tetraaqua(μ3-naphthalene-1,6-disulfonato-κ4O1:O6,O6′:O6′′strontium(II] monohydrate
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Shan Gao
2011-12-01
Full Text Available In the crystal structure of the polymeric title compound, {[Sr(C10H6O6S2(H2O4]·H2O}n, the naphthalene-1,6-disulfonate dianion uses one –SO3 unit to O,O′-chelate to an SrII cation and its third O atom to bind to another SrII cation. The other –SO3 unit binds to yet another SrII atom. The four coordinated water molecules are monodentate but one is disordered over two positions in a 1:1 ratio. The μ3-bonding mode of the dianion generates a polymeric three-dimensional network; the network is consolidated by O—H...O hydrogen bonds. The SrII cation exists in an undefined eight-coordinate environment.
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Van Tuyen Nguyen
2017-03-01
Full Text Available The title compound, C20H24N2O4, is the product of a ring-expansion reaction from a seven-membered hexahydroazepine to a nine-membered azonine. The azonine ring of the molecule adopts a chair–boat conformation. In the crystal, molecules are linked by bifurcated N—H...(O,O hydrogen bonds, generating [010] zigzag chains. The title compound shows inhibitory activity against acetylcholinesterase and butyrylcholinesterase, and might be considered as a candidate for the design of new types of anti-Alzheimer's drugs.
4-{[(1-Phenyl-1H-pyrazol-3-yloxy]methyl}-1,3-dioxolan-2-one
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Algirdas Šačkus
2012-11-01
Full Text Available The title compound was obtained by the reaction of tosylated glycerol carbonate with 1-phenyl-1H-pyrazol-3-ol in a good 71% yield. Detailed spectroscopic data (1H-NMR, 13C-NMR, 15N-NMR, IR, MS are presented.
(2E-3-(3-Methoxy-1-phenyl-1H-pyrazol-4-yl-2-propenal
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Algirdas Šačkus
2009-12-01
Full Text Available The palladium-catalyzed reaction of 4-bromo-3-methoxy-1-phenyl-1H-pyrazole with acrolein diethyl acetal gives the title compound in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.
Rhodamine 6G hexachloridostannate(IV acetonitrile disolvate
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Ramaiyer Venkatraman
2008-01-01
Full Text Available In the title compound, bis({6-ethylamino-10-[2-(methoxycarbonylphenyl]-2,7-dimethylxanthen-3-ylidene}ethanaminium hexachloridotin(IV acetonitrile disolvate, (C27H29N2O32[SnCl6]·2C2H3N, the octahedral SnCl62− anion lies on an inversion center. The xanthene ring system is essentially planar, with an average deviation of 0.020 Å, and the substituent benzene ring forms a dihedral angle of 85.89 (2° with it. The Sn—Cl distances are in the range 2.4237 (3–2.4454 (3 Å. There are N—H...Cl hydrogen bonds between SnCl62− ions and rhodamine 6G cations as well as π–π stacking interactions between rhodamine 6G cations (interplanar distance of 3.827 Å.
2-{N-[(2,3,4,9-Tetrahydro-1H-carbazol-3-ylmethyl]methylsulfonamido}ethyl methanesulfonate
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Mustafa Göçmentürk
2014-01-01
Full Text Available In the title compound, C17H24N2O5S2, the indole ring system is nearly planar [maximum deviation = 0.032 (1 Å] and the cyclohexene ring has a half-chair conformation. In the crystal, N—H...O hydrogen bonds link the molecules into a chain running along the b-axis direction. Weak C—H...O hydrogen bonds and weak C—H...π interactions are observed between the chains.
(6S,7S,8S,8aS-6-Ethyl-7,8-dihydroxy-1,5,6,7,8,8a-hexahydroindolizin-3(2H-one monohydrate
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Jozefína Žúžiová
2010-12-01
Full Text Available The absolute configuration of the title compound, C10H17NO3·H2O, was assigned from the synthesis. In the molecular structure, the central six-membered ring of the indolizine moiety adopts a chair conformation, with two atoms displaced by −0.578 (2 and 0.651 (1 Å from the plane of the other four atoms [maximum deviation 0.019 (2 Å] The conformation of the fused oxopyrrolidine ring is close to that of a flat envelope, with the flap atom displaced by 0.294 (1 Å from the plane through the remaining four atoms. In the crystal, one of the hydroxy groups is hydrogen-bonded to two water molecules, while the other hydroxy group exhibits an intermolecular hydrogen bond to the carbonyl O atom, resulting in a chain parallel to the b axis.
Characterization of a n+3C/n−4H SiC heterojunction diode
Energy Technology Data Exchange (ETDEWEB)
Minamisawa, R. A.; Mihaila, A. [Department of Power Electronics, ABB Corporate Research Center, CH-5405 Baden-Dättwil (Switzerland); Farkas, I.; Hsu, C.-W.; Janzén, E. [Semiconductor Materials, IFM, Linköping University, SE-58183 Linköping (Sweden); Teodorescu, V. S. [National Institute of Material Physics, R-077125 Bucharest-Măgurele (Romania); Afanas' ev, V. V. [Semiconductor Physics Laboratory, KU Leuven, 3001 Leuven (Belgium); Rahimo, M. [ABB Semiconductors, Fabrikstrasse 3, CH-5600 Lenzburg (Switzerland)
2016-04-04
We report on the fabrication of n + 3C/n-4H SiC heterojunction diodes (HJDs) potentially promising the ultimate thermal stability of the junction. The diodes were systematically analyzed by TEM, X-ray diffraction, AFM, and secondary ion mass spectroscopy, indicating the formation of epitaxial 3C-SiC crystal on top of 4H-SiC substrate with continuous interface, low surface roughness, and up to ∼7 × 10{sup 17 }cm{sup −3} dopant impurity concentration. The conduction band off-set is about 1 V as extracted from CV measurements, while the valence bands of both SiC polytypes are aligned. The HJDs feature opening voltage of 1.65 V, consistent with the barrier height of about 1.5 eV extracted from CV measurement. We finally compare the electrical results of the n + 3C/n-4H SiC heterojunction diodes with those featuring Si and Ge doped anodes in order to evaluate current challenges involved in the fabrication of such devices.
Aquabis(3,5-dimethyl-1H-pyrazole-κN(oxalato-κ2O,O′copper(II
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Andrii I. Buvailo
2008-01-01
Full Text Available In the title compound, [Cu(C2O4(C5H8N22(H2O], the CuII atom is coordinated in a slightly distorted square-pyramidal geometry by two N atoms belonging to the two 3,5-dimethyl-1H-pyrazole ligands, two O atoms of the oxalate anion providing an O,O′-chelating coordination mode, and an O atom of the water molecule occupying the apical position. The crystal packing shows a well defined layer structure. Intra-layer connections are realised through a system of hydrogen bonds while the nature of the inter-layer interactions is completely hydrophobic, including no hydrogen-bonding interactions.
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Ísmail Çelik
2017-06-01
Full Text Available In the title compound, C26H48N2Si4, the cycloheptane ring adopts a chair conformation, while the quinolinyl ring system is almost planar [maximum deviation = 0.040 (3 Å for one of the C atoms carrying a Me3Si group]. In the crystal, in the absence of classical hydrogen bonding, the packing is dominated by van der Waals forces. One of the N-bound trimethylsilyl groups is disordered by rotation about the C—SiMe3 bond, and was modelled over two sets of sites in the ratio 0.873 (8:0.127 (8.
International Nuclear Information System (INIS)
Lee, Yu-Fang; Kong, Lin-Jun; Lee, Yuan-Pern
2012-01-01
Irradiation at 239 ± 20 nm of a p-H 2 matrix containing methoxysulfinyl chloride, CH 3 OS(O)Cl, at 3.2 K with filtered light from a medium-pressure mercury lamp produced infrared (IR) absorption lines at 3028.4 (attributable to ν 1 , CH 2 antisymmetric stretching), 2999.5 (ν 2 , CH 3 antisymmetric stretching), 2950.4 (ν 3 , CH 3 symmetric stretching), 1465.2 (ν 4 , CH 2 scissoring), 1452.0 (ν 5 , CH 3 deformation), 1417.8 (ν 6 , CH 3 umbrella), 1165.2 (ν 7 , CH 3 wagging), 1152.1 (ν 8 , S=O stretching mixed with CH 3 rocking), 1147.8 (ν 9 , S=O stretching mixed with CH 3 wagging), 989.7 (ν 10 , C-O stretching), and 714.5 cm -1 (ν 11 , S-O stretching) modes of syn-CH 3 OSO. When CD 3 OS(O)Cl in a p-H 2 matrix was used, lines at 2275.9 (ν 1 ), 2251.9 (ν 2 ), 2083.3 (ν 3 ), 1070.3 (ν 4 ), 1056.0 (ν 5 ), 1085.5 (ν 6 ), 1159.7 (ν 7 ), 920.1 (ν 8 ), 889.0 (ν 9 ), 976.9 (ν 10 ), and 688.9 (ν 11 ) cm -1 appeared and are assigned to syn-CD 3 OSO; the mode numbers correspond to those used for syn-CH 3 OSO. The assignments are based on the photolytic behavior and a comparison of observed vibrational wavenumbers, infrared intensities, and deuterium isotopic shifts with those predicted with the B3P86/aug-cc-pVTZ method. Our results extend the previously reported four transient IR absorption bands of gaseous syn-CH 3 OSO near 2991, 2956, 1152, and 994 cm -1 to 11 lines, including those associated with C-O, O-S, and S=O stretching modes. Vibrational wavenumbers of syn-CD 3 OSO are new. These results demonstrate the advantage of a diminished cage effect of solid p-H 2 such that the Cl atom, produced via UV photodissociation of CH 3 OS(O)Cl in situ, might escape from the original cage to yield isolated CH 3 OSO radicals.
Lee, Yu-Fang; Kong, Lin-Jun; Lee, Yuan-Pern
2012-03-28
Irradiation at 239 ± 20 nm of a p-H(2) matrix containing methoxysulfinyl chloride, CH(3)OS(O)Cl, at 3.2 K with filtered light from a medium-pressure mercury lamp produced infrared (IR) absorption lines at 3028.4 (attributable to ν(1), CH(2) antisymmetric stretching), 2999.5 (ν(2), CH(3) antisymmetric stretching), 2950.4 (ν(3), CH(3) symmetric stretching), 1465.2 (ν(4), CH(2) scissoring), 1452.0 (ν(5), CH(3) deformation), 1417.8 (ν(6), CH(3) umbrella), 1165.2 (ν(7), CH(3) wagging), 1152.1 (ν(8), S=O stretching mixed with CH(3) rocking), 1147.8 (ν(9), S=O stretching mixed with CH(3) wagging), 989.7 (ν(10), C-O stretching), and 714.5 cm(-1) (ν(11), S-O stretching) modes of syn-CH(3)OSO. When CD(3)OS(O)Cl in a p-H(2) matrix was used, lines at 2275.9 (ν(1)), 2251.9 (ν(2)), 2083.3 (ν(3)), 1070.3 (ν(4)), 1056.0 (ν(5)), 1085.5 (ν(6)), 1159.7 (ν(7)), 920.1 (ν(8)), 889.0 (ν(9)), 976.9 (ν(10)), and 688.9 (ν(11)) cm(-1) appeared and are assigned to syn-CD(3)OSO; the mode numbers correspond to those used for syn-CH(3)OSO. The assignments are based on the photolytic behavior and a comparison of observed vibrational wavenumbers, infrared intensities, and deuterium isotopic shifts with those predicted with the B3P86∕aug-cc-pVTZ method. Our results extend the previously reported four transient IR absorption bands of gaseous syn-CH(3)OSO near 2991, 2956, 1152, and 994 cm(-1) to 11 lines, including those associated with C-O, O-S, and S=O stretching modes. Vibrational wavenumbers of syn-CD(3)OSO are new. These results demonstrate the advantage of a diminished cage effect of solid p-H(2) such that the Cl atom, produced via UV photodissociation of CH(3)OS(O)Cl in situ, might escape from the original cage to yield isolated CH(3)OSO radicals.
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Hoong-Kun Fun
2009-01-01
Full Text Available The asymmetric unit of the title compound, C27H24N4O2·0.5C2H6O, comprises two crystallographically independent molecules (A and B with slightly different conformations, and one ethanol molecule of crystallization. Intramolecular C—H...O and O—H...O hydrogen bonds generate six- and eight-membered rings, producing S(6 and S(8 ring motifs, respectively. In molecule A, one of the benzene rings is disordered over two positions, with site-occupancy factors of 0.542 (11 and 0.458 (11. The dihedral angles between the central benzene ring and the two outer benzene rings are 73.88 (9 and 82.6 (2/88.9 (2° in molecule A, and 80.81 (8 and 79.38 (8° in molecule B. In the crystal structure, molecules form infinite one-dimensional chains in the (101 plane. The crystal structure is stabilized by intermolecular O—H...N, N—H...N, N—H...O and C—H...O hydrogen bonds, weak C—H...π and π–π [centroid–centroid = 3.5496 (1 Å] interactions.
International Nuclear Information System (INIS)
Vaqueiro, Paz
2006-01-01
Two new main group metal sulphides, [C 1 N 4 H 26 ] 0.5 [InS 2 ] (1) and [C 1 N 4 H 26 ] 0.5 [GaS 2 ] (2) have been prepared solvothermally in the presence of 1,4-bis(3-aminopropyl)piperazine and their crystal structures determined by single-crystal X-ray diffraction. Both compounds are isostructural and crystallise in the monoclinic space group P2 1 /n (Z=4), with a=6.5628(5), b=11.2008(9), c=12.6611(9) A and β=94.410(4) o (wR=0.035) for compound (1) and a=6.1094(5), b=11.2469(9), c=12.7064(10) A and β=94.313(4) o (wR=0.021) for compound (2). The structure of [C 1 N 4 H 26 ] 0.5 [MS 2 ] (M=In,Ga) consists of one-dimensional [MS 2 ] - chains which run parallel to the crystallographic a axis and are separated by diprotonated amine molecules. These materials represent the first example of solvothermally prepared one-dimensional gallium and indium sulphides. -- Graphical abstract: [C 1 N 4 H 26 ] 0.5 [InS 2 ] and [C 1 N 4 H 26 ] 0.5 [GaS 2 ], prepared under solvothermal conditions, consist of one-dimensional [MS 2 ] - chains separated by diprotonated 1,4-bis(3-aminopropyl)piperazine molecules
Energy Technology Data Exchange (ETDEWEB)
Valencia, Israel, E-mail: israelv@unam.mx
2016-09-12
Highlights: • Optimized structures of iron clusters capped with one benzene molecule. • Adsorption of benzene molecules quenches the magnetic moment of Fe clusters. • Adsorption of benzene on iron clusters leads to activation of non IR active vibrations of benzene. • Adsorption of benzene in small Fe{sub n} clusters is explained by the charge transfer model. • Relation between Fe{sub n}–benzene electron affinity and reactivity is observed. - Abstract: The structural, energetic, electronic, vibrational, and magnetic properties of iron–benzene clusters, Fe{sub n}–C{sub 6}H{sub 6}, n ⩽ 7, were calculated using an all-electron density functional theory, DFT, with the generalized gradient approximation and the 6−311++G(2d,2p) basis set. A proposal regarding the mechanism of the adsorption of benzene on iron clusters related to the charge transfer model is described. A direct relation between the calculated electron affinity, EA, of the Fe{sub n}–C{sub 6}H{sub 6} clusters and their reactivity were also determined.
Crystal structure of tetraaqua[2-(pyridin-2-yl-1H-imidazole-κ2N2,N3]iron(II sulfate
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Zouaoui Setifi
2015-04-01
Full Text Available In the title compound, [Fe(C8H7N3(H2O4]SO4, the central FeII ion is octahedrally coordinated by two N atoms from the bidentate 2-(pyridin-2-yl-1H-imidazole ligand and by four O atoms of the aqua ligands. The largest deviation from the ideal octahedral geometry is reflected by the small N—Fe—N bite angle of 76.0 (1°. The Fe—N coordination bonds have markedly different lengths [2.1361 (17 and 2.243 (2 Å], with the shorter one to the pyrimidine N atom. The four Fe—O coordination bond lengths vary from 2.1191 (18 to 2.1340 (17 Å. In the crystal, the cations and anions are arranged by means of medium-strength O—H...O hydrogen bonds into layers parallel to the ab plane. Neighbouring layers further interconnect by N—H...O hydrogen bonds involving the imidazole fragment as donor group to one sulfate O atom as an acceptor. The resulting three-dimensional network is consolidated by C—H...O, C—H...π and π–π interactions.
Aquachloridobis[5-(2-pyridyl-1H-tetrazolato-κN1]iron(III
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Bo Wang
2009-08-01
Full Text Available The title compound, [Fe(C6H4N52Cl(H2O], was synthesized by hydrothermal reaction of FeCl3 with 2-(1H-tetrazol-5-ylpyridine. The iron(III metal centre exhibits a distorted octahedral coordination geometry provided by four N atoms from two bidentate organic ligands, one water O atom and one chloride anion. The pyridine and tetrazole rings are nearly coplanar [dihedral angles = 4.32 (15 and 5.04 (14°]. In the crystal structure, intermolecular O—H...N hydrogen bonds link the complex molecules into a two-dimensional network parallel to (100.
International Nuclear Information System (INIS)
Boyter, H.A. Jr.; Grimes, R.N.
1988-01-01
The open-chain dialkynes EtC≡C(CH 2 ) n C≡CEt (n = 4, 6), the trialkyne HC≡C(CH 2 ) 5 C≡CH, and the cyclic dialkynes CH 2 (CH 2 ) 4 C≡C(CH 2 ) n C≡C (n = 4-6) were treated with B 5 H 9 and (C 2 H 5 ) 3 to give the corresponding nido-carborane oligomers, in which the original -C≡C- units are converted to -CB 4 H 6 C- nido-carborane cages. In each case, all available -C≡C- groups were transformed to carborane moieties. No partially converted products (having both carborane and -C≡C- groups in the chain) were found; when the B 5 H 9 /-C≡C- ratio employed was 2+ and oxidative fusion, forming products incorporating C 4 B 8 cages. The cyclic bis(carborane) CH 2 (CH 2 ) 4 CB 4 H 6 C(CH 2 ) 5 CB 4 H 6 C is an air-stable oil that can be deprotonated but does not under metal-promoted oxidative fusion. All products were characterized by 11 B and 1 H NMR, infrared, visible-uv, and mass spectroscopy, and the 13 C NMR spectra of linear bis(carboranes) are reported. 9 references, 7 figures, 4 tables
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Schultz, Peter; Oeckler, Oliver [Institute of Mineralogy, Crystallography and Materials Science, Faculty of Chemistry and Mineralogy, Leipzig University, Scharnhorststrasse 20, 04275 Leipzig (Germany); Durach, Dajana; Schnick, Wolfgang [Department of Chemistry, University of Munich (LMU), Butenandtstrasse 5-13, 81377 Munich (Germany)
2016-05-15
The nitridosilicate chloride Ba{sub 1.63}La{sub 7.39}Si{sub 11}N{sub 23}Cl{sub 0.42}:Ce{sup 3+} was synthesized by metathesis reaction starting from LaCl{sub 3}, BaH{sub 2}, CeF{sub 3} and the product of the ammonolysis of Si{sub 2}Cl{sub 6}. The title compound is stable towards air and moisture. Diffraction data of a microcrystal were recorded using microfocused synchrotron radiation. X-ray spectroscopy confirms the chemical composition of the crystal. IR spectra corroborate absence of N-H bonds. The compound is homeotypic to Ba{sub 2}Nd{sub 7}Si{sub 11}N{sub 23} and crystallizes in space group Cmmm with a = 11.009(3), b = 23.243(8), c = 9.706(4) Aa and Z = 4, R{sub 1}(all) = 0.0174. According to bond valence sum calculations, some crystallographic positions show complete occupancy by Ba or La whereas others contain significant amounts of both elements. In contrast to the structure prototype Ba{sub 2}Nd{sub 7}Si{sub 11}N{sub 23}, Ba{sub 1.63}La{sub 7.39}Si{sub 11}N{sub 23}Cl{sub 0.42}:Ce{sup 3+} contains chloride ions in channels of the SiN{sub 4} tetrahedra network, hinting at various substitution possibilities of the complex zeolite-like structure. (Copyright copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)
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Ahmed Benzalim
2016-08-01
Full Text Available The title compound, C16H24Cl2O, was synthesized by treating (1S,3R,8S,9R,10S-2,2-dichloro-3,7,7,10-tetramethyl-9,10-epoxytricyclo[6.4.0.01,3]dodecane with a concentrated solution of hydrobromic acid. It is built up from three fused rings: a cycloheptane ring, a cyclohexyl ring bearing alkene and hydroxy substituents, and a cyclopropane ring bearing two chlorine atoms. The asymmetric unit contains two molecules linked by an O—H...O hydrogen bond. In the crystal, further O—H...O hydrogen bonds build up an R44(8 cyclic tetramer. One of the molecules presents disorder that affects the seven-membered ring. In both molecules, the six-membered rings display a chair conformation, whereas the seven-membered rings display conformations intermediate between boat and twist-boat for the non-disordered molecule and either a chair or boat and twist-boat for the disordered molecule owing to the disorder. The absolute configuration for both molecules is 1S,3R,8R,9R and was deduced from the chemical pathway and further confirmed by the X-ray structural analysis.
trans-Tetraaquabis(isonicotinamide-κN1cobalt(II bis(3-hydroxybenzoate tetrahydrate
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Tuncer Hökelek
2012-03-01
Full Text Available The asymmetric unit of the title compound, [Co(C6H6N2O2(H2O4](C7H5O32·4H2O, contains one-half of the complex cation with the CoII ion located on an inversion center, a 3-hydroxybenzoate counter-anion and two uncoordinated water molecules. Four water O atoms in the equatorial plane around the CoII ion [Co—O = 2.0593 (16 and 2.1118 (16 Å] form a slightly distorted square-planar arrangement, and the distorted octahedral geometry is completed by the two N atoms [Co—N = 2.1306 (18 Å] from two isonicotinamide ligands. In the anion, the carboxylate group is twisted from the attached benzene ring at 8.84 (17°. In the crystal, a three-dimensional hydrogen-bonding network, formed by classical O—H...O and N—H...O hydrogen bonds, consolidates the crystal packing, which exhibits π–π interactions between the benzene and pyridine rings, with centroid–centroid distances of 3.458 (1 and 3.606 (1 Å, respectively.
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Ming-Hua Yang
2008-11-01
Full Text Available In the title compound, {[Ni2(C7H3NO52(C12H12N2(H2O2]·4H2O}n, two NiII ions, two tridentate pyridine-2,6-dicarboxylate N-oxide ligands and two coordinated water molecules form centrosymmetric dinuclear units, which are further bridged by centrosymmetric 1,2-di-4-pyridylethane ligands into polymeric chains along [210]. Each NiII ion has a distorted square-pyramidal environment, with the basal plane formed by three O [Ni—O = 1.9290 (16–1.9588 (10 Å] and one N [Ni—N = 1.9828 (18 Å] atoms and the apical position occupied by the water molecule [Ni—O = 2.2643 (11 Å]. The water molecules are involved in the formation of O—H...O hydrogen bonds.
Crystal structure of 2-cyano-N-(furan-2-ylmethyl-3-(3-nitrophenylpropanamide
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Shivanna Subhadramma
2015-08-01
Full Text Available In the title compound, C15H11N3O4, the acetamide group is inclined to the furan ring by 66.5 (1°. The dihedral angle between the furan ring and the benzene ring is 66.8 (1°. In the crystal, molecules are linked by pairs of N—H...N hydrogen bonds, forming inversion dimers with an R22(12 ring motif. The dimers are linked via two pairs of C—H...O hydrogen bonds to the same acceptor oxygen atom, enclosing R21(6 ring motifs, forming chains along the [101] direction.
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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.
Crystal structure of 5,7,12,14-tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-dione
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Mohammad Nozari
2016-12-01
Full Text Available The lattice of 5,7,12,14-tetrahydro-5,14:7,12-bis([1,2]benzenopentacene-6,13-dione, C34H20O2, at 173 K has triclinic (P-1 symmetry and crystallizes with four independent half-molecules in the asymmetric unit. Each molecule is generated from a C17H10O substructure through an inversion center at the centroid of the central quinone ring, generating a wide H-shaped molecule, with a dihedral angle between the mean planes of the terminal benzene rings in each of the two symmetry-related pairs over the four molecules of 68.6 (1 (A, 65.5 (4 (B, 62.3 (9 (C, and 65.8 (8° (D, an average of 65.6 (1°. This compound has applications in gas-separation membranes constructed from polymers of intrinsic microporosity (PIM. The title compound is a product of a double Diels–Alder reaction between anthracene and p-benzoquinone followed by dehydrogenation. It has also been characterized by cyclic voltammetry and rotating disc electrode polarography, FT–IR, high resolution mass spectrometry, elemental analysis, and 1H NMR.
5-Isobutyl-4-phenylsulfonyl-1H-pyrazol-3(2H-one
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M. Venkatesh
2010-12-01
Full Text Available The title compound, C13H16N2O3S, consists of two crystallographically independent molecules with similar geometries and exists in a keto form, the C=O bond lengths being 1.267 (2 and 1.254 (2 Å. In both molecules, the pyrazole rings are approximately planar, with maximum deviations of 0.017 (2 and 0.010 (2 Å, and the dihedral angles between the pyrazole and phenyl rings are 83.63 (11 and 70.07 (12°. In one molecule, an intramolecular C—H...O hydrogen bond with an S(6 ring motif is observed. In the crystal, intermolecular N—H...O and C—H...O hydrogen bonds link the molecules into two-dimensional networks parallel to the ab plane.
N-Cyclohexyl-2-(5-fluoro-1H-indol-3-yl-2-oxoacetamide
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Dan-Li Tian
2011-07-01
Full Text Available In title compound, C16H17FN2O2, the cyclohexane ring adopts a chair conformation.. The crystal packing is stabilized by weak π–π stacking interactions [centroid–centroid distance = 3.503 (5 Å] and intermolecular C—H...O, N—H...O and N—H...F hydrogen-bond interactions.
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Xiulan Zhang
2013-07-01
Full Text Available In the asymmetric unit of the title compound, (C16H38N2O6[Zn(C3S52], two independent cations lie across inversion centers. In one of the cations, the three symmetry-unique O—H groups are disordered over two sets of sites with refined occupancy ratios of 0.701 (9:0.299 (9, 0.671 (8:0.329 (8 and 0.566 (7:0.434 (7. In the anion, the ZnII ion is coordinated in a distorted tetrahedral environment by four S atoms of two chelating 1,3-dithiole-2-thione-4,5-dithiolato ligands. The dihedral angle between the mean planes [maximun deviations = 0.022 (3 and 0.0656 (6 Å] of the two ligands is 87.76 (3°. An intamolecular O—H...O hydrogen bond occurs in the disordered cation. In the crystal, O—H...O and O—H...S hydrogen bonds link the components into a two-dimensional network parallel to (0-11.
(E-N-(3,3-Diphenylallylidene-3-nitroaniline
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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.
N,N′-Bis[3,5-bis(2,6-diisopropylphenylphenyl]butane-2,3-diimine
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Tracy L. Lohr
2011-09-01
Full Text Available The title molecule, C64H80N2, lies on an inversion center wherein the central butanediimine fragment [N=C(Me—C(Me=N] is essentially planar [maximum deviation = 0.002 (2 Å] and its mean plane forms a dihedral of 70.88 (10° with the attached benzene ring. In the symmetry-unique part of the molecule, the dihedral angles between the benzene ring bonded to the N atom and the other two benzene rings are 89.61 (6 and 82.77 (6°.
9-Ethyl-2,3-dihydro-9H-carbazol-4(1H-one
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S. Sriman Narayanan
2008-09-01
Full Text Available In the title compound, C28H30N2O2, the cyclohexene ring system adopts a sofa conformation. The crystal structure is stabilized by C—H...O interactions between methyl H atoms of the ethyl substituents and the O atoms of carbonyl groups of adjacent molecules, and by an intermolecular carbonyl–carbonyl interactions [3.207 (2 Å
2-[2-Benzoyl-3,3-bis(methylsulfanylprop-2-enylidene]malononitrile
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Joseph Nirmala
2009-08-01
Full Text Available The title compound, C15H12N2OS2, is an example of a push–pull butadiene in which the electron-releasing methylsulfanyl groups and electron-withdrawing nitrile groups on either end of the butadiene chain enhance the conjugation in the system. Short intramolecular C—H...S interactions are observed. In the crystal structure, an O...C short contact of 2.917 (3 Å is observed.
4-{(E-[2-(4-Iodobutoxybenzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one
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Hoong-Kun Fun
2010-07-01
Full Text Available The title Schiff base compound, C22H24IN3O2, adopts an E configuration about the central C=N bond. The pyrazolone ring makes a dihedral angle of 49.68 (10° with its attached phenyl ring. The phenolate plane makes dihedral angles of 16.78 (9 and 50.54 (9°, respectively, with the pyrazolone ring and the terminal phenyl ring. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, an intermolecular C—H...O hydrogen bond is also observed.
Bis[2-(2-aminoethyl-1H-benzimidazole-κ2N2,N3](nitrato-κ2O,O′cobalt(II chloride trihydrate
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Jing Zhao
2012-06-01
Full Text Available In the title compound, [Co(NO3(C9H11N32]Cl·3H2O, the CoII atom is coordinated by four N atoms from two chelating 2-(2-aminoethyl-1H-benzimidazole ligands and two O atoms from one nitrate anion in a distorted octahedral coordination environment. In the crystal, N—H...Cl, N—H...O, O—H...Cl and O—H...O hydrogen bonds link the complex cations, chloride anions and solvent water molecules into a three-dimensional network. π–π interactions between the imidazole and benzene rings and between the benzene rings are observed [centroid–centroid distances = 3.903 (3, 3.720 (3, 3.774 (3 and 3.926 (3 Å].
A NEW METHOD FOR PREPARING 6-NITRO-2-(4-BOC-PIPERAZIN-1-YL-3H-QUINAZOLIN-4-ONE
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A. Yu. Kornylov
2017-11-01
Full Text Available The 2-amino-3H-quinazolin-4-one scaffold is found in a large number of molecules with physiological significance and pharmaceutical utility. Previously we synthesized a series of potent antagonists of fibrinogen receptor, derivatives of 2-(piperazin-1-yl-3H-quinazolin-4-one. The key building block for preparing the above series of compounds is 6-amino-2-(4-Boc-piperazin-1-yl-3H-quinazolin-4-one, which was synthesized by hydrogenation of 6-nitro-2-(4-Boc-piperazin-1-yl-3H-quinazolin-4-one. In turn, the nitro derivative was obtained starting from isatoic anhydride in four stages, by a method that can be considered classical, but difficult. The purpose of this work is to simplify the preparation of 6-nitro-2-(4-Boc-piperazin-1-yl-3H-quinazolin-4-one. We proposed an effective method for the synthesis of 6-nitro-2-(4-Boc-piperazin-1-yl-3H-quinazolin-4-one based on a sequential process, C-N cross-coupling and intramolecular amidation. As the arylhalogenide, 2-bromo-5-nitrobenzoic acid methyl ester was used, as the N-nucleophile, 4-Boc-piperazine-1-carboxamidine, a guanidine derivative, was used. In the study, we used two types of catalytic systems, which both gave good results. The application of the third generation of Palladacycleprecatalyst –[(4,5-Bis(diphenylphosphino-9,9-dimethylxanthene-2-(2′-amino-1,1′-biphenyl] palladium(II methanesulfonate, leads to the production of the target product in a high yield, in comparison with the use of the catalytic system: precatalyst – Tris(dibenzylideneacetone dipalladium(0 chloroform adduct and Buchwald Ligands – 4,5-Bis(diphenylphosphino-9,9-dimethylxanthene. The structure of the title compound was confirmed by spectroscopy 1H and 13C NMR, and FAB mass spectrometry methods, purity was controlled by HPLC. This method has potential implications for the design of various 2-amino-3H-quinazolin-4-ones.
Kuchár, Juraj; Cernák, Juraj
2009-07-01
The title compound, catena-poly[[bis[(triazacyclononane-kappa(3)N,N',N'')copper(II)]-di-mu-cyanido-kappa(4)N:C-palladate(II)-di-mu-cyanido-kappa(4)C:N] dibromide bis[[(triazacyclononane-kappa(3)N,N',N'')copper(II)]-mu-cyanido-kappa(2)N:C-[dicyanidopalladate(II)]-mu-cyanido-kappa(2)C:N] monohydrate], {[Cu(2)Pd(CN)(4)(C(6)H(15)N(3))(2)]Br(2).[Cu(2)Pd(2)(CN)(8)(C(6)H(15)N(3))(2)].H(2)O}(n), (I), was isolated from an aqueous solution containing tacn.3HBr (tacn is 1,4,7-triazacyclononane), Cu(2+) and tetracyanidopalladate(2-) anions. The crystal structure of (I) is essentially ionic and built up of 2,2-electroneutral chains, viz. [Cu(tacn)(NC)-Pd(CN)(2)-(CN)-], positively charged 2,4-ribbons exhibiting the composition {[Cu(tacn)(NC)(2)-Pd(CN)(2)-Cu(tacn)](2n+)}(n), bromide anions and one disordered water molecule of crystallization. The O atom of the water molecule occupies two unique crystallographic positions, one on a centre of symmetry, which is half occupied, and the other in a general position with one-quarter occupancy. One of the tacn ligands also exhibits disorder. The formation of two different types of one-dimensional structural motif within the same structure is a unique feature of this compound.
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Thomas Brietzke
2014-06-01
Full Text Available In the title compound, rac-[Ru(C14H16N22(C16H8N4](PF62·3C2H3N, discrete dimers of complex cations, [Ru(tmbpy2tape]2+, of opposite chirality are formed (tmbpy = tetramethylbipyridine; tape = tetraazaperylene, held together by π–π stacking interactions between the tetraazaperylene moieties with centroid–centroid distances in the range 3.563 (3–3.837 (3 Å. These interactions exhibit a parallel displaced π–π stacking mode. Additional weak C—H...π-ring and C—H...N and C—H...F interactions are found, leading to a three-dimensional architecture. The RuII atom is coordinated in a distorted octahedral geometry. The counter-charge is provided by two hexafluoridophosphate anions and the asymmetric unit is completed by three acetonitrile solvent molecules of crystallization. Four F atoms of one PF6− anion are disordered over three sets of sites with occupancies of 0.517 (3:0.244 (3:0.239 (3. Two acetonitrile solvent molecules are highly disordered and their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155].
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Khaled Boukebbous
2016-10-01
Full Text Available The almost planar (r.m.s. deviation = 0.034 Å title compound, C7H4S3, was synthesized by reacting 2,2-dithiodibenzoic acid with phosphorus pentasulfide in xylene solution. In the crystal, short S...S [3.3727 (14, 3.3765 (13 and 3.4284 (13 Å] contacts and aromatic π–π stacking [shortest centroid–centroid separation = 3.618 (2 Å] are observed.
International Nuclear Information System (INIS)
Subbiah, Ayyappan; Bhuvanesh, Nattamai; Clearfield, Abraham
2005-01-01
A novel tin(II) phenylbis(phosphonate) compound has been synthesized hydrothermally and its structure has been determined by single crystal X-ray diffraction. The structure is monoclinic, space group P2 1 /c (no. 14), a=4.8094(4), b=16.2871(13), c=6.9107(6)A; β=106.292(6) o , V=519.59(7)A 3 , Z=2. The three-dimensional structure consists of 3-coordinated tin and 4-coordinated phosphorus double layers separated (pillared) by phenyl rings. These phenyl rings are placed 4.8A apart along the a-axis in the structure resulting in lower surface area (∼14m 2 /g). The porosity has been increased by replacing phenyl groups by methyl groups (∼31m 2 /g)
3-Chloro-N-(4-sulfamoylphenylpropanamide
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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.
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Zihua Wang
2009-06-01
Full Text Available In the title molecule, C24H28N6O2S2, the dihedral angle between the aromatic ring planes is 42.2 (1°. In the crystal structure, the hydroxy groups are involved in O—H...S hydrogen bonding, which links the molecules into corrugated layers propagating parallel to the bc plane.
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)
N-(4-Chlorophenyl-4-nitrobenzamide
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Ghulam Waris
2012-09-01
Full Text Available The title compound, C13H9ClN2O3, is almost planar, showing a dihedral angle of 4.63 (6° between the aromatic ring planes. The nitro group also lies in the plane, the C—C—N—O torsion angle being 6.7 (2°. There is an intamolecular C—H...O hydrogen bond. The crystal structure features N—H...O(nitro hydrogen bonds that link the molecules into zigzag chains extending along [010].
9-Ethyl-3,6-diformyl-9H-carbazole
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Jun Jie Wang
2008-07-01
Full Text Available The structure of the title compound, C16H13NO2, was determined as a part of a project on the synthesis of new compounds which can make two-photon absorptions. In the crystal structure, both aldehyde groups are located within the carbazole plane. One of these groups is disordered and was refined using a split model with site-occupation factors for each position of 0.5.
5-Imino-3,4-diphenyl-1H-pyrrol-2-one
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Evgeny Bulatov
2014-02-01
Full Text Available The title compound, C16H12N2O, exists in the crystalline state as the 5-imino-3,4-diphenyl-1H-pyrrol-2-one tautomer. The dihedral angles between the pyrrole and phenyl rings are 35.3 (2 and 55.3 (2°. In the crystal, inversion dimers linked by pairs of N—H...N hydrogen bonds generate a graph-set motif of R22(8 via N—H...N hydrogen bonds.
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Esen Nur Kantar
2013-06-01
Full Text Available The title Schiff base, C23H27ClN2O adopts the phenol–imine tautomeric form, with an intramolecular O—H...N hydrogen bond, which generates an S(6 ring motif. Three C atoms of the heterocyclic moiety of the hexahydropyridoquinoline unit, as well as the two methyl groups bonded to one of these C atoms, are disordered over two set of sites, with anoccupancy ratio of 0.740 (4:0.260 (4.
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Barbara Dmochowska
2013-07-01
Full Text Available The structure of the title compound, [C12H24NO4][C7H7O3S]·1.5H2O, contains alternating layers parallel to (001 of hydrophobic and polar character, stabilized by C—H...O hydrogen bonding. The furan ring adopts an envelope conformation with the C(OMe atom as the flap, and the dioxolane ring is twisted about one of the O—C(methine bonds. A comparison to related compounds is presented. The tosylate-O atoms were disordered over two positions with the major component having a site occupancy factor = 0.566 (12. The structure was refined as a rotary twin with regard to rotation about the c axis with the contribution of the second component being 0.0048 (6. Solvate water molecules are highly disordered and were removed using the SQUEEZE procedure; the unit cell characteristics take into account the presence of the disordered solvent. High-resolution 1H and 13C NMR spectroscopic data are also presented.
Zheoat, Ahmed M.; Gray, Alexander I.; Igoli, John O.; Kennedy, Alan R.; Ferro, Valerie A.
2017-01-01
The biologically active title compounds have been isolated from Hibiscus sabdariffa plants, hibiscus acid as a dimethyl sulfoxide monosolvate [systematic name: (2S,3R)-3-hy?droxy-5-oxo-2,3,4,5-tetra?hydro?furan-2,3-di?carb?oxy?lic acid dimethyl sulfoxide monosolvate], C6H6O7?C2H6OS, (I), and hibiscus acid dimethyl ester [systematic name: dimethyl (2S,3R)-3-hy?droxy-5-oxo-2,3,4,5-tetra?hydro?furan-2,3-di?carboxyl?ate], C8H10O7, (II). Compound (I) forms a layered structure with alternating laye...
Investigation of ZnI2-KI-C3H7NO system by ultrasonic method
International Nuclear Information System (INIS)
Shevchenko, V.M.; Surovtsev, V.I.; Gorenbejn, E.Ya.
1975-01-01
Applicability of the ultrasonic impulses for the research of complex formation in the solutions was demonstrated using ZnI 2 -KI-C 3 H 7 NO system as an example. Changing the solvent structure during complexing was studied. It was determined that ion solvation numbers reflect electrostriction influence of ions on the surrounding solvent moleculas. The maximum effect on dimethylformamide (C 3 H 7 NO) was made by the complex compound KZnI 3 acting as destrictor and the sound speed decrease was the highest in its solution. Possibility of using adiabatic compressibility of the solutions for complexing studies is analysed
Synthesis, crystal structure, and properties of the ordered double perovskite Sr_2CoOsO_6
International Nuclear Information System (INIS)
Kumar Paul, Avijit; Reehuis, Manfred; Felser, Claudia; Abdala, Paula M.; Jansen, Martin
2013-01-01
Sr_2CoOsO_6, a new osmium based ordered semiconductor double perovskite was prepared by solid state synthesis from the respective binary oxides. Room temperature PXRD analysis shows the compound to be tetragonal [I4/m; a = 5.5503(1) Aa and c = 7.9320(1) Aa], whereas low temperature synchrotron data refinement has revealed a second monoclinic polymorph [I2/m; a = 5.4969(2) Aa, b = 5.4979(2) Aa, c = 8.0090(1) Aa and γ = 90.527(1) ] with a fully ordered rocksalt arrangement of cobalt and osmium atoms over the perovskite B-sites. Heat capacity and magnetic measurements indicate that Sr_2CoOsO_6 shows antiferromagnetic ordering below T_N = 108 K followed by a second magnetic transition at T_2 = 65 K. It was shown that the change from the tetragonal to the monoclinic phase occurs at T_N. (Copyright copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)
Subasri, S; Kumar, Timiri Ajay; Sinha, Barij Nayan; Jayaprakash, Venkatesan; Viswanathan, Vijayan; Velmurugan, Devadasan
2017-02-01
The title compounds, C 16 H 15 N 5 OS, (I), and C 12 H 12 FN 5 OS, (II), are [(di-amino-pyrimidine)-sulfan-yl]acetamide derivatives. In (I), the pyrimidine ring is inclined to the naphthalene ring system by 55.5 (1)°, while in (II), the pyrimidine ring is inclined to the benzene ring by 58.93 (8)°. In (II), there is an intra-molecular N-H⋯N hydrogen bond and a short C-H⋯O contact. In the crystals of (I) and (II), mol-ecules are linked by pairs of N-H⋯N hydrogen bonds, forming inversion dimers with R 2 2 (8) ring motifs. In the crystal of (I), the dimers are linked by bifurcated N-H⋯(O,O) and C-H⋯O hydrogen bonds, forming layers parallel to (100). In the crystal of (II), the dimers are linked by N-H⋯O hydrogen bonds, also forming layers parallel to (100). The layers are linked by C-H⋯F hydrogen bonds, forming a three-dimensional architecture.
3,5-Dimethyl-4-nitroso-1H-pyrazole
Safyanova, Inna; Dudarenko, Nikolay M.; Pavlenko, Vadim A.; Iskenderov, Turganbay S.; Haukka, Matti
2011-01-01
In the unit cell of the title compound, C5H7N3O, there are two conformers (A and B) which differ in the position of the oxime group with respect to the protonated pyrazole nitrogen (trans in the A conformer and cis in the B conformer) and in the geometric parameters. The oxime group exists in the nitroso form in both conformers. In the crystal, molecules are linked by intermolecular N—H⋯O and N—H⋯N hydrogen bonds into zigzag-like chains along the b axis. PMID:22059058
International Nuclear Information System (INIS)
Chernorukov, N.G.; Sulejmanov, E.V.; Barch, S.V.
2001-01-01
The technique of synthesis of hydroxyuranophosphate and hydroxyuranoarsenate of aluminium is developed. Hydroxyuranophosphates and hydroxyuranoarsenates of aluminium are prepared by reaction of interaction of aqueous solutions of orthophosphoric (orthoarsenic) acid (0.05 mol/l), uranyl nitrate (0.05 mol/l) and aluminium nitrate (0.1 mol/l) at 20 Deg C. Peculiarities of the structure and thermal degradation reactions are studied by the methods of x-ray diffraction, IR spectroscopy, thermography. It is shown that in dependence on outer conditions in the systems Al[PUO 6 ] 2 ·[OH]·nH 2 O and Al[AsUO 6 ] 2 ·[OH]·nH 2 O crystal hydrates with hydrate numbers n=3-11(13) and anhydrous compounds form. The compounds have laminated type of lattice. Two-dimensional layers of [P(As)UO 6 ] ∞ n- are the basis of anion sublattice of these compounds. Aluminium in coordination surrounding of hydroxy groups and water molecules forms cationic sublattice [ru
1,5,6-Triphenyl-8-oxa-7-selena-6-phosphabicyclo[3.2.1]octane-6-selone
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Yang Li
2008-01-01
Full Text Available The structure of the title compound, C23H21OPSe2, consists of fused puckered five- and six-membered rings, PSeC2O and C5O, respectively, with a C2O bridgehead. The C5O ring adopts a chair conformation, whilst the C2PSeO ring has an envelope conformation.
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Delgado Torralbo Elena
2000-01-01
Full Text Available FUNDAMENTO: En 1997 el 18,5% de los casos de Enfermedad Meningocócica por serogrupo C en Andalucía fueron niños de 2 a 4 años de edad; edades donde respuesta inmune inicial y duración de la vacuna antimeningocócica de polisacárido capsular A+C, es menor que en edades superiores. Se diseñó una investigación para medir la respuesta inmune producida por esta vacuna, en niños de 2 a 6 años de edad, y compararla con la inmunidad natural presente en niños no vacunados. MÉTODOS: I.- Doble estudio de seguimiento: a grupos de niños previamente vacunados y grupos control, b grupo de niños que iba a ser vacunado, para análisis pre y postvacunal (1, 6 y 12 meses y grupo control. II.- La actividad bactericida se midió según protocolo estandarizado del CDC frente a cepa de N. meningítidis C-11. Los sueros con título de actividad bactericida (TAB > o = 1:8 se consideraron protectores. RESULTADOS: Al mes y a los 2 meses de vacunarse la proporción de TAB > o = 1:8 era significativamente superior a la del grupo control (65,5% y 73,9% frente a 2,2% y 12%. En el prevacunal y en el postvacunal a los 6, 7, 12 y 13 meses no se observó diferencia significativa entre vacunados y controles. CONCLUSIONES: Las diferencias entre vacunados y no vacunados 1 y 2 meses después de la vacunación indican seroconversión en los vacunados. Para el grupo de edad de 2 a 6 años la actividad bactericida adquirida declina rápidamente, ya que a los 6 meses dejan de observarse diferencias con el grupo control.
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Elena Delgado Torralbo
2000-01-01
Full Text Available FUNDAMENTO: En 1997 el 18,5% de los casos de Enfermedad Meningocócica por serogrupo C en Andalucía fueron niños de 2 a 4 años de edad; edades donde respuesta inmune inicial y duración de la vacuna antimeningocócica de polisacárido capsular A+C, es menor que en edades superiores. Se diseñó una investigación para medir la respuesta inmune producida por esta vacuna, en niños de 2 a 6 años de edad, y compararla con la inmunidad natural presente en niños no vacunados. MÉTODOS: I.- Doble estudio de seguimiento: a grupos de niños previamente vacunados y grupos control, b grupo de niños que iba a ser vacunado, para análisis pre y postvacunal (1, 6 y 12 meses y grupo control. II.- La actividad bactericida se midió según protocolo estandarizado del CDC frente a cepa de N. meningítidis C-11. Los sueros con título de actividad bactericida (TAB ³ 1:8 se consideraron protectores. RESULTADOS: Al mes y a los 2 meses de vacunarse la proporción de TAB³ 1:8 era significativamente superior a la del grupo control (65,5% y 73,9% frente a 2,2% y 12%. En el prevacunal y en el postvacunal a los 6, 7, 12 y 13 meses no se observó diferencia significativa entre vacunados y controles. CONCLUSIONES: Las diferencias entre vacunados y no vacunados 1 y 2 meses después de la vacunación indican seroconversión en los vacunados. Para el grupo de edad de 2 a 6 años la actividad bactericida adquirida declina rápidamente, ya que a los 6 meses dejan de observarse diferencias con el grupo control.
Vishwakarma, Ashok K.; Kumari, Reema; Ghalsasi, Prasanna S.; Arulsamy, Navamoney
2017-08-01
The synthesis, thermal analysis, crystal structure and magnetic properties of (2-aminobenzothiazolium)2CuCl4, organic-inorganic hybrid compound, have been described. The compound crystallizes in the monoclinic space group P21/c with two formula units in a unit cell of dimensions a = 6.9522(4) Å, b = 9.6979(4) Å, c = 13.9633(6) Å, β = 97.849(3)° and volume 930.83(8) Å3 at 150(2) K. The structure consists of isolated nearly square planer [CuC14]2- units, with somewhat longer than normal Cusbnd Cl bond lengths [Cusbnd Cl (average) = 2.2711 Å]. The magnetic measurements of (2-aminobenzothiazolium)2CuCl4 using SQUID magnetometer show paramagnetic nature of the compound. Thermal measurements (TG-DTA and DSC) on this compound showed reversible phase transition at 83 °C. This transition is accompanied by the reversible change in colour of the prismatic crystal from green to dark brown, thermochromic behaviour. Temperature dependent EPR measurements on powdered sample ascertain change in coordination sphere around Cu(II) with shift in g|| = 2.150 and g⊥ = 2.071 at room temperature, typical of square planar, to g|| = 2.201 and g⊥ = 2.182 at 170 °C, typical of distorted tetrahedral geometry.
Photodissociation of C3H5Br and C4H7Br at 234 nm
International Nuclear Information System (INIS)
Kim, Hyun Kook; Paul, Dababrata; Hong, Ki Ryong; Cho, Ha Na; Kim, Tae Kyu; Lee, Kyoung Seok
2012-01-01
The photodissociation dynamics of cyclopropyl bromide (C-3H 5 Br) and cyclobutyl bromide (C 4 H 7 Br) at 234 nm was investigated. A two-dimensional photofragment ion-imaging technique coupled with a [2+1] resonance enhanced multiphoton ionization scheme was utilized to obtain speed and angular distributions of the nascent Br( 2 P 3/2 ) and Br*( 2 P 1/2 ) atoms. The recoil anisotropies for the Br and Br* channels were measured to be βBr = 0.92 ± 0.03 and βBr* = 1.52 ± 0.04 for C 3 H 5 Br and βBr = 1.10 ± 0.03 and βBr* = 1.49 ± 0.05 for C 4 H 7 Br. The relative quantum yield for Br was found to be ΦBr = 0.13 ± 0.03 and for C 3 H 5 Br and C 4 H 7 Br, respectively. The soft radical limit of the impulsive model adequately modeled the related energy partitioning. The nonadiabatic transition probability from the 3A' and 4A' potential energy surfaces was estimated and discussed
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Igor O. Fritsky
2008-02-01
Full Text Available The title compound, {[Co2(C15H14N4O32(C5H5N4(H2O2]ClO4·3.66H2O}n, is a one-dimensional coordination polymer, with both CoII and CoIII centres in its structure. The ligand environment surrounding CoIII is formed by two N,N-chelating pyrazole-containing ligands and two pyridine molecules in axial positions. The high-spin CoII ions, situated at crystallographic centres of inversion, exhibit a distorted octahedral coordination mode. The ClO4− anion is linked to the polymer chain via hydrogen bonds. The chains are connected by hydrogen bonds to produce a three-dimensional structure.
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.
Bruce, Michael I; Costuas, Karine; Davin, Thomas; Halet, Jean-François; Kramarczuk, Kathy A; Low, Paul J; Nicholson, Brian K; Perkins, Gary J; Roberts, Rachel L; Skelton, Brian W; Smith, Mark E; White, Allan H
2007-12-14
The sequential conversion of [OsBr(cod)Cp*] (9) to [OsBr(dppe)Cp*] (10), [Os([=C=CH2)(dppe)Cp*]PF6 ([11]PF6), [Os(C triple bond CH)(dppe)Cp*] (12), [{Os(dppe)Cp*}2{mu-(=C=CH-CH=C=)}][PF6]2 ([13](PF6)2) and finally [{Os(dppe)Cp*}(2)(mu-C triple bond CC triple bond C)] (14) has been used to make the third member of the triad [{M(dppe)Cp*}2(mu-C triple bond CC triple bond C)] (M = Fe, Ru, Os). The molecular structures of []PF6, 12 and 14, together with those of the related osmium complexes [Os(NCMe)(dppe)Cp*]PF6 ([15]PF6) and [Os(C triple bond CPh)(dppe)Cp*] (16), have been determined by single-crystal X-ray diffraction studies. Comparison of the redox properties of 14 with those of its iron and ruthenium congeners shows that the first oxidation potential E1 varies as: Fe approximately Os < Ru. Whereas the Fe complex has been shown to undergo three sequential 1-electron oxidation processes within conventional electrochemical solvent windows, the Ru and Os compounds undergo no fewer than four sequential oxidation events giving rise to a five-membered series of redox related complexes [{M(dppe)Cp*}2(mu-C4)]n+ (n = 0, 1, 2, 3 and 4), the osmium derivatives being obtained at considerably lower potentials than the ruthenium analogues. These results are complimented by DFT and DT DFT calculations.
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K. Gurunathan
2009-05-01
Full Text Available In the title compound, C18H20N2O3, the N-methylpiperidone ring adopts a chair conformation. The pyrrolidine ring and the five-membered cyclopentane rings adopt envelope conformations. The five-membered ring of the ninhydrin system adopts an envelope conformation with the central C atom deviating by 0.217 (1Å from the mean plane through the other atoms. The molecular packing is characterized by intermolecular C—H...O and intramolecular C—H...O and O—H...N interactions.
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Ming-Ming Yu
2009-02-01
Full Text Available In the cation of the title compound, [Mn(C18H18N2O4(H2O2]ClO4·0.5C12H24O6·H2O, the MnIII ion is coordinated by two water O atoms, and two O atoms and two N atoms from the tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolate ligand, completing a distorted octahedral geometry. One O atom of the 18-crown-6-ether is disordered over two positions with occupancies of 0.70 (2 and 0.30 (2.
Ethyl 2-(3,4-dimethyl-5,5-dioxo-1H,4H-benzo[e]pyrazolo[4,3-c][1,2]thiazin-1-ylacetate
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Sana Aslam
2012-10-01
Full Text Available In the title molecule, C15H17N3O4S, the heterocyclic thiazine ring adopts a twist-boat conformation, which differs from that in related compounds, with adjacent S and C atoms displaced by 0.981 (4 and 0.413 (5 Å, respectively, on the same side of the mean plane formed by the remaining ring atoms. The mean plane of the benzene ring makes a dihedral angle of 23.43 (14° with the mean plane of the pyrazole ring. In the crystal, molecules are connected by weak C—H...O hydrogen bonds to form a three-dimensional network. The H atoms of the methyl group attached to the pyrazole ring were refined over six sites with equal occupancies.
Semenov, K. N.; Ivanova, N. M.; Charykov, N. A.; Keskinov, V. A.; Kalacheva, S. S.; Duryagina, N. N.; Garamova, P. V.; Kulenova, N. A.; Nabieva, A.
2017-02-01
Concentration dependences of the density of aqueous solutions of bisadducts of light fullerene C60 and essential amino acids are studied by pycnometry. Concentration dependences of the average molar volumes and partial volumes of components (H2O and corresponding bisadducts) are calculated for C60(C6H13N2O2)2-H2O, C60(C4H8NO3)2-H2O, and C60(C5H9NO2)2-H2O binary systems at 25°C. Concentration dependences of the indices of refraction of C60(C6H13N2O2)2-H2O, C60(C4H8NO3)2-H2O, and C60(C5H9NO2)2-H2O binary systems are determined at 25°C. The concentration dependences of specific refraction and molar refraction of bisadducts and aqueous solutions of them are calculated.
Crystal structure of 4-(4b,8a-dihydro-9H-pyrido[3,4-b]indol-1-yl-7-methyl-2H-chromen-2-one
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S. Samundeeswari
2017-01-01
Full Text Available The title compound, C21H14N2O2, was prepared by Pictet–Spengler cyclization of tryptamine and 4-formyl coumarin. In the molecule, the dihedral angle between the mean planes of the coumarin and β-carboline ring systems is 63.8 (2°. In the crystal, molecules are linked via N—H...N hydrogen bonds, forming chains along the b-axis direction. Within the chains, there are a number of offset π–π interactions present [shortest intercentroid distance = 3.457 (2 Å].
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Nitin Kumar
2017-05-01
Full Text Available A novel series of 3-(4, 5-dihydro-1-phenyl-5-substituted phenyl-1H-pyrazol-3-yl-2H-chromen-2-one derivatives were synthesized. In the first step salicylaldehyde was reacted with ethylacetoacetate at room temperature by stirring which gives compound (I. Compound (I when refluxed with substituted benzaldehyde and diethylamine in the presence of n-butanol for 4–5 h gives substituted derivatives (IIa–d. Compounds synthesized in step 2 when refluxed with phenyl hydrazine in the presence of pyridine for 6–7 h gives the title compounds (IIIa–d. All the synthesized compounds were sent to NCI for anticancer activity. Synthesized compounds were tested for anticancer activity against 60 different cell lines. From the data thus obtained it was observed that simple coumarin ring derivatives were more effective in inhibiting the growth of cancerous cell lines, than coumarin-pyrazoline derivatives. Among all the synthesized compounds, irrespective of compounds having simple coumarin ring and coumarin-pyrazoline combination, compounds IIa–c, IIIb and IIId were potent anticancer agents. Compounds were active for the single dose therapeutic program at the dose of 1.00E-5 molar concentration. The main anti cancer activity is assumed to be due to the presence of the lactone structure in coumarin moiety.
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Siwar Ghannay
2016-08-01
Full Text Available In the title compound, C24H32BrN3O2, the six-membered cyclohexane ring adopts a chair conformation and the isoxasolidine ring adopts a twisted conformation. The molecule has five chiral centres and the absolute configuration has been determined in this analysis. The molecular structure is stabilized by weak intramolecular C—H...O and C—H...N contacts. In the crystal, molecules are linked by N—H...N and C—H...O hydrogen bonds, forming undulating sheets parallel to the bc plane.
(Acetylacetonato-κ2O,O′bis[5-methoxy-2-(naphth[1,2-d][1,3]oxazol-2-ylphenyl-κ2C1,N]iridium(III
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Yuan-Yuan Zhou
2011-10-01
Full Text Available In the title compound, [Ir(C18H12NO22(C5H7O2], the Ir atom is O,O′-chelated by the acetylacetonate group and C,N-chelated by the 2-arylnaphth[1,2-d]oxazole groups. The six-coordinate metal atom displays a distorted octahedral geometry. Intramolecular C—H...O hydrogen bonds occur. In the crystal, intermolecular C—H...O hydrogen bonds link the molecules into columns parallel to the b axis.
(Benzyl isocyanide-κC1chlorido(2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl-κ2C1,Npalladium(II
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Ana C. Mafud
2013-01-01
Full Text Available In the title compound, [Pd(C11H13ClNCl(C8H7N], which crystallized in the chiral space group P212121, the PdII atom is coordinated by two C atoms, a Csp2 atom of the 2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl ligand and a Csp atom from the benzyl isocyanide ligand, as well as an N atom of the ligand and a Cl atom, in a square-planar geometry. In the complex, there is a short C—H...Cl hydrogen bond and a C—H...π interaction. In the crystal, molecules are linked via C—H...Cl hydrogen bonds, forming chains along the a-axis direction.
2,2,6-Trimethyl-5-[2-(4-methylphenylethynyl]-4H-1,3-dioxin-4-one
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Ignez Caracelli
2009-11-01
Full Text Available The 1,3-dioxin-4-one ring in the title compound, C16H16O3, is in a half-boat conformation with the quaternary O—C(CH32—O atom lying 0.546 (1 Å out of the plane defined by the remaining five atoms. The crystal structure is consolidated by C—H...O contacts that lead to supramolecular layers.
Kuruvilla, Tintu K.; Prasana, Johanan Christian; Muthu, S.; George, Jacob
2018-04-01
The spectroscopic properties of 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine were investigated in the present study using FT-IR and FT-Raman techniques. The results obtained were compared with quantum mechanical methods, as it serves as an important tool in interpreting and predicting vibrational spectra. The optimized molecular geometry, the vibrational wavenumbers, the infrared intensities and Raman scattering were calculated using density functional theory B3LYP method with 6-311++g (d,p) basis set. All the experimental results were in line with the theoretical data. The molecular electrostatic potential (MEP) and HOMO LUMO energies of the title compound were accounted. The results indicated that the title compound has a lower softness value (0.27) and high electrophilicity index (4.98) hence describing its biological activity. Further, natural bond orbital was also analyzed as part of the work. Fukui functions were calculated in order to explain the chemical selectivity or the reactivity site in 4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno [3,2-f] [1,2,4] triazolo [4,3-a] [1,4] diazepine. The thermodynamic properties of the title compound were closely examined at different temperatures. It revealed the correlations between heat capacity (C), entropy (S) and enthalpy changes (H) with temperatures. The paper further explains that the title compound can act as good antidepressant through molecular docking studies.
Arslan, Hakan; Algül, Öztekin; Önkol, Tijen
2008-08-01
The molecular structure, vibrational frequencies and infrared intensities of the 3-(6-benzoyl-2-oxobenzo[ d]oxazol-3(2 H)-yl)propanoic acid were calculated by the HF and DFT methods using 6-31G(d) basis set. The FT-infrared spectra have been measured for the title compound in the solid state. We obtained 11 stable conformers for the title compound, however the Conformer 1 is approximately 3.88 kcal/mol more stable than the Conformer 11. The comparison of the theoretical and experimental geometry of the title compound shows that the X-ray parameters fairly well reproduce the geometry of the Conformer 1. The harmonic vibrations computed of this compound by the B3LYP/6-31G(d) method are in a good agreement with the observed IR spectral data. Theoretical vibrational spectra of the title compound were interpreted by means of PEDs using VEDA 4 program.
Diodes of nanocrystalline SiC on n-/n+-type epitaxial crystalline 6H-SiC
Zheng, Junding; Wei, Wensheng; Zhang, Chunxi; He, Mingchang; Li, Chang
2018-03-01
The diodes of nanocrystalline SiC on epitaxial crystalline (n-/n+)6H-SiC wafers were investigated, where the (n+)6H-SiC layer was treated as cathode. For the first unit, a heavily boron doped SiC film as anode was directly deposited by plasma enhanced chemical vapor deposition method on the wafer. As to the second one, an intrinsic SiC film was fabricated to insert between the wafer and the SiC anode. The third one included the SiC anode, an intrinsic SiC layer and a lightly phosphorus doped SiC film besides the wafer. Nanocrystallization in the yielded films was illustrated by means of X-ray diffraction, transmission electronic microscope and Raman spectrum respectively. Current vs. voltage traces of the obtained devices were checked to show as rectifying behaviors of semiconductor diodes, the conduction mechanisms were studied. Reverse recovery current waveforms were detected to analyze the recovery performance. The nanocrystalline SiC films in base region of the fabricated diodes are demonstrated as local regions for lifetime control of minority carriers to improve the reverse recovery properties.
Densities, viscosities, and refractive indexes for {C2H5CO2(CH2)2CH3+C6H13OH+C6H6} at T=308.15 K
International Nuclear Information System (INIS)
Casas, Herminio; Garcia-Garabal, Sandra; Segade, Luisa; Cabeza, Oscar.; Franjo, Carlos; Jimenez, Eulogio
2003-01-01
In this work we present densities, kinematic viscosities, and refractive indexes of the ternary system {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 13 OH+C 6 H 6 } and the corresponding binary mixtures {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 6 }, {C 2 H 5 CO 2 (CH 2 ) 2 CH 3 +C 6 H 13 OH}, and {C 6 H 13 OH+C 6 H 6 }. All data have been measured at T=308.15 K and atmospheric pressure over the whole composition range. The excess molar volumes, dynamic viscosity deviations, and changes of the refractive index on mixing were calculated from experimental measurements. The results for binary mixtures were fitted to a polynomial relationship to estimate the coefficients and standard deviations. The Cibulka equation has been used to correlate the experimental values of ternary mixtures. Also, the experimental values obtained for the ternary mixture were used to test the empirical methods of Kohler, Jacob and Fitzner, Colinet, Tsao and Smith, Toop, Scatchard et al., and Hillert. These methods predict excess properties of the ternary mixtures from those of the involved binary mixtures. The results obtained for dynamic viscosities of the binary mixtures were used to test the semi-empirical relations of Grunberg-Nissan, McAllister, Auslaender, and Teja-Rice. Finally, the experimental refractive indexes were compared with the predicted results for the Lorentz-Lorenz, Gladstone-Dale, Wiener, Heller, and Arago-Biot equations. In all cases, we give the standard deviation between the experimental data and that calculated with the above named relations
1-Benzyl-3-(2-furylmethyl-1,2,3,4,5,6-hexahydrospiro[benzo[h]quinazoline-5,1′-cyclohexane]-2,4-dione
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Siranush Gabrielyan
2008-04-01
Full Text Available The title compound, C29H28N2O3, displays antidepressant and anticancer activities. The furan ring is disordered over two orientations [site occupancies 0.690 (12/0.310 (12] related by a rotation of 180°. The ring conformations are chair for the cyclohexane ring, boat for the cyclohexadiene ring and twist for the pyrimidine ring. The crystal packing is determined solely by van der Waals interactions.