catena-Poly[[dichloridocobalt(II]-μ-1,3-di-4-pyridylpropane-κ2N:N′

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Wei Xu

2008-08-01

Full Text Available In the title compound, [CoCl2(C13H14N2]n, 1,3-bis(4-pyridylpropane (bpp ligands bridge four-coordinate Co atoms, generating an extended one-dimensional zigzag chain. Both the Co and two Cl atoms in the tetrahedral coordination polyhedron lie on a mirror plane, while the bbp ligand is bisected through the central C atom in the chain by a second mirror plane. There are some π–π stacking interations in the crystal structure, with interplanar distances of 3.449 Å, which are responsible for the supramolecular assembly.

Poly[dibromidobis[μ-1-(pyridin-4-ylmethyl-1H-1,2,4-triazole-κ2N:N′]cadmium

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Xiu-Zhi Xu

2011-02-01

Full Text Available The title coordination polymer, [CdBr2(C8H8N42]n, arose from a layer-separated diffusion synthesis at room temperature. The title compound is isotypic with the I and Cl analogues. The Cd atom, located on an inversion center, is coordinated by two bromide ions and four N atoms (two from triazole rings and two from pyridyl rings in a distorted trans-CdBr2N4 octahedral arrangement. The bridging 1-(4-pyridylmethyl-1H-1,2,4-triazole ligands are twisted [dihedral angle between the triazole and pyridine rings = 72.56 (13°], affording a two-dimensional 44 sheet structure in the crystal.

A convenient method for 14C-labeling of 2-methylthio-1-[4-N-α-ethoxycarbonylbenzyl)-amino-benzyl] -5-hydroxymethyl-2-[14C]-1H-imidazole and 1-[4-N-α-ethoxy-carbonylbenzyl)-aminobenzyl]-5-hydroxymethyl-2-[14C] -1H-imidazole as potential antihypertensives

International Nuclear Information System (INIS)

Nader Saemian; Gholamhossein Shirvani; Mohsen Javaheri; Sayed Sajad Oliyaee

2012-01-01

The key synthetic intermediate, (2-mercapto-1-(4-nitrobenzyl)-1H-imidazol-5-yl)methanol-[2- 14 C], has been synthesized by using one pot procedure from potassium[ 14 C]-thiocyanate. It was converted to two nonpeptide angiotensin II receptor antagonists, 2-methylthio-1-[4-N-α-ethoxycarbonyl benzyl)-aminobenzyl]-5-hydroxymethyl-1H-imidazole-[2- 14 C] and 1-[4-N-α-ethoxy-carbonylbenzyl)-aminobenzyl] -5-hydroxymethyl-1H-imidazole-[2- 14 C] via a 3-step sequence synthetic pathway. (author)

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

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Vladimir P. Zaytsev

2014-12-01

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

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

Science.gov (United States)

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

2011-01-08

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

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

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Fortune Ezemobi

2014-12-01

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

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

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Assem Barakat

2016-09-01

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

A new Schiff base compound N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone): synthesis, experimental and theoretical studies on its crystal structure, FTIR, UV-visible, 1H NMR and 13C NMR spectra.

Science.gov (United States)

Saheb, Vahid; Sheikhshoaie, Iran

2011-10-15

The Schiff base compound, N,N'-(2,2-dimetylpropane)-bis(dihydroxylacetophenone) (NDHA) is synthesized through the condensation of 2-hydroxylacetophenone and 2,2-dimethyl 1,3-amino propane in methanol at ambient temperature. The yellow crystalline precipitate is used for X-ray single-crystal determination and measuring Fourier transform infrared (FTIR), UV-visible, (1)H NMR and (13)C NMR spectra. Electronic structure calculations at the B3LYP, PBEPBE and PW91PW91 levels of theory are performed to optimize the molecular geometry and to calculate the FTIR, (1)H NMR and (13)C NMR spectra of the compound. Time-dependent density functional theory (TDDFT) method is used to calculate the UV-visible spectrum of NDHA. Vibrational frequencies are determined experimentally and compared with those obtained theoretically. Vibrational assignments and analysis of the fundamental modes of the compound are also performed. All theoretical methods can well reproduce the structure of the compound. The (1)H NMR and (13)C NMR chemical shifts calculated by all DFT methods are consistent with the experimental data. However, the NMR shielding tensors computed at the B3LYP/6-31+G(d,p) level of theory are in better agreement with experimental (1)H NMR and (13)C NMR spectra. The electronic absorption spectrum calculated at the B3LYP/6-31+G(d,p) level by using TD-DFT method is in accordance with the observed UV-visible spectrum of NDHA. In addition, some quantum descriptors of the molecule are calculated and conformational analysis is performed and the results were compared with the crystallographic data. Copyright © 2011 Elsevier B.V. All rights reserved.

2-Benzylsulfanyl-N-(1,3-dimethylimidazolidin-2-ylideneaniline

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Ulrich Flörke

2013-04-01

Full Text Available The molecular structure of the title compound, C18H21N3S, shows a twisted conformation with a dihedral angle of 67.45 (4° between the aromatic ring planes and an N—C—C—S torsion angle of −5.01 (13°. The imidazolidine ring and the aniline moiety make a dihedral angle of 56.03 (4° and the asscociated C—N—C angle is 125.71 (10°. The guanidine-like C=N double bond is clearly localized, with a bond length of 1.2879 (14 Å. The C—S—C angle is 102.12 (5° and the S—C(aromatic and S—C bond lengths are 1.7643 (11 and 1.8159 (12 Å.

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].

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

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Chi-Heon Lee

2016-12-01

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

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

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Wolfgang Holzer

2010-09-01

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

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

International Nuclear Information System (INIS)

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

1991-01-01

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

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

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Guo-Liang Zhao

2012-05-01

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

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].

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].

N-(Thiazol-2-ylacetamide

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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.

A coordination polymer of CdII with benzene-1,3-dicarboxylate and 1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane

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Wei-Ping Zhang

2009-11-01

Full Text Available The title CdII coordination polymer, catena-poly[[{1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane}cadmium(II]-μ-benzene-1,3-dicarboxylato], [Cd(C8H4O4(C30H28N6]n, was obtained by reaction of CdCO3, benzene-1,3-dicarboxylic acid (H2btc and 1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane (L. The CdII cation is six-coordinated by an N2O4-donor set. L acts as a bidentate ligand and btc anions link CdII centers into a chain propagating parallel to [010].

New homo- and heteroleptic derivatives of trivalent ytterbium containing anion-radical 1,4-diazadiene ligands. Synthesis, properties and crystal structure of (C9H7)2Yb[2-MeC6H4NC(Me)C(Me)NC6H4Me-2] and [PhNC(Ph)C(Ph)NPh]3Yb complexes

International Nuclear Information System (INIS)

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

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

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Zheyu Zhang

2009-12-01

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

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

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Aliou H. Barry

2003-12-01

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

N-(2-Chlorophenyl-2-methylbenzamide

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B. Thimme Gowda

2008-08-01

Full Text Available In the structure of the title compound (N2CP2MBA, C14H12ClNO, the conformations of the N—H and C=O bonds are trans to each other. Furthermore, the conformation of the N—H bond is syn to the ortho-chloro group in the aniline ring and the C=O bond is syn to the ortho-methyl substituent in the benzoyl ring, similar to what is observed in 2-chloro-N-(2-chlorophenylbenzamide and 2-methyl-N-phenylbenzamide. The amide group makes almost the same dihedral angles of 41.2 (14 and 42.2 (13° with the aniline and benzoyl rings, respectively, while the dihedral angle between the benzoyl and aniline rings is only 7.4 (3°. The molecules in N2CP2MBA are packed into chains through N—H...O hydrogen bonds.

catena-Poly[[(triphenylphosphane-κPcopper(I]-di-μ-bromido-[(triphenylphosphane-κPcopper(I]-μ-1,3-bis(pyridin-4-ylpropane-κ2N:N′

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Jinfang Zhang

2012-03-01

Full Text Available Through a diffusion reaction, cuprous bromide, triphenylphosphane and 1,3-bis(pyridin-4-ylpropane (bpp were self-assembled to form the one-dimensional title compound, [Cu2Br2(C13H14N2(C18H15P2]n. Each CuI atom is coordinated by two Br atoms, one P atom from a triphenylphosphane ligand and one N atom from a bpp molecule in a distorted tetrahedral geometry. Two μ2-Br bridges connect two [Cu(PPh3]+ units to form neutral [CuBr(PPh3]2 dimers, which are linked by the flexible bridging bpp ligands to form a one-dimensional chain structure parallel to the c axis. The dihedral angle between the pyridine rings of the bpp ligand is 34.59 (14°.

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.

Synthesis of 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2-14C and N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-YL-2-14C)acetamide

International Nuclear Information System (INIS)

Fong, M.T.; Leaffer, M.A.

1986-01-01

We have prepared the 14 C-labeled analogs of NSC 261036, 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2- 14 C, and NSC 301467, N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-yl-2- 14 C) acetamide, for pharmacological, drug distribution, and mechanisms of action studies. The latter is an analog designed for lower toxicity and improved properties. The former is a metabolite of, and appears to be less toxic than, misonidazole. (author)

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

International Nuclear Information System (INIS)

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

1974-01-01

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

The nido-osmaboranes [2,2,2-(CO)(PPh(3))(2)-nido-2-OsB(5)H(9)] and [6,6,6-(CO)(PPh(3))(2)-nido-6-OsB(9)H(13)].

Science.gov (United States)

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].

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.

Crystal structure of (E-N-phenyl-N′-[1-(thiophen-2-ylethylidene]formohydrazide

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C. S. Dileep

2014-09-01

Full Text Available In the title compound, C13H12N2OS, the planes of the thiophene and phenyl rings are nearly perpendicular to each other, making a dihedral angle of 86.42 (12°. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a helical chain along the b-axis direction.

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.

Poly[[[diaquacobalt(II]-bis[μ2-1,1′-(butane-1,4-diyldiimidazole-κ2N3:N3′

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2009-03-01

Full Text Available In the title compound, {[Co(C10H14N42(H2O2](NO32}n, the CoII ion lies on an inversion center and is six-coordinated in an octahedral environment by four N atoms from four different 1,1′-butane-1,4-diyldiimidazole ligands and two O atoms from the two water molecules. The CoII atoms are bridged by ligands, generating a two-dimensional (4,4-network. Adjacent fishnet planes are linked to the nitrate anions via O—H...O hydrogen bonds, forming a three-dimensional supramolecular structure.

Diaqua[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II dibromide–aquabromido[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II bromide–dibromido[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II (1/2/1

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In-Chul Hwang

2009-01-01

Full Text Available There are three different MnII complexes in the asymmetric unit of the title compound, [Mn(C15H16N4(H2O2]Br2·2{[MnBr(C15H16N4(H2O]Br}·[MnBr2(C15H16N4]. In the neutral complex, the Mn2+ ion is six-coordinated in a distorted octahedral environment by four N atoms of the tetradentate ligand N,N′-bis(2-pyridylmethylenepropane-1,3-diamine (bppd and two bromide ligands. In the two cationic complexes, the Mn2+ ions are also six-coordinated in similar environments, but one Mn ion is coordinated by four N atoms of bppd, one Br atom and one O atom of a coordinating water molecule, whereas the other Mn ion is coordinated by four N atoms of bppd and two O atoms of water ligands. The complexes with two coordinated Br atoms or two H2O ligands are disposed about a twofold axis through Mn and C atoms with the special positions ({script{1over 2}}, y, 0 and (0, y, {script{1over 2}}, respectively. The compound displays intermolecular O—H...Br hydrogen bonding. There are intermolecular π–π interactions between adjacent pyridine rings, with centroid–centroid distances of 3.822 and 3.833 Å, and a C—H...O interaction is also present.

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

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Sarah Maloney

2013-02-01

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

Phenyl N-(2-methylphenylcarbamate

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Durre Shahwar

2009-07-01

Full Text Available In the title compound, C14H13NO2, the aromatic rings attached to the O and N atoms make dihedral angles of 62.65 (9 and 38.28 (11°, respectively, with the central carbamate group. The benzene rings are oriented at a dihedral angle of 39.22 (10°. In the crystal, a very weak C—H...π interaction occurs.

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

Science.gov (United States)

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

2017-02-28

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

Bis[2-(1,3-benzothiazol-2-ylphenyl-κ2C1,N][1,3-bis(4-bromophenylpropane-1,3-dionato-κ2O,O′]iridium(III

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Sung Kwon Kang

2013-08-01

Full Text Available The title complex, [Ir(C15H9Br2O2(C13H8NS2], lies about a crystallographic twofold rotation axis passing through the IrIII atom and the central C atom of the bis(bromophenylpropane-1,3-dionate ligand. The IrIII atom adopts a distorted octahedral geometry coordinated by two N atoms in the axial positions, and two C and two O atoms in the equatorial plane. The dihedral angle between the two thiazole ring systems in the complex is 77.45 (10°.

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

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Eyad Mallah

2015-01-01

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

Syntheses, structures and redox properties of some complexes containing the Os(dppe)Cp* fragment, including [{Os(dppe)Cp*}2(mu-C triple bondCC triple bond C)].

Science.gov (United States)

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.

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

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Augusto Rivera

2013-02-01

Full Text Available In the crystal structure of the title compound, C21H24F2N2O2, there are two intramolecular O—H...N hydrogen bonds involving the N atoms of the imidazolidine ring and the hydroxy groups. The crystal studied was a meso compound obtained by the reaction of the aminal (2S,7R,11S,16R-1,8,10,17-tetraazapentacyclo[8.8.1.18,17.02,7.011,16]cosane with 4-fluorophenol. The imidazolidine ring has a twisted conformation with a CH—CH—N—CH2 torsion angle of 44.99 (14° and, surprisingly, the lone pairs of the N atoms are disposed in a syn isomerism, making the title compound an exception to the typical `rabbit-ear effect' in 1,2-diamines. In the crystal, molecules are linked via C—H...F hydrogen bonds, forming chains along the c-axis direction. These chains are linked via another C—H...F hydrogen bond, forming a three-dimensional network.

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

International Nuclear Information System (INIS)

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

1996-01-01

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

(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.

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.

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.

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

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Salman A. Khan

2010-03-01

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

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

International Nuclear Information System (INIS)

Jagannatha Swamy, S.

2002-01-01

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

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.

Crystal structures of N-(4-chlorophenyl-2-[(4,6-diaminopyrimidin-2-ylsulfanyl]acetamide and N-(3-chlorophenyl-2-[(4,6-diaminopyrimidin-2-ylsulfanyl]acetamide

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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.

2-((1E-1-{2-[(2Z-3,4-Diphenyl-2,3-dihydro-1,3-thiazol-2-ylidene]hydrazin-1-ylidene}ethylpyridin-1-ium bromide monohydrate

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Mehmet Akkurt

2014-04-01

Full Text Available In the title compound, C22H19N4S+·Br−·H2O, the dihedral angles between the phenyl groups and the mean plane of the thiazolylidene ring are 34.69 (13 and 64.27 (13°, respectively, while that between the thiazolylidene and pyridinium rings is 14.73 (13°. In the crystal, zigzag chains of alternating bromide ions and water molecules associate through O—H...Br interactions run in channels approximately parallel to the b axis. These chains help form parallel chains of cations through N—H...O, C—H...N and C—H...Br hydrogen bonds.

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

OpenAIRE

Xu, Sheng-Zhen

2007-01-01

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

(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.

N-(4-Nitrobenzoyl)-N'-(1,5-dimethyl-3-oxo-2-phenyl-1H-3(2H)-pyrazolyl)-thiourea hydrate: Synthesis, spectroscopic characterization, X-ray structure and DFT studies

Science.gov (United States)

Arslan, N. Burcu; Kazak, Canan; Aydın, Fatma

2012-04-01

The title molecule (C19H17N5O4S·H2O) was synthesized and characterized by IR-NMR spectroscopy, MS and single-crystal X-ray diffraction. The molecular geometry, vibrational frequencies and gauge-independent atomic orbital (GIAO) 1H and 13C NMR chemical shift values of the compound in the ground state have been calculated by using the density functional theory (DFT) method with 6-31G(d) basis set, and compared with the experimental data. All the assignments of the theoretical frequencies were performed by potential energy distributions using VEDA 4 program. The calculated results show that the optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies and 1H and 13C NMR chemical shift values show good agreement with experimental data. To determine conformational flexibility, the molecular energy profile of the title compound was obtained with respect to the selected torsion angle, which was varied from -180° to +180° in steps of 10°. Besides, molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and thermodynamic properties of the compound were investigated by theoretical calculations.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-12-01

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

The synthesis of 2-14C-N-nitrosothiazolidine

International Nuclear Information System (INIS)

Cragin, D.W.; Shibamoto, Takayuki

1989-01-01

2- 14 C-N-Nitrosothiazolidine was synthesized with a chemical purity of 99.6%, a radio chemical purity of 99.4%, and an overall yield of 30.7%. Unlabelled N-nitrosothiazolidine, synthesized using the same method, resulted in a purity of 99.85% by capillary GC and 99.7% by HPLC. Analysis of N-nitrosothiazolidine by GC was found to require a low injection port temperature of 160 0 C to prevent denitrosation in the injection port. During the nitrosation of thiazolidine, if the pH was reduced below 4 with hydrochloric acid, ring hydrolysis occurred, and chlorinated disulfide compounds formed. (author)

N,N,N,N′,N′,N′-Hexakis(2-hydroxyethylbutane-1,4-diaminium bis(2-sulfanylidene-1,3-dithiole-4,5-dithiolato-κ2S4,S5zincate

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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.

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

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Wolfgang Frey

2008-03-01

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

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

Science.gov (United States)

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

2018-06-01

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

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.

Synthesis of 7-[α-(2-amino-[2-14C]thiazol-4-yl)-α-(Z)-methoxyimin oacetamido]-3-(1-methylpyrrolidinio)methyl-3-cephem-4-carboxylate hydrochloride ([14C]cefepime hydrochloride)

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)

cis-[1,4-Bis(diphenylphosphanylbutane-κ2P,P′]dichlorido(cyclohexane-1,2-diamine-κ2N,N′ruthenium(II dichloromethane monosolvate

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Ismail Warad

2012-05-01

Full Text Available In the title compound, [RuCl2(C6H14N2(C28H28P2]·CH2Cl2, the RuII ion is coordinated in a slightly distorted octahedral environment, formed by two cis-oriented chloride ligands, two cis P atoms of a 1,4-bis(diphenylphosphanylbutane ligand and two cis-chelating N atoms of a bidentate cyclohexane-1,2-diamine ligand. In the crystal, pairs of molecules form inversion dimers via N—H...Cl hydrogen bonds. In addition, intramolecular N—H...Cl and weak C—H...Cl, C—H...N, N—H...π and C—H...π hydrogen bonds are observed. One of the Cl atoms of the solvent molecule is disordered over two sites with refined occupancies of 0.62 (1 and 0.38 (1.

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

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Valentina A. Kalibabchuk

2009-09-01

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

(C6H16N2)Zn3(HPO3)4H2O: a new layered zinc phosphite templated by diprotonated trans-1,4-diaminocyclohexane

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

(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.

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

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Jing Xu

2009-08-01

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

1,4-Dihexyloxy-2,5-bis(2-nitrophenylbenzene

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Norma Wrobel

2012-04-01

Full Text Available The title compound, C30H36N2O6, was prepared via twofold Suzuki coupling of a diboronic acid with bromonitrobenzene. The molecule is located on a crystallographic inversion centre. The lateral benzene ring and the central ring make a dihedral angle of 48.75 (14° and the nitro group is twisted by 41.47 (13° out of the plane of the benzene ring. The nitro and hexyloxy groups are in close proximity and the hexyloxy chain adopts an all-anti conformation.

Low-temperature heat capacities and thermodynamic properties of ethylenediammonium tetrachlorozincate chloride (C2H10N2)2(ZnCl4)Cl2

International Nuclear Information System (INIS)

He, Dong-Hua; Di, You-Ying; Wang, Bin; Dan, Wen-Yan; Tan, Zhi-Cheng

2010-01-01

The ethylenediammonium tetrachlorozincate chloride (C 2 H 10 N 2 ) 2 (ZnCl 4 )Cl 2 was synthesized. Chemical analysis, elemental analysis, and X-ray crystallography were applied to characterize the composition and crystal structure of the complex. Low-temperature heat capacities of the compound were measured by a precision automatic adiabatic calorimeter over the temperature range from T = 77-377 K. A polynomial equation of heat capacities as a function of the reduced temperature was fitted by a least square method. Based on the polynomial equation, the smoothed heat capacities and thermodynamic functions of the title compound relative to the standard reference temperature 298.15 K were calculated at intervals of 5 K. A thermochemical cycle was designed and the enthalpy change of the solid phase reaction of ethylenediamine dihydrochloride with zinc chloride was determined to be Δ r H m o =-(17.9±0.6)kJmol -1 by an isoperibol solution-reaction calorimeter. Finally, the standard molar enthalpy of formation of the title compound was derived to be Δ f H m o [(C 2 H 10 N 2 ) 2 (ZnCl 4 )Cl 2 ,s]=-(1514.4±2.7)kJmol -1 in accordance with Hess law.

(μ-trans-1,2-Di-4-pyridylethylene-κ2N:N′bis[bis(N,N-diisopropyldithiocarbamato-κ2S,S′zinc(II

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Hadi D. Arman

2009-11-01

Full Text Available The dinuclear title compound, [Zn2(C7H14NS24(C12H10N2], is centrosymmetric about the central C=C bond. The five-coordinate Zn atom is bonded to two asymmetrically chelating dithiocarbamate ligands and a pyridine N atom to define an NS4 coordination geometry tending towards a square pyramid, with the N atom in the apical site. In the crystal structure, C—H...S contacts lead to supramolecular chains.

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

International Nuclear Information System (INIS)

Vaqueiro, Paz

2006-01-01

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

Determination of astrophysical 13N(p, γ)14O S-factors from the asymptotic normalization coefficient of 14C→13C + n

International Nuclear Information System (INIS)

Guo Bing; Li Zhihong

2007-01-01

The angular distribution of the 13 C(d,p) 14 C reaction is reanalysed using the Johnson-Soper approach. The squared asymptotic normalization coefficient (ANC) of virtual decay 14 C→ 13 C + n is then derived to be 21.4 ± 5.0 fm -1 . The squared ANC and spectroscopic factor (SF) of 14 O→ 13 N + p are extracted to be 30.4 ± 7.1 fm -1 and 1.94 ± 0.45, respectively. The astrophysical S-factors and reaction rates of 13 N(p, γ) 14 O are determined from the ANC of 14 O→ 13 N + p using the R-matrix approach. (authors)

4-Bromo-N-(di-n-propyl-carbamothioyl)-benzamide.

Science.gov (United States)

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.

Crystal structure of poly[[μ-1,1′-(butane-1,4-diylbis(1H-benzimidazole-κ2N3:N3′]{μ-4,4′-[1,4-phenylenebis(oxy]dibenzoato-κ4O,O′:O′′,O′′′}cobalt(II

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Chen Xie

2015-06-01

Full Text Available In the title compound, [Co(C20H12O6(C18H18N4]n, the CoII atom, located on a twofold rotation axis, is hexacoordinated to four O from two bis-bidentate 4,4′-[phenylenebis(oxy]dibenzoate (L ligands and two N atoms from two 1,1′-(butane-1,4-diylbis(1H-benzimidazole (bbbm ligands, forming a distorted octahedral cis-N2O4 coordination environment. Polymeric zigzag chains along [102] are built up by the bridging L ligands. These chains are additionally connected by the bbbm ligands to produce a two-dimensional coordination polymer parallel too (010.

2-Phenylimidazolium hemi(benzene-1,3-dicarboxylate monohydrate

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Wen-Yu Zhang

2011-08-01

Full Text Available The asymmetric unit of the title compound, C9H9N2+·0.5C8H4O4−·H2O, contains one 2-phenylimidazolium cation, half a benzene-1,3-dicarboxylate anion and one water molecule. In the crystal, components are connected by N—H...O and O—H...O hydrogen-bonding interactions into a three-dimensional network.

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

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Ming-Jian Li

2009-09-01

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

Synthesis and structure of the extended phosphazane ligand [(1,4-C6H4){N(μ-PN(t)Bu)2N(t)Bu}2](4).

Science.gov (United States)

Sevilla, Raquel; Less, Robert J; García-Rodríguez, Raúl; Bond, Andrew D; Wright, Dominic S

2016-02-07

The reaction of the phenylene-bridged precursor (1,4-C6H4)[N(PCl2)2]2 with (t)BuNH2 in the presence of Et3N gives the new ligand precursor (1,4-C6H4)[N(μ-N(t)Bu)2(PNH(t)Bu)2]2, deprotonation of which with Bu2Mg gives the novel tetraanion [(1,4-C6H4){N(μ-N(t)Bu)2(PN(t)Bu)2}2](4-).

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.

4-Bromo-N-(di-n-propyl­carbamothioyl)­benzamide

OpenAIRE

Binzet, Gün; Flörke, Ulrich; Külcü, Nevzat; Arslan, Hakan

2009-01-01

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 asymmet...

Dual element ((15)N/(14)N, (13)C/(12)C) isotope analysis of glyphosate and AMPA by derivatization-gas chromatography isotope ratio mass spectrometry (GC/IRMS) combined with LC/IRMS.

Science.gov (United States)

Mogusu, Emmanuel O; Wolbert, J Benjamin; Kujawinski, Dorothea M; Jochmann, Maik A; Elsner, Martin

2015-07-01

To assess sources and degradation of the herbicide glyphosate [N-(phosphonomethyl) glycine] and its metabolite AMPA (aminomethylphosphonic acid), concentration measurements are often inconclusive and even (13)C/(12)C analysis alone may give limited information. To advance isotope ratio analysis of an additional element, we present compound-specific (15)N/(14)N analysis of glyphosate and AMPA by a two step derivatization in combination with gas chromatography/isotope ratio mass spectrometry (GC/IRMS). The N-H group was derivatized with isopropyl chloroformate (iso-PCF), and remaining acidic groups were subsequently methylated with trimethylsilyldiazomethane (TMSD). Iso-PCF treatment at pH 10 indicated decomposition of the derivative. At pH 10, and with an excess of iso-PCF by 10-24, greatest yields and accurate (15)N/(14)N ratios were obtained (deviation from elemental analyzer-IRMS: -0.2 ± 0.9% for glyphosate; -0.4 ± 0.7% for AMPA). Limits for accurate δ(15)N analysis of glyphosate and AMPA were 150 and 250 ng injected, respectively. A combination of δ(15)N and δ(13)C analysis by liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) (1) enabled an improved distinction of commercial glyphosate products and (2) showed that glyphosate isotope values during degradation by MnO2 clearly fell outside the commercial product range. This highlights the potential of combined carbon and nitrogen isotopes analysis to trace sources and degradation of glyphosate.

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

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Khadija El Bourakadi

2017-05-01

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

Crystal structure of tri­chlorido­(4'-ferrocenyl-2,2':6',2''-terpyridine-[kappa]3N,N',N'')iridium(III) aceto­nitrile disolvate

KAUST Repository

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

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

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Jiang-Sheng Li

2009-08-01

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

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

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Abdullah M. Asiri

2011-02-01

Full Text Available The title compound 2-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-indane-1,3-dione (3 was synthesized in high yield by reaction of 3,5-dimethyl-1-phenyl-pyrazole-4-carbaldehyde and indane-1,3-dione in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H NMR, 13C NMR and GC-MS spectral analysis.

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

Science.gov (United States)

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

2011-01-01

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

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

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Nada Kheira Sebbar

2015-06-01

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

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

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Hoong-Kun Fun

2009-04-01

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

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.

Synthesis of pinacolyl [14C]methylphosphonochloridate

International Nuclear Information System (INIS)

Horvat, J.; Keglevic, D.; Klaic, B.; Kveder, S.; Ladesic, B.; Cosic, M.; Zupanc, S.

1982-01-01

A three-step synthetic route to pinacolyl [ 14 C]methylphosphonochloridate (3) from [ 14 C]methyl iodide is described. Condensation of sodium di-n-butyl phosphite with [ 14 C]methyl iodide gave di-n-butyl [ 14 C]methylphosphonate (1) which was converted into [ 14 C]methylphosphonic dichloride (2) by prolonged refluxing with thionyl chloride. Reaction of 2 with pinacolyl alcohol in the presence of N,N-di-n--propylaniline as the base afforded the title compound 3. The radiochemical yield of redistilled 3 was 34,2% based on 1, and the overall radiochemical yield was 20,0% from [ 14 C]methyl iodide. (author)

Volume properties and refraction of aqueous solutions of bisadducts of light fullerene C60 and essential amino acids lysine, threonine, and oxyproline (C60(C6H13N2O2)2, C60(C4H8NO3)2, and C60(C5H9NO2)2) at 25°C

Science.gov (United States)

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.

4-((E-{2-[N-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylcarboximidoyl]benzylidene}amino-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one

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Richard Betz

2011-10-01

Full Text Available The title compound, C30H28N6O2, is a symmetric diimine derived from ortho-dibenzaldehyde. Both C=N bonds are (E-configured. The terminal N-bonded phenyl groups adopt staggered conformations relative to their respective parent heterocycles, the relevant least-squares planes intersect at angles of 32.35 (11 and 38.59 (10°. In the crystal, C—H...O contacts connect the molecules into chains along the b axis and give rise to a C11(14C11(14 and a R22(12 pattern on different levels of graph-set analysis. The shortest intercentroid distance between two centroids was found at 4.2074 (11 Å between the two five-membered heterocycles.

Synthesis of [14C]-62514, a radiolabelled derivative of erythromycin A, via [2-14C]N,N-dimethylethylenediamine

International Nuclear Information System (INIS)

Surber, B.W.; Baker, W.R.; Seif, L.

1991-01-01

The synthesis of [ 14 C]A-62514, 11-deoxy-11[carboxy(2-dimethylamino-[1- 14 C]ethyl)amino]-6-0-methyl-e rythromycin A 11,12-(cyclic ester), was performed in five steps. The key intermediate, [2- 14 C]N,N-dimethylethyl-enediamine, was obtained in 80% yield by reacting Eschenmoser's salt with K 14 CN and reducing the resulting [1- 14 C]N,N-dimethylglycinonitrile with H 2 and Raney Ni in methanol and ammonium hydroxide. The final product was obtained 97% radiochemically pure in an overall radiochemical yield of 14%, with a specific activity of 39 mCi/mmol. (author)

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

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Jan Světlík

2009-05-01

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

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

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Özden Özel Güven

2010-04-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-12-15

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

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.

Diammine{N-[2-(hydroxyiminopropionyl]-N′-[2-(oxidoiminopropionyl]propane-1,3-diaminido-κ4N,N′,N′′,N′′′}iron(III

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Stefania Tomyn

2012-12-01

Full Text Available In the title compound, [Fe(C9H13N4O4(NH32], the FeIII atom, lying on a mirror plane, is coordinated by four N atoms of a triply deprotonated tetradentate N-[2-(hydroxyiminopropionyl]-N′-[2-(oxidoiminopropionyl]propane-1,3-diaminide ligand in the equatorial plane and two N atoms of two ammonia molecules at the axial positions in a distorted octahedral geometry. A short intramolecular O—H...O hydrogen bond between the cis-disposed oxime O atoms stabilizes the pseudo-macrocyclic configuration of the ligand. In the crystal, molecules are linked by N—H...O hydrogen bonds into a three-dimensional network. The ligand has a mirror-plane symmetry. One of the methylene groups of the propane bridge is disordered over two sets of sites with equal occupancy factors.

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

DEFF Research Database (Denmark)

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

2003-01-01

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

Synthesis of 1-amino-2-[3-(3-[2,6-14C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3,4-dione hydrochloride

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)

(Acetonitrile-κNchloridobis[2-(pyridin-2-ylphenyl-κ2C1,N]iridium(III

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Florian Blasberg

2011-12-01

Full Text Available The IrIII atom of the title compound, [Ir(C11H8N2Cl(CH3CN], displays a distorted octahedral coordination. The pyridyl groups are in trans positions [N—Ir—N = 173.07 (10°], while the phenyl groups are trans with respect to the acetonitrile and chloride groups [C—Ir—N = 178.13 (11 and C—Ir—Cl = 176.22 (9°]. The pyridylphenyl groups only show a small deviation from planarity, with the dihedral angle between the planes of the two six-membered rings in each pyridylphenyl group being 5.6 (2 and 5.8 (1°. The crystal packing shows intermolecular C—H...Cl, C—H...π(acetonitrile and C—H...π(pyridylphenyl contacts.

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.

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

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Ke, W.; Sun, N.B.

2013-01-01

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

(Z-3-(4-Chlorophenyl-1-(2,4-difluorophenyl-2-(1H-1,2,4-triazol-1-ylprop-2-en-1-one

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Xin-Mei Peng

2012-06-01

Full Text Available The asymmetric unit of the title compound, C17H10ClF2N3O, contains three independent molecules. In each molecule, the C=C bond has a cis conformation with respect to the triazole and chlorophenyl groups. The dihedral angles formed by the triazole ring with the diflurophenyl and chlorophenyl benzene rings, respectively, are 20.10 (14 and 73.22 (15, 25.31 (15 and 84.44 (15, and 16.44 (13 and 61.72 (14° in the three molecules while the dihedral angles between the benzene rings are 66.54 (13, 85.82 (12 and 58.37 (12°.

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

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

2018-06-01

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

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

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Augusto Rivera

2013-07-01

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

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

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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].

Hydrothermal synthesis, structural elucidation, spectroscopic studies, thermal behavior and luminescence properties of a new 3-d compound: FeAlF2(C10H8N2)(HPO4)2(H2O)

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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.

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.

catena-Poly[[[tetraaquazinc(II]-μ-4,4′-bipyridine-κ2N:N′] benzene-1,4-dicarboxylate

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Ming-Bo Ruan

2009-07-01

Full Text Available In the title compound, {[Zn(C10H8N2(H2O4](C8H4O4}n, the ZnII atoms, lying on a twofold rotation axis, are bridged by 4,4′-bipyridine ligands, resulting in a linear chain along the b axis. In the chain, the ZnII atom adopts a slightly distorted octahedral coordination geometry involving four water molecules at the equatorial positions. The noncoordinated benzene-1,4-dicarboxylate anion, which is also located on a twofold rotation axis, bridges adjacent chains through O—H...O hydrogen bonds, forming a three-dimensional supramolecular network.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

N,N′-Bis(diphenylmethylbenzene-1,4-diamine

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Aeed S. Al-Fahdawi

2014-01-01

Full Text Available The complete molecule of the title compound, C32H28N2, is generated by crystallographic inversion symmetry. The dihedral angles between the central aromatic ring and the pendant adjacent rings are 61.37 (16 and 74.20 (14°. The N—H group does not participate in hydrogen bonds and there are no aromatic π–π stacking interactions in the crystal.

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

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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.

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.

4,4′,6,6′-Tetra-tert-butyl-2,2′-[1,3-diazinane-1,3-diylbis(methylene]diphenol 0.25-hydrate

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Manman Zhang

2012-07-01

Full Text Available The title compound, C34H54N2O2·0.25H2O, the organic molecule, a potential tetradentate ligand with a bulky phenolic donor, has overall mirror symmetry. A partially occupied water molecule of solvation is present in the lattice. The six-membered 1,3-diazinane ring displays a chair conformation. An intramolecular O—H...N hydrogen bond ocurs. In the crystal, molecules are linked by O—H...O interactions.

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

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2009-03-01

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

trans-(2-Benzoylpyridine-κ2N,Odichlorido[2-(2-pyridylcarbonylphenyl-κ2C1,N]iridium(III dichloromethane solvate

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2009-03-01

Full Text Available The title compound, [Ir(C12H8NOCl2(C12H9NO]·CH2Cl2, which was obtained from the reaction of iridium(III chloride trihydrate and 2-benzoylpyridine, contains an IrIII atom coordinated by two N, one O, one C and two Cl atoms in trans positions, forming a distorted octahedral environment. The solvent molecule CH2Cl2 is disordered over two positions with an occupancy of 0.8:0.2.

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.

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

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Sammer Yousuf

2012-08-01

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

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

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Kai-Long Zhong

2010-03-01

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

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

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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.

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.

Synthesis and biological activity of some 1,3-dihydro-2H-3-benzazepin-2-ones with a piperazine moiety as bradycardic agents.

Science.gov (United States)

Liang, Hong-Yu; Zhang, Deng-Qing; Yue, Yun; Shi, Zhe; Zhao, Sheng-Yin

2010-02-01

A series of 1,3-dihydro-2H-3-benzazepin-2-ones with a piperazine moiety were designed and synthesized by treating the common intermediate of 1,3-dihydro-7,8-dimethoxy-3-[3-(1-piperazinyl)propyl]-2H-3-benzazepin-2-ones with a variety of N-aryl-2-chloroacetamides and acyl chlorides. Their structures have been characterized by (1)H-NMR, MS, and elemental analysis. The title compounds were evaluated for their bradycardic activity in vitro. Most of the synthesized compounds exhibited some vasorelaxant activity and heart-rate-reducing activity with bradycardic potency.

Synthesis, characterization, and anomalous dielectric and conductivity performance of one-dimensional (bdaH)InSe2 (bda = 1,4-butanediamine)

International Nuclear Information System (INIS)

Du, Ke-Zhao; Hu, Wan-Biao; Hu, Bing; Guan, Xiang-Feng; Huang, Xiao-Ying

2011-01-01

Graphical abstract: Anomalous dielectric and conductivity performance have been observed in the organic-containing indium selenide (bdaH)InSe 2 , which are attributed to the water molecules existing in the crystal boundary rather than phase transition. Highlights: → The title compound is the first example of organic-containing one-dimensional indium selenide. → The anomalous dielectric peak is attributed to water molecules in crystal boundary. → The inorganic and organic components of the title compound are connected via hydrogen bonding to form a supramolecular three-dimensional network. -- Abstract: A new indium selenide, namely (bdaH)InSe 2 (1) (bda = 1,4-butanediamine) has been solvothermally synthesized and structurally characterized. It belongs to the non-centrosymmetric space group Fdd2. Its structure features an infinite one-dimensional anionic chain of [InSe 2 ] n n- with monoprotonated [bdaH] + as charge compensating cation. The organic [bdaH] + cations are joined into a supramolecular one-dimensional chain via N-H...N hydrogen bonding, which further interacts with the inorganic chain via N-H...Se and C-H...Se hydrogen bonding, forming a supramolecular three-dimensional network. Based on such a well-defined structure, the thermal stability, optical, conductivity, and dielectric properties were systematically investigated, showing that dielectric constant, as well as conductivity, had a hump at about 95 o C, which could be attributed to water molecules in the crystal boundary.

Synthesis of 14C-labeled 3-{[1-ethoxycarbonyl-3-phenyl-(1S)-propyl]amino}-2,3,4,5-tetrahydro-2-oxo -1H-1-(3S)-benzazepine-1-acetic acid hydrochloride ([14C]CGS 14824A)

International Nuclear Information System (INIS)

Chaudhuri, N.K.; Patera, R.; Markus, B.; Mingsang Sung

1987-01-01

The title compound, CGS 14824A, was synthesized with a 14 C-label in the azepine ring in 14 steps starting with 1-bromo-3-phenylpropane (1) and K 14 CN in an overall yield of 1.31%. The reaction of 1 with K 14 CN yielded the nitrile 2 which upon hydrolysis followed by ring closure gave α-tetralone-1- 14 C (4). Bromination of 4 followed by oxime formation gave the bromo oxime 5, which upon Beckmann rearrangement by acid treatment yielded the ring expansion product 6. The bromine atom of 6 was then replaced by an azido group, and an acetic ester side chain was introduced at the nitrogen atom. Catalytic reduction of the azido compound 8 gave a mixture of epimeric amino esters which was resolved by salt formation with L-tartaric acid. The negatively rotating isomer was then reacted with 4-phenyl-2-oxo-butanoate in presence of sodium cyanoborohydride to give a mixture of diastereoisomers which were separated as their benzyl esters by chromatography. The major isomer was then converted to labeled CGS 14824A. (author)

Nido-Carborane building-block reagents. 2. Bulky-substituent (alkyl)2C2B4H6 derivatives and (C6H5)2C2B4H6: synthesis and properties

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

A conformational study of the adducts of 2'-deoxythymidine and 2,2,6,6-tetramethyl-1,4-piperidone-N-oxyl by sup(1)H and sup(13)C nuclear magnetic resonance

International Nuclear Information System (INIS)

Hruska, F.E.; Berger, Maurice; Cadet, Jean; Remin, Mieczyslaw

1985-01-01

γ-Irradiation of oxygen-free, aqueous solutions of 2'-deoxythymidine in the presence of the organic nitroxide free radical, 2,2,6,6-tetramethyl-1,4-piperidone-N-oxyl (TAN) leads to a complex mixture of products in which the TAN moiety is linked to the C5 or C6 position of a 5,6-saturated thymine ring. Extensive sup(1)H and sup(13)C nmr data are provided for the eight TAN-dT adducts which are produced in the largest amounts. The results show that the conformational properties of the sugar moiety are dependent on the point of attachment of the TAN group and the configuration of the standard thymine ring

Synthesis of {sup 13}C- and {sup 14}C-labeled 1192U90, an ortho-amino benzamide with a preclinical atypical antipsychotic profile

Energy Technology Data Exchange (ETDEWEB)

Norman, M.H.; Gabriel, S.D. [Glaxo Wellcome Inc., Research Triangle Park, NC (United States)

1996-03-01

Three isotopic forms of potential antipsychotic agent 1192U90 (2-amino-N-(4-(4-(1,2-benzisthiazol-3-yl)-piperazinyl)butyl)benzam ide) were synthesized: one containing {sup 13}C-isotopes and two containing {sup 14}C-isotopes. The compound in which the ortho-amino benzamide ring is completely {sup 13}C-labeled was prepared in a four-step sequence starting from [{sup 13}C{sub 6}]aniline. The {sup 14}C-labeled compounds were prepared by methods analogous to those previously described for the unlabeled material. The key step involved the condensation of 3-(4-(4aminobutyl)-1-piperazinyl)-1,2-benzisothiazole with isatoic anhydride. The first {sup 14}C-labeled compound (3) was prepared from {sup 14}C-labeled 3-(4-(4-aminobutyl)-1-piperazinyl)-1,2-benzisothiazole, while the second compound (4) derived its isotopic label from [{sup 14}C]isatoic anhydride. Compound 3 had a specific activity of 26.55 mCi/mmol, a radiochemical purity of 99.3%, and a radiochemical yield of 3.4%. Compound 4 had a specific activity of 22.67 mCi/mmol and a radiochemical purity of 99.2%. (author).

(R-N-{2-tert-Butyl-2-[(R-tert-butylsulfonamido]ethylidene}-tert-butanesulfonamide

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Cong-Bin Fan

2008-10-01

Full Text Available The title compound, C14H30N2O2S2, is the product of the monoaddition reaction of tert-butyl magnesium chloride with bis-[(R-N-tert-butanesulfinyl]ethanediimine. There are two almost identical molecules in the asymmetric unit, the molecular conformation of which is stabilized by an intramolecular N—H...N hydrogen bond.

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

Science.gov (United States)

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

2015-10-05

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

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

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Khaled Boukebbous

2016-10-01

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

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

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Igor O. Fritsky

2008-02-01

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

[μ-1,1′-(Butane-1,4-diyldi-1H-benzimidazole-κ2N3:N3′]bis{[N,N′-bis(carboxymethylethylenediamine-N,N′-diacetato-κ5O,O′,O′′,N,N′]mercury(II} methanol disolvate

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Gang-Sen Li

2009-08-01

Full Text Available The binuclear title complex, [Hg2(C10H14N2O82(C18H18N4]·2CH3OH, lies on an inversion center with the unique HgII ion coordinated in a disorted octahedral environment with one Hg—N bond significantly shorter than the other two. In the crystal structure, intermolecular O—H...O hydrogen bonds link complex and solvent molecules into a three-dimensional network.

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.

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.

Molecular dynamics simulation investigations of H2/D2 dissocitive chemisorption dynamics on Cun(n=13-14) Rigid/nonrigid clusters

International Nuclear Information System (INIS)

Elzein, N.

2004-01-01

In this work with a use of molecular dynamic simulations we have reported the results of a quasiclassical simulation study of the interaction of H2/(D2) with Cu N (N=13-14) atoms in both rigid /(non rigid) clusters.The geometry of the cluster is obtained by an embedded-atom (EA) mode potential, and the interaction between the molecule and cIuster is described by a LEPS -London-Eyring -Polanyi-Sato) potential energy function.Both channels the reactive dissociative adsorption of the molecule on the cIuster) and non reactive (scattering of the molecule from the cluster) are considered. The dissociative chemisorption probability, cross section and rate constant are studied as functions of the initial quantal rovibrational state of the molecule, collision energy, impact parameter and the temperature (OK,296K,834K ,1014K,1554K) of the clusters

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.

Synthesis of 14C- and 2H-labeled 1,3 dihydro-3, 3-dimethyl-5-(1,4,5,6,- tetrahydro-6-oxo-3-pyridazinyl)-2H-indol-2-one (LY195115), an orally effective positive inotrope

International Nuclear Information System (INIS)

Robertson, D.W.; Krushinski, J.H.; Kau, D.

1986-01-01

The synthesis of 14 C- and 2 H-labeled 1,3-dihydro-3,3-dimethyl-5-(1,4,5,6-tetrahydro-6-oxo-3-pyridazinyl)-2H-indol -2-one (LY195115), an extremely potent, orally-effective cardiotonic with inotropic and vasodilator activities is described. The 14 C-label was introduced in the antepenultimate step by reaction of a β-chloroketone precursor with Na 14 CN; acid-catalyzed hydrolysis and cyclization with hydrazine provided the tetrahydropyridazinone bearing the 14 C-label in the oxo-carbon. 1,3-Dihydro-3,3-di(methyl-d 3 ) -2H-indol-2-one was prepared by exhaustive methylation of 1-acetyl-1,3-dihydro-2H-indol-2-one with sodium hydride and iodomethane-d 3 , followed by removal of the nitrogen protecting group. This labeled material was converted in two steps to [ 2 H 6 ]-LY195115. (author)

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

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Hui-Ping Xiong

2012-08-01

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

Crystal structure, NMR study, dc-conductivity and dielectric relaxation studies of a new compound [C2H10N2]Cd(SCN2Cl2

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Gargouri M.

2012-06-01

Full Text Available The crystal structure, the solid NMR spectroscopy and the complex impedance study have been carried out on [C2H10N2]CdCl2(SCN2. Characterization by single crystal X-ray crystallography shows that the cadmium atoms have à 2N2S2Cl hexa-coordination sphere, exhibiting pseudo-octahedral geometry. The cadmium atoms are bridged by two thiocyanate ions generating 1-D polymeric-chains. These chains are themselves interconnected by means of N-H…Cl(NCS hydrogen bonds originating from the organic cation [(NH32(CH22]2+. 111Cd isotropic chemical shifts span a range of 268ppm. The cadmium atom exhibits multiplets that result from 111Cd-14N spin-spin coupling. Examination of 111Cd and 13C MAS line shapes shows direct measurement of the indirect spin-spin coupling constant 2J(111Cd, 14N = 105Hz and the dipolar coupling constant of 1381Hz . Impedance spectroscopy measurements of [C2H10N2]CdCl2(SCN2 have been studied from 209Hz to 5 MHz over the temperature range 300-370 K. The Cole-Cole (Z” versus Z’ plots are fitted to two equivalent circuits models. The formalism of complex permittivity and impedance were employed to analyze the experimental data. The dc conductivity follows the Arrhenius relation with an activation energy Ea = 0.54 (3 eV.

The synthesis of 5'-[14C1] and 3a, 4-[13C2] labelled panadiplon (U-78875; 3-(5'-cyclopropyl-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)-imidazo-[1,5a]-quinoxalin-4(5H)-one)

International Nuclear Information System (INIS)

Ackland, M.J.; Howard, M.R.; Dring, L.G.

1993-01-01

5'-[ 14 C 1 ]Panadiplon was prepared in 3 steps starting from [ 14 C 1 ]cyclopropane carboxylic acid and 3-(5'-cyano-1,2,4-oxadiazol-3-yl)-5-(1-methylethyl)-imidazo-[1,5a] -quinoxalin-4(5H)-one. 3a, 4-[ 13 C 2 ]Panadiplon was prepared in two steps from 13 C 2 -oxalic acid and N-1-(1-methylethyl)-o-phenylenediamine. The position of labelling was confirmed by the appearance of two coupled resonances (J C-C =80.59 Hz) at 121.95 and 154.39 ppm in the assigned 13 C-NMR spectrum. (Author)

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

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Dong-liang Liu

2011-12-01

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

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

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Xu Zhu

2013-10-01

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

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

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Narsimha Reddy Penthala

2009-08-01

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

Fragmentations and rearrangements of metastable [C2H5OS]+ ions

NARCIS (Netherlands)

de Vries, Marcel; Oudman, D; Weringa, WD

1992-01-01

Several [C2H5OS]+ ions with different structures were generated from the appropriate precursors and their metastable ion spectra were determined. Deuterium labelled analogues of some of the [C2H5OS]+ ions were used to elucidate the nature of the observed fragmentations and their mechanisms.

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.

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].

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°.

N-Cyclohexyl-N-ethylbenzenesulfonamide

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Islam Ullah Khan

2009-11-01

Full Text Available The title compound, C14H21NO2S, synthesized by N-methylation of cyclohexylamine sulfonamide with ethyl iodide is of interest as a precursor to biologically active sulfur-containing heterocyclic compounds. There are two independent molecules in the asymmetric unit. The dihedral angles between the mean planes of the phenyl ring and the cyclohexyl ring are 40.29 (11 and 37.91 (13° in the two molecules.

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

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Flavien A. A. Toze

2011-11-01

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

Influence of bulky substituents on the regioselective group-transfer reactions of diorganozinc compounds with N,N'-bis(2,6-di-isopropylphenyl)-1,4-diaza-1,3-butadiene

NARCIS (Netherlands)

Koten, G. van; Wissing, E.; Gorp, K. van; Boersma, J.

1994-01-01

Diorganozinc compounds R{2}Zn (R=alkyl or aryl) react with N, N'-bis(2,6-di-isopropylphenyl)-1,4-diaza-1,3-butadiene, (i-Pr{2}Ph)N@?CHCHp@?N(i-Pr{2}Ph) (i-Pr{2}Ph-DAB) to give thermally unstable 1:1 coordination complexes R{2}Zn(i-Pr2Ph-DAB), which subsequently undergo a slow regioselective alkyl or

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

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Dun-Ru Zhu

2009-05-01

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

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.

N-[(1,3-Benzodioxol-5-ylmethyl]benzenesulfonamide: an analogue of capsaicin

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Stella H. Maganhi

2013-11-01

Full Text Available The title compound, C14H13NO4S, an analogue of capsaicin, differs from the latter by having a 1,3-benzodioxole ring rather than a 2-methoxyphenol moiety, and having a benzenesulfonamide group instead of an aliphatic amide chain. The five-membered ring is in an envelope conformation with the methylene C atom lying 0.221 (6 Å out of the plane formed by the other four atoms. The dihedral angle between the phenyl ring and the mean plane of the 1,3-benzodioxole fused-ring system is 84.65 (4°. In the crystal, molecules aggregate into supramolecular layers in the ac plane through C—H...O, N—H...O and C—H...π interactions.

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

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A. Gayathri

2017-12-01

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

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].

catena-Poly[[[dichloridozinc(II]-μ-1,4-bis(1H-benzimidazol-2-yl-κN3butane] 1,4-bis(1H-benzimidazol-2-ylbutane solvate

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Yan-Ling Zhou

2010-01-01

Full Text Available In the crystal structure of the title coordination polymer/co-crystal, {[ZnCl2(C18H18N4]·C18H18N4}n, the tetrahedrally coordinated ZnII ions are linked by the N-heterocycle into a linear chain. Another N-heterocycle present is not coordinated to the metal atom but interacts with the chain through N—H...N and N—H...Cl hydrogen bonds. The butyl chain of the uncoordinated ligand is disordered over three positions in a 0.511 (4:0.289 (5:0.200 (5 ratio.

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.

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.

(E-4-Bromo-N-(2,3-dimethoxybenzylideneaniline

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Karla Fejfarová

2010-09-01

Full Text Available The title Schiff base compound, C15H14BrNO2, was prepared by the condensation of 2,3-dimethoxybenzaldehyde with 4-bromoaniline. It adopts an E configuration with respect to the C=N bond. The dihedral angle between the two aromatic rings is 56.79 (8°. Weak C—H...O and C—-H...π bonds can be found in the crystal structure.

2-(3,5-Dimethyl-1H-pyrazol-1-yl-2-hydroxyimino-N′-[1-(pyridin-2-ylethylidene]acetohydrazide

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Maxym O. Plutenko

2012-12-01

Full Text Available In the title compound, C14H16N6O2, the dihedral angles formed by the mean plane of the acetohydrazide group [maximum deviation 0.0629 (12 Å] with the pyrazole and pyridine rings are 81.62 (6 and 38.38 (4° respectively. In the crystal, molecules are connected by N—H...O and O—H...N hydrogen bonds into supramolecular chains extending parallel to the c-axis direction.

1,3-Di-4-pyridylpropane–4,4′-oxydibenzoic acid (1/1

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Hirofumi Hinode

2008-12-01

Full Text Available The hydrothermal reaction of Cd(NO32·4H2O, 1,3-di-4-pyridylpropane (BPP and 4,4′-oxydibenzoic acid (OBA led to the formation of the title compound, C13H14N2·C14H10O5. The asymmetric unit consists of one molecule of OBA and one of BPP. In the OBA molecule, one COOH group is nearly planar with its attached benzene ring [dihedral angle = 0.9 (1°], while the other COOH group is slightly twisted with a dihedral angle of 10.8 (3°. The carboxyl groups form strong intermolecular O—H...N hydrogen bonds with N atoms of the pyridine rings in BPP, linking the molecules into zigzag chains.

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.

Synthesis, characterization, and anomalous dielectric and conductivity performance of one-dimensional (bdaH)InSe{sub 2} (bda = 1,4-butanediamine)

Energy Technology Data Exchange (ETDEWEB)

Du, Ke-Zhao; Hu, Wan-Biao [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Hu, Bing; Guan, Xiang-Feng [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Huang, Xiao-Ying, E-mail: xyhuang@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

2011-11-15

Graphical abstract: Anomalous dielectric and conductivity performance have been observed in the organic-containing indium selenide (bdaH)InSe{sub 2}, which are attributed to the water molecules existing in the crystal boundary rather than phase transition. Highlights: {yields} The title compound is the first example of organic-containing one-dimensional indium selenide. {yields} The anomalous dielectric peak is attributed to water molecules in crystal boundary. {yields} The inorganic and organic components of the title compound are connected via hydrogen bonding to form a supramolecular three-dimensional network. -- Abstract: A new indium selenide, namely (bdaH)InSe{sub 2} (1) (bda = 1,4-butanediamine) has been solvothermally synthesized and structurally characterized. It belongs to the non-centrosymmetric space group Fdd2. Its structure features an infinite one-dimensional anionic chain of [InSe{sub 2}]{sub n}{sup n-} with monoprotonated [bdaH]{sup +} as charge compensating cation. The organic [bdaH]{sup +} cations are joined into a supramolecular one-dimensional chain via N-H...N hydrogen bonding, which further interacts with the inorganic chain via N-H...Se and C-H...Se hydrogen bonding, forming a supramolecular three-dimensional network. Based on such a well-defined structure, the thermal stability, optical, conductivity, and dielectric properties were systematically investigated, showing that dielectric constant, as well as conductivity, had a hump at about 95 {sup o}C, which could be attributed to water molecules in the crystal boundary.

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

Science.gov (United States)

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

2007-10-01

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

Anti-inflammatory drugs. X. Hydrated pyrrolidinium [2-[(2,6-dichlorophenyl)amino]phenyl]acetate(HP.D.H2O).

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Castellari, C; Comelli, F; Ottani, S

2001-10-01

In the solid-state structure of the title compound, C(4)H(10)N(+).C(14)H(10)Cl(2)NO(2)(-).H(2)O, the asymmetric unit contains one cation, one anion and a water molecule. There is a network of hydrogen bonds which is similar to that found in the hydrated diethylammonium diclofenac salt. A comparison is made of the molecular conformation of the anions in the two related structures.

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.

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Synthesis of 14C- and 3H-labelled 4-(4-nitrophenyl)aminophenylisothiocyanate (Go 9333/CGP 4540; amoscanate)

International Nuclear Information System (INIS)

Anjaneyulu, B.; Maller, R.K.; Nagarajan, K.

1985-01-01

Amoscanate, a broad spectrum anthelmintic, labelled with carbon-14 on the isothiocyanate carbon atom was prepared in an overall yield of 13% at a specific activity of 4.13 μCi/mg from potassium [ 14 C]thiocyanate. The 4-nitro[U- 14 C]phenyl ring labelled compound was synthesized in 20.4% overall yield from [U- 14 C]aniline at a specific activity of 12.2 μCi/mg. The corresponding tritiated compound was prepared from 4-amino[2- 3 H]acetanilide at 112 μCi/mg. Labelling with tritium in the aromatic ring bearing the isothiocyanate group was achieved by catalysed halogen-tritium replacement. However, for pharmacokinetic and metabolism studies in experimental animals, the 14 C- and 3 H-labels associated with the phenylisothiocyanate moiety subsequently proved disadvantageous because of the instability of the labels in vivo. (author)

2D 1H -13C Heteronuclear Shift Correlation Of 2a - Hydroxy Aiantolactone From Pulicaria Undulata C.A. Mey

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A. Rustaiyan

1992-07-01

Full Text Available We have reported recently the isolation and characterization of several sesquiterpene lactones from Pulicaria undulata (1."nThe lactones were isolated from an Et20 - Petrol (1:3 fraction by different chromatographic techniques including HPLC (RP 8, MeOH - H2O, 13:7."nIn this way three eudesmanolides 1 - 3, a guaianolide 4, a nor -guaianolide 5, as well as the pseudoguaianolide 6 and the xanthanolide 7 were isolated. One of the eudesmanolides (2a - hydroxy aiantolactone, 1, was present as the main component."nSuch lactones being known as biologically active substances, we have decided to describe for the first time a detailed interpretation of proton, 1H -NMR, 13C - NMR and 2D lH -13C - heteronuclear shift correlation spectra of 2a - hydroxy aiantolactone. The stereochemistry of C - 2 , C - 7 and C - 8 was determined by the NOESY experiments, H - 7 and H - 8 are in the a configuration and H - 2 is in the b configuration.

Synthesis, crystal and supramolecular structure of rac-N-acetyl-2- thiohydantoin-asparagine

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Gerzon E. Delgado

2014-05-01

Full Text Available The title compound, C7H9N3O3S, also known as rac-N-acetyl-5-propionamide-2-thioxo-imidazolidin-4-one, crystallize in the monoclinic system with space group P21/n (Nº14, Z=4, and unit cell parameters a= 9.338 (7 Å, b= 7.545 (5 Å, c= 13.212 (10 Å, E= 97.10 (2°, V= 932.8 (12 Å3. The acetyl group and the mean plane of the ureido group form an angle of 81.0 (2°. In the supramolecular structure, the molecules are joined by N--H···O hydrogen bonds into cyclic structures with graph-set R2 2(14 and R2 2(16, forming a three-dimensional network.

Astrophysical S factor for 13C(p,γ)14N and asymptotic normalization coefficients

International Nuclear Information System (INIS)

Mukhamedzhanov, A.M.; Azhari, A.; Gagliardi, C.A.; Sattarov, A.; Tang, X.; Trache, L.; Tribble, R.E.; Burjan, V.; Kroha, V.

2002-01-01

We reanalyze the 13 C(p,γ) 14 N radiative capture reaction within the R-matrix approach. The low-energy astrophysical S factor has important contributions from both resonant and onresonant captures. The normalization of the nonresonant component of the transition to a particular 14 N bound state is expressed in terms of the asymptotic normalization coefficient (ANC). In the analysis we use the experimental ANC's inferred from the 13 C( 14 N, 13 C) 14 N and 13 C( 3 He,d) 14 N reactions. The fits of the calculated S factors to the experimental data are sensitive to the ANC values and are used to test the extracted ANC's. We find that for transitions to all the states in 14 N, except the third excited state, the ANC's determined from the transfer reactions provide the best fit. The astrophysical factor we obtain, S(0)=7.7±1.1 keV b, is in excellent agreement with previous results

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

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Gün Binzet

2011-05-01

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

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

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Gabriela Ledesma

2017-12-01

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

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

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Diwaker

2014-07-01

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

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.

N-(4-Methoxyphenyl-tert-butanesulfinamide

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Mrityunjoy Datta

2009-11-01

Full Text Available In the title compound, C11H17NO2S, the molecules interact head-to-tail through N—H...OS hydrogen bonds, giving discrete centrosymmetric cyclic dimers. The N—Caryl bond length [1.4225 (14 Å] is intermediate between that in N-phenyl-tert-butanesulfinamide [1.4083 (12 Å] and the N—Calkyl bond lengths in N-alkylalkanesulfinamides (1.470–1.530 Å, suggesting weaker delocalization of electrons over the N atom and the aromatic ring due to the presence of the 4-methoxy group.

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

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Augusto Rivera

2011-09-01

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

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

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Gene-Hsiang Lee

2006-03-01

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

N-(2-Chlorophenyl-2-({5-[4-(methylsulfanylbenzyl]-4-phenyl-4H-1,2,4-triazol-3-yl}sulfanylacetamide

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Hoong-Kun Fun

2011-08-01

Full Text Available In the title molecule, C24H21ClN4OS2, the central 1,2,4-triazole ring forms dihedral angles of 89.05 (9, 86.66 (9 and 82.70 (10° with the chloro-substituted benzene ring, the methylsulfanyl-substituted benzene ring and the phenyl ring, respectively. In the crystal, molecules are linked into sheets parallel to (100 by intermolecular N—H...N and weak C—H...O hydrogen bonds.

Preparation of 2H- and 13C-labelled precursors of 2-hydroxy-1, 3-butadiene

International Nuclear Information System (INIS)

Turecek, F.

1987-01-01

2-exo-Vinylbicyclo[2.2.1]hept-5-en-2-ols, specifically labelled with 2 H at C-3 and in the vinyl group were prepared from bicyclo[2.2.1]hept-5-en-2-one in several steps. [4- 13 C]oct-1-en-3-one was prepared in five steps from 13 CO 2 . These compounds serve as precursors for the preparation of specifically labelled neutral and ionized 2-hydroxy-1, 3-butadienes. (author)

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

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2009-03-01

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

13C, 1H spin-spin coupling constants. Pt. 4

International Nuclear Information System (INIS)

Aydin, R.; Guenther, H.

1979-01-01

One-bond, geminal, and vicinal 13 C, 1 H coupling constants have been determined for adamantane using α-and β-[D]adamantane and the relation sup(n)J( 13 C, 1 H)=6,5144sup(n)J( 13 C, 2 H) for the conversion of the measured sup(n)J( 13 C, 2 H) values. It is shown that the magnitude of 3 Jsub(trans) is strongly influenced by the substitution pattern. Relative H,D isotope effects for 13 C chemical shifts are given. (orig.) [de

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.

l-2-Nitrimino-1,3-diazepane-4-carboxylic acid monohydrate

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Harutyun A. Karapetyan

2008-07-01

Full Text Available The title compound, C6H10N4O4·H2O, crystallizes with two independent formula units in the asymmetric unit, their geometric parameters being quite similar. The conformations of the 1,3-diazepane rings are also similar and close to a twist-boat. All ten O- and N-bound H atoms are involved in hydrogen bonds, two of which are intra- and eight intermolecular linking crystallographically independent molecules, into a three-dimensional hydrogen-bonded network.

C-C bond formation and related reactions at the CNC backbone in (smif)FeX (smif = 1,3-di-(2-pyridyl)-2-azaallyl): dimerizations, 3 + 2 cyclization, and nucleophilic attack; transfer hydrogenations and alkyne trimerization (X = N(TMS)2, dpma = (di-(2-pyridyl-methyl)-amide)).

Science.gov (United States)

Frazier, Brenda A; Williams, Valerie A; Wolczanski, Peter T; Bart, Suzanne C; Meyer, Karsten; Cundari, Thomas R; Lobkovsky, Emil B

2013-03-18

Molecular orbital analysis depicts the CNC(nb) backbone of the smif (1,3-di-(2-pyridyl)-2-azaallyl) ligand as having singlet diradical and/or ionic character where electrophilic or nucleophilic attack is plausible. Reversible dimerization of (smif)Fe{N(SiMe3)2} (1) to [{(Me3Si)2N}Fe]2(μ-κ(3),κ(3)-N,py2-smif,smif) (2) may be construed as diradical coupling. A proton transfer within the backbone-methylated, and o-pyridine-methylated smif of putative ((b)Me2(o)Me2smif)FeN(SiMe3)2 (8) provides a route to [{(Me3Si)2N}Fe]2(μ-κ(4),κ(4)-N,py2,C-((b)Me,(b)CH2,(o)Me2(smif)H))2 (9). A 3 + 2 cyclization of ditolyl-acetylene occurs with 1, leading to the dimer [{2,5-di(pyridin-2-yl)-3,4-di-(p-tolyl-2,5-dihydropyrrol-1-ide)}FeN(SiMe3)2]2 (11), and the collateral discovery of alkyne cyclotrimerization led to a brief study that identified Fe(N(SiMe3)2(THF) as an effective catalyst. Nucleophilic attack by (smif)2Fe (13) on (t)BuNCO and (2,6-(i)Pr2C6H3)NCO afforded (RNHCO-smif)2Fe (14a, R = (t)Bu; 14b, 2,6-(i)PrC6H3). Calculations suggested that (dpma)2Fe (15) would favorably lose dihydrogen to afford (smif)2Fe (13). H2-transfer to alkynes, olefins, imines, PhN═NPh, and ketones was explored, but only stoichiometric reactions were affected. Some physical properties of the compounds were examined, and X-ray structural studies on several dinuclear species were conducted.

(4-Chloroacetanilido-κ2N,Obis[2-(pyridin-2-ylphenyl-κ2C1,N]iridium(III

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Lijun Sun

2013-02-01

Full Text Available In the neutral mononuclear iridium(III title compound, [Ir(C8H7ClNO(C11H8N2], the IrIII atom adopts an octahedral geometry, and is coordinated by two 2-phenylpyridyl ligands and one anionic 4-chloroacetanilide ligand. The 2-phenylpyridyl ligands are arranged in a cis-C,C′ and cis-N,N′ fashion. Each 2-phenylpyridyl ligand forms a five-membered ring with the IrIII atom. The 2-phenylpyridyl planes are perpendicular to each other [dihedral angle = 89.9 (1°]. The Ir—C and Ir—N bond lengths are comparable to those reported for related iridium(III 2-phenylpyridyl complexes. The remaining two coordination sites are occupied by the amidate N and O atoms, which form a four-membered ring with the iridium atom (Ir—N—C—O. The amidate plane is nearly perpendicular to both 2-phenylpyridyl ligands [dihedral angles = 87.8 (2 and 88.3 (2°].

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

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Samra Rahmouni

2016-05-01

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

2-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.

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.

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.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

4-Aminobenzoic acid–4,4′-(propane-1,3-diyldipyridine (1/1

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Fwu Ming Shen

2010-11-01

Full Text Available In the crystal structure of the title compound, C13H14N2·C7H7NO2, the 4,4′-trimethylene-dipyridine (TMDP molecule displays an approximately planar structure, the maximum atomic deviation excluding H atoms being 0.118 (2 Å and the dihedral angle between the pyridine rings 4.59 (10°. The TMDP and 4-aminobenzoic acid (ABA molecules are linked by O—H...N and N—H...N hydrogen bonding, while ABA molecules are linked by O—H...O hydrogen bonding. C—H...π interactions are also observed between the methylene groups of TMDP molecules and the benzene rings of ABA molecules.

N-Phenylmorpholine-4-carboxamide

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Yong Guo

2011-01-01

Full Text Available In the title compound, C11H14N2O2, the urea-type NC=ON moiety [planar to within 0.0002 (13 Å] is inclined to the phenyl ring by 42.88 (8 Å, and the morpholine ring has a chair conformation. In the crystal, intermolecular N—H...O hydrogen bonds link the molecules into infinite chains in [001].

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

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Quanying Gan

2010-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-01-15

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

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

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Michal Dušek

2010-10-01

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

Rubidium 2,4,6-trioxo-1,3-diazinan-5-ide–1,3-diazinane-2,4,6-trione–water (1/1/1

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Marlena Gryl

2011-05-01

Full Text Available The asymmetric unit of the title compound, Rb+·C4H3N2O3−·C4H4N2O3·H2O, consists of one rubidium cation, a barbituric acid molecule, a barbiturate anion and one water molecule. The rubidium ion has seven close-contact interactions with O atoms, with Rb...O distances ranging from 2.8594 (16 to 3.2641 (14 Å. These seven O atoms together with an eighth O atom at 3.492 (2 Å away from Rb form a distorted polyhedron with shape intermediate between an antiprism and a dodecahedron. The Rb+ ions connect layers built of organic components and water molecules linked via N—H...O and O—H...O hydrogen bonds.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-01

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

N-{4-[(2E-3-(2H-1,3-Benzodioxol-5-ylprop-2-enoyl]phenyl}quinoline-3-carboxamide

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Efrain Polo

2017-10-01

Full Text Available An amide chalconehas been synthesized in a two-step reaction. First, N-(4-acetylphenylquinoline-3-carboxamide 2 was synthesized by the reaction of quinoline-3-carboxylic acid 1 and thionyl chloride (SOCl2, following the addition of 4-aminoacetophenone. Then, a typical Claisen–Schmidtreactionwas made between 2 and piperonal using KOH solution as a catalystin ethanol, under ultrasonic irradiation. The structure of the target compound was established by FTIR (Fourier-transform infrared spectroscopy, HRMS, 1H and 13C-NMR.

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

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Laila El Foujji

2018-04-01

Full Text Available In the title compound, C16H20N2O2, the seven-membered ring adopts a bowl-shaped conformation while the orientation of the 2-oxopropylidene substituent is determined by an intramolecular N—H...O hydrogen bond, which generates an S(6 ring. In the crystal, inversion dimers linked by pairs of very weak C—H...O interactions occur, which generate R22(8 loops.

Poly[[μ2-2,2′-diethyl-1,1′-(butane-1,4-diyldiimidazole-κ2N3:N3′](μ2-5-hydroxyisophthalato-κ2O1:O3zinc

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Ying-Ying Liu

2011-11-01

Full Text Available In the title coordination polymer, [Zn(C8H4O5(C14H22N4]n, the ZnII cation is coordinated by an O2N2 donor set in a distorted tetrahedral geometry. The ZnII ions are linked by μ2-OH-bdc (OH-H2bdc = 5-hydroxyisophthalic acid and bbie ligands [bbie = 2,2′-diethyl-1,1′-(butane-1,4-diyldiimidazole], forming a two-dimensional layer parallel to the ab plane. The layers are further connected through intermolecular C—H...O and O—H...O hydrogen bonds, forming a three-dimensional supramolecular structure. In the bbie ligand, the two C atoms in the ethyl group are each disordered over two positions with a site-occupancy ratio of 0.69:0.31.

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

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Yan Jiang

2012-02-01

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

Hexaaquacopper(II bis(tetrafluoridoborate–pyrazine 1,4-dioxide (1/3

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Jan L. Wikaira

2013-04-01

Full Text Available The crystal structure of the title compound, [Cu(H2O6](BF42·3C4H4N2O2, comprises discrete [Cu(H2O6]2+ cations and BF4− anions along with three equivalents of pyrazine 1,4-dioxide (pzdo. The hexaaquacopper(II ion and all three pzdo molecules lie about crystallographic inversion centers. The lattice is supported by an extensive hydrogen-bonding network. O—H...O hydrogen bonding between the [Cu(H2O6]2+ and pzdo units creates a pseudo-hexagonal lattice parallel to the bc plane. The BF4− anions lie in the voids of that lattice, held in place by O—H...F hydrogen bonds, and also generate BF4−–pzdo–BF4−–pzdo stacks via short F...N contacts [2.866 (3–3.283 (4 Å].

Synthesis of deleobuvir, a potent hepatitis C virus polymerase inhibitor, and its major metabolites labeled with carbon-13 and carbon-14.

Science.gov (United States)

Latli, Bachir; Hrapchak, Matt; Chevliakov, Maxim; Li, Guisheng; Campbell, Scot; Busacca, Carl A; Senanayake, Chris H

2015-05-30

Deleobuvir, (2E)-3-(2-{1-[2-(5-bromopyrimidin-2-yl)-3-cyclopentyl-1-methyl-1H-indole-6-carboxamido]cyclobutyl}-1-methyl-1H-benzimidazol-6-yl)prop-2-enoic acid (1), is a non-nucleoside, potent, and selective inhibitor of hepatitis C virus NS5B polymerase. Herein, we describe the detailed synthesis of this compound labeled with carbon-13 and carbon-14. The synthesis of its three major metabolites, namely, the reduced double bond metabolite (2) and the acyl glucuronide derivatives of (1) and (2), is also reported. Aniline-(13) C6 was the starting material to prepare butyl (E)-3-(3-methylamino-4-nitrophenyl-(13) C6 )acrylate [(13) C6 ]-(11) in six steps. This intermediate was then used to obtain [(13) C6 ]-(1) and [(13) C6 ]-(2) in five and four more steps, respectively. For the radioactive synthesis, potassium cyanide-(14) C was used to prepare 1-cylobutylaminoacid [(14) C]-(23) via Buchrer-Bergs reaction. The carbonyl chloride of this acid was then used to access both [(14) C]-(1) and [(14) C]-(2) in four steps. The acyl glucuronide derivatives [(13) C6 ]-(3), [(13) C6 ]-(4) and [(14) C]-(3) were synthesized in three steps from the acids [(13) C6 ]-(1), [(13) C6 ]-(2) and [(14) C]-(1) using known procedures. Copyright © 2015 John Wiley & Sons, Ltd.

A study of the 10, 11B(p,n)10, 11C reactions between Ep=13,7 and 14,7 MeV

International Nuclear Information System (INIS)

Schelin, H.R.

1985-01-01

Using time-of-flight facilities of the Sao Paulo 8UD Pelletron Accelerator, absolute differential cross sections for the n 0 , n 1 , n 2 , n 3 , (n 4 +n 5 ), n 6 and n 7 groups for the reaction 11 B(p,n) 11 C and the n 0 and n 1 neutron groups for the reaction 10 B(p,n) 10 C have been measured at incident proton energies of 14.0, 14.3 and 14.6 MeV in the angular interval of 20 to 160 degrees. Excitation functions at θ lab =20 deg from Ep=13.7 to 14.7 MeV in intervals of 100 KeV were also measured. The theoretical analysis was conducted to determine relative contributions of the diret and compound nucleus processes in the differential cross sections. To this end, a two couple channel model model for the reactions was assumed. The DWBA model for the direct and the Hauser-Feshbch for the compound nucleus processes were in such a way as to simulate the exact coupled channels calculation through an appropriate choice of the absorption term W in the optical potential. The results indicate that about half of the cross section is due to the compound nucleus mechanism. The theoretical analysis aimed at obtaining the elastic enhancement factor for the channel 11 B(p,n 0 ) 11 C at Ep=14.3 MeV. This has been demonstrated to appear in compound nucleus charge reactions by Harney, Weidemueller and Richter and predicted to attain the value 2 when isospin is conserved. Our results show an enhancement factor larger than 1 indicating that isospin mixing is weak in this reaction. (Author) [pt

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

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Abdellah N'ait Ousidi

2016-03-01

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

Production of N-13 labeled compounds with high specific activity

Energy Technology Data Exchange (ETDEWEB)

Suzuki, Kazutoshi; Sasaki, Motoji; Yoshida, Yuichiro; Haradahira, Terushi; Inoue, Osamu [National Inst. of Radiological Sciences, Chiba (Japan)

1997-03-01

Nitrogen-13 was produced by irradiating ultra pure water saturated with a pure gas (N2, O2, He, H2) with 18 MeV protons. Ion species generated by irradiation were analyzed with radio ion chromatography systems. An automated equipment was developed to synthesize anhydrous (13N)NH3 as a synthetic precursor and (13N)p-nitrophenyl carbamate ((13N)NPC) as a model compound, using the (13N)NH3. The radiochemical yield and specific activity of (13N)NPC was high enough to carry out the receptor study with PET. (author)

Aqua[bis(2-ethyl-5-methyl-1H-imidazol-4-yl-κN3methane]oxalatocopper(II dihydrate

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Yang-Hui Luo

2011-02-01

Full Text Available In the title compound, [Cu(C2O4(C13H20N4(H2O]·2H2O, the CuII atom exhibits a distorted square-pyramidal geometry with the two N atoms of the imidazole ligand and the two O atoms of the oxalate ligand forming the basal plane, while the O atom of the coordinated water molecule is in an apical position. The CuII atom is shifted 0.232 (2 Å out of the basal plane toward the water molecule. The asymmetric unit is completed by two solvent water molecules. These water molecules participate in the formation of an intricate three-dimensionnal network of hydrogen bonds involving the coordinated water molecule and the NH groups.

5-[3-(2,5-Dimethoxyphenylprop-2-enylidene]-1,3-diethyl-2-thioxohexahydropyrimidine-4,6-dione

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Abdullah Mohamed Asiri

2009-08-01

Full Text Available 1,3-Diethyl-2-thiobarbituric acid reacts with 2,5-dimethoxybenzaldehyde to form the title Knoevenagel product, C19H22N2O4S. In the compound, the two six-membered rings at either end of the three-membered –CHCHCH– chain are nearly coplanar with this fragment (r.m.s. deviation of the two six-membered rings and the three chain atoms = 0.08 Å.

Tris(2,2′-bipyridine-κ2 N,N′)cobalt(III) bis­[bis­(pyridine-2,6-dicarboxyl­ato-κ3 O 2,N,O 6)cobaltate(III)] perchlorate dimethyl­formamide hemisolvate 1.3-hydrate

Science.gov (United States)

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

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

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Tuncer Hökelek

2008-10-01

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

Dimethyl (E-2-(N-phenylacetamidobut-2-enedioate

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Ting Bin Wen

2011-01-01

Full Text Available The title compound, C14H15NO5, was obtained from the reaction of acetanilide with dimethyl acetylenedicarboxylate in the presence of potassium carbonate. The C=C double bond adopts an E configuration and the geometry around the amide N atom is almost planar rather than pyramidal (mean deviation of 0.0032 Å from the C3N plane. The packing of the molecules in the crystal structure is stabilized by intermolecular C—H...O hydrogen bonds.

Three closely related (2E,2′E-3,3′-(1,4-phenylenebis[1-(methoxyphenylprop-2-en-1-ones]: supramolecular assemblies in one dimension mediated by hydrogen bonding and C—H...π interactions

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Aijia Sim

2017-06-01

Full Text Available In the title compounds, (2E,2′E-3,3′-(1,4-phenylenebis[1-(2-methoxyphenylprop-2-en-1-one], C26H22O4 (I, (2E,2′E-3,3′-(1,4-phenylenebis[1-(3-methoxyphenylprop-2-en-1-one], C26H22O4 (II and (2E,2′E-3,3′-(1,4-phenylenebis[1-(3,4-dimethoxyphenylprop-2-en-1-one], C28H26O6 (III, the asymmetric unit consists of a half-molecule, completed by crystallographic inversion symmetry. The dihedral angles between the central and terminal benzene rings are 56.98 (8, 7.74 (7 and 7.73 (7° for (I, (II and (III, respectively. In the crystal of (I, molecules are linked by pairs of C—H...π interactions into chains running parallel to [101]. The packing for (II and (III, features inversion dimers linked by pairs of C—H...O hydrogen bonds, forming R22(16 and R22(14 ring motifs, respectively, as parts of [201] and [101] chains, respectively.

1-(4-Bromobenzoyl-2-phenylpyrrolidine-2-carboxamide

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Vahan Martirosyan

2008-03-01

Full Text Available In the title compound, C18H17BrN2O2, which is a potential human immunodeficiency virus type 1 (HIV-1 non-nucleoside reverse transcriptase inhibitor, the pyrrolidine ring exhibits an envelope conformation. In the crystal structure, intermolecular N—H...O hydrogen bonds [N...O = 2.861 (3 Å] link the molecules into centrosymmetric dimers.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-03-15

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

2,4,8,10,13-Pentamethyl-6-phenyl-13,14-dihydro-12H-6λ5-dibenzo[d,i][1,3,7,2]dioxazaphosphecin-6-thione

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M. Krishnaiah

2010-01-01

Full Text Available In the title compound, C25H28NO2PS, the cyclodecene ring exhibits a crown conformation. The two dimethylbenzene rings which are fused symmetrically on either side of the ten-membered ring, make dihedral angles of 20.2 (1 and 18.0 (1°. The phenyl ring substituted at P is perpendicular to the heterocyclic ring, making a dihedral angle of 88.4 (1°. The crystal structure is stabilized by very weak intramolecular C—H...O hydrogen bonding.

CORRELATION ANALYSIS OF IR, 1 H- AND 13 C-NMR SPECTRAL DATA OF N-ALKYL AND N-CYCLOALKYL CYANOACETAMIDES

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Aleksandar D. Marinković

2011-09-01

Full Text Available Linear free energy relationships (LFER were applied to the IR, 1H- and 13C--NMR spectral data in N-alkyl and N-cycloalkyl cyanoacetamides. N-alkyl and N-cycloalkyl cyanocetamides were synthesized from corresponding amine and ethyl cyanoacetate. A number of substituents were employed for alkyl substitution, and fairly good correlations were obtained, using simple Hammett equation. In N-alkyl and N-cycloalkyl cyanoacetamides substituent cause SCS of N-H hydrogen primarily by steric interaction, polar subtituent effect influences SCS shift of C=O carbon, while steric effect of N-alkyl substituent causes IR stretching frequencies of N-H, C=O and CN group. The conformations of investigated compounds have been studied by the use of semiempirical PM6 method, and together with LFER analysis, give a better insight into the influence of such a structure on the transmission of electronic substituent effects. Negative ρ values for several correlations (reverse substituent effect were found.

14C2H4: distribution of 14C-labeled tissue metabolites in pea seedlings

International Nuclear Information System (INIS)

Giaquinta, R.; Beyer, E. Jr.

1977-01-01

The 14 C-metabolite distribution pattern following 14 C 2 H 4 metabolism in intact pea seedlings (Pisum sativum L.) was determined under various conditions. After a 24 hr exposure to 14 C 2 H 4 , the majority of 14 C-metabolites were water-soluble (60-70%) with lesser amounts in the protein (10-15%), lipid (1%), and insoluble (1-2%) fractions. Ion exchange chromatography of the water-soluble components into basic, neutral, and acidic fractions revealed a 50:40:10 distribution, respectively. Chromatography of the neutral fraction revealed two regions of radioactivity (Rf=0.38) and 0.63 which did not cochromatograph with twenty-two known sugars or neutral metabolites. Chromatograms of the basic fraction contained 3 regions of radioactivity. Similar distribution patterns were noted when 14 C 2 H 4 exposure was followed by a 6 hr air chase or when 5% CO 2 , an antagonist of ethylene action, was present during the exposure. Marked differences in the 14 C-metabolite distribution patterns were obtained when 14 CO 2 was substituted for 14 C 2 H 4 . These results indicate that the metabolic pathway involved in ethylene metabolism is different from that involved in intermediately carbon metabolism. (auth.)

Bromidotetra?kis?(1H-2-ethyl-5-methyl?imidazole-?N 3)copper(II) bromide

OpenAIRE

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 ...

Poly[propane-1,3-diammonium [cuprate(II-bis(μ2-pyridine-2,3-dicarboxylato] trihydrate

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Shabnam Hooshmand

2008-02-01

Full Text Available The title polymeric compound {(C3H12N2[Cu(C7H3NO42]·3H2O}n or {(pnH2[Cu(py-2,3-dc2]·3H2O}n (pn is propane-1,3-diamine and py-2,3-dcH2 is pyridine-2,3-dicarboxylic acid, was synthesized by reaction of copper(II chloride dihydrate with a proton-transfer compound, propane-1,3-diammonium pyridine-2,3-dicarboxylate or (pnH2(py-2,3-dc, in aqueous solution. The anion is a six-coordinate complex (site symmetry overline{1}, with a distorted octahedral geometry around CuII, consisting of two bidentate pyridine-2,3-dicarboxylate groups and two O atoms of bridging ligands from (py-2,3-dc2− fragments, which are located in trans positions. The (pnH22+ cation is disordered over two sites by the center of inversion. Intermolecular hydrogen bonds, π–π [centroid–centroid distances of 3.539 (3 Å] and C—O...π stacking interactions [O...Cg = 3.240 (5 Å; Cg is the center of the pyridine ring], connect the various components into a supramolecular structure.

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

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Youssef Ramli

2018-03-01

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

(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.

{2-[(3,5-Dichloro-2-oxidobenzylideneamino-κ2N,O]-3-methylpentanoato-κO}(N,N′-dimethylformamide-κOcopper(II

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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.

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

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Mehmet Akkurt

2010-08-01

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

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

International Nuclear Information System (INIS)

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

1986-01-01

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

Solvent-Mediated Synthesis of M(II-Coordination Polymer Part 1: Crystal Structure of Poly(1,2-di(4-pyridylethylene-k2N,N'-bis(1,4-benzenediacetato-k4O,O′,O′′,O′′'zinc(II], C22H18ZnN2O4

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Stephen Adie Adalikwu

2017-08-01

Full Text Available An interaction of water-methanol solution of sodium1,4-benzenediacetate (bda and 4,4′-bipyridylethelene (bpee with aqueous solution of Zn(NO32·6H2O at room temperature yielded colourless crystals of 1 after three weeks in a sealed glass tube. The compound with composition C22H18ZnN2O4 crystallizes in monoclinic space group P21/c, with the following cell dimensions: a = 10.4566(2, b = 13.3085(2, c = 13.7189(2 Å, β = 101.491(1°. In the structure of 1, two Zn(II neighbours are connected by two bda ligands adopting chelating and bidentate-bridging coordination modes to form a dimeric unit (Zn2O8N4 with the Zn–Zn distance of 4.0432(6 Å. The carboxyl-bridged dimeric units are extended along the [001] direction by bpee co-ligands and further linked by bda ligand to form a three-dimensional network structure. The IR shows the characteristic bands of the carboxylates at 1611/1507 cm−1 and 1424/1373 cm−1, respectively, for asymmetric and symmetric stretching −CO2− vibrations. The separation ∆[νasym(CO2− − νsym(CO2−] values of 187 and 134 cm−1 are indicative of chelating and bidentate bridging coordination modes of the carboxylate to the metal centre.

Synthesis of /sup 14/C- and /sup 3/H-labelled 4-(4-nitrophenyl)aminophenylisothiocyanate (Go 9333/CGP 4540; amoscanate)

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Anjaneyulu, B.; Maller, R.K.; Nagarajan, K. (Hindustan Ciba-Geigy Ltd., Bombay (India). Isotope Lab.); Kueng, W.; Wirz, B. (Ciba-Geigy A.G., Basel (Switzerland))

1985-04-01

Amoscanate, a broad spectrum anthelmintic, labelled with carbon-14 on the isothiocyanate carbon atom was prepared in an overall yield of 13% at a specific activity of 4.13 ..mu..Ci/mg from potassium (/sup 14/C)thiocyanate. The 4-nitro(U-/sup 14/C)phenyl ring labelled compound was synthesized in 20.4% overall yield from (U-/sup 14/C)aniline at a specific activity of 12.2 ..mu..Ci/mg. The corresponding tritiated compound was prepared from 4-amino(2-/sup 3/H)acetanilide at 112 ..mu..Ci/mg. Labelling with tritium in the aromatic ring bearing the isothiocyanate group was achieved by catalysed halogen-tritium replacement. However, for pharmacokinetic and metabolism studies in experimental animals, the /sup 14/C- and /sup 3/H-labels associated with the phenylisothiocyanate moiety subsequently proved disadvantageous because of the instability of the labels in vivo.

2-(2-Hydroxy-3-methoxyphenyl-1H-benzimidazol-3-ium perchlorate

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Chuan Chen

2012-06-01

Full Text Available In the title molecular salt, C14H13N2O2+·ClO4−, the ring systems in the cation are almost coplanar [dihedral angle = 5.53 (13°]. Intramolecular N—H...O and O—H...O hydrogen bonds generate S(6 and S(5 rings, respectively. In the crystal, the two H atoms involved in the intramolecular hydrogen bonds also participate in intermolecular links to acceptor O atoms of the perchlorate anions. A simple intermolecular N—H...O bond also occurs. Together, these form a double-chain structure along [101].

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.

Poly[(μ4-biphenyl-3,3′-dicarboxylatobis[μ2-1,1′-(butane-1,4-diyldiimidazole](μ2-oxalatodimanganese(II

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Bao-Yong Zhu

2010-10-01

Full Text Available In the title coordination compound, [Mn2(C14H8O4(C2O4(C10H14N42]n, the biphenyl-3,3′-dicarboxylate and oxalate anions, both situated on inversion centres, function in a bridging mode, linking the dinuclear MnII atoms into wave-like layers. Each 1,1′-(1,4-butane-1,4-diyldiimidazole ligand coordinates to two MnII atoms located in adjacent layers via Mn—N coordination bonds, giving a three-dimensional network. As the methylene groups can bend freely relative to each other due to the C atoms connected via single bonds, the 1,1′-(butane-1,4-diyldiimidazole ligand forms an S-shaped conformation, which makes the void in the three-dimensional network distorted.

Structure of 14C via elastic and inelastic neutron scattering from 13C: Measurement, R-matrix analysis, and shell model calculations

International Nuclear Information System (INIS)

Resler, D.A.

1987-03-01

The specific purpose of this work is to provide a better understanding of the 14 C level structure; the general purpose is to provide the details for using shell model calculations in R-matrix analyses. Using the TOF facilities of the Ohio University Accelerator Laboratory, the elastic and first 3 inelastic differential scattering cross sections for 13 C + n were measured at 69 energies for 4.5 ≤ E/sub n/ ≤ 11 MeV. A multiple scattering code was developed which provided a simulation of the experimental scattering process allowing accurate corrections to the small inelastic data. The integrated 13 C(n,α) 10 Be cross section is estimated. The sequential 2n-decay of 14 C states populated by 13 C + n was observed. A shell model code was developed. Normal and nonnormal parity calculations were made for the lithium isotopes using a new two-body interaction. The results for 5 Li predict the 2s/sub 1/2/ and 1d/sub 5/2/ single-particle states to be located below the 3/2 + state. Similar calculations were made for 13 C, 13 N, and 14 C. Results for 13 C and 13 N show for E/sub x/ 7 Li and 14 C, 2 h-barω calculations were done. Shell model calculations generated the R-matrix parameters for the elastic and first 3 inelastic channels of 13 C + n. After adjusting some energies, the predicted structure generally agrees with experiment for E/sub n/ 13 C + n data were refit to replace R 0 background terms by more realistic broad states and to get better agreement with model calculations. R-matrix fitting of the full data set produced new 14 C level information. For E/sub n/ > 4 MeV (E/sub x/ > 12 MeV), 5 states are given definite J/sup π/ assignments; 3, tentative assignments. 122 refs., 91 figs., 30 tabs

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.

Solid-state NMR detection of 14N-13C dipolar couplings between amino acid side groups provides constraints on amyloid fibril architecture.

Science.gov (United States)

Middleton, David A

2011-02-01

Solid-state nuclear magnetic resonance (SSNMR) is a powerful technique for the structural analysis of amyloid fibrils. With suitable isotope labelling patterns, SSNMR can provide constraints on the secondary structure, alignment and registration of β-strands within amyloid fibrils and identify the tertiary and quaternary contacts defining the packing of the β-sheet layers. Detection of (14)N-(13)C dipolar couplings may provide potentially useful additional structural constraints on β-sheet packing within amyloid fibrils but has not until now been exploited for this purpose. Here a frequency-selective, transfer of population in double resonance SSNMR experiment is used to detect a weak (14)N-(13)C dipolar coupling in amyloid-like fibrils of the peptide H(2)N-SNNFGAILSS-COOH, which was uniformly (13)C and (15)N labelled across the four C-terminal amino acids. The (14)N-(13)C interatomic distance between leucine and asparagine side groups is constrained between 2.4 and 3.8 Å, which allows current structural models of the β-spine arrangement within the fibrils to be refined. This procedure could be useful for the general structural analysis of other proteins in condensed phases and environments, such as biological membranes. Copyright © 2011 John Wiley & Sons, Ltd.

2,2′-{1,1′-[Butane-1,4-diylbis(oxynitrilo]diethylidyne}di-1-naphthol

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Wen-Kui Dong

2009-06-01

Full Text Available The title compound, C28H28N2O4, was synthesized by the reaction of 2-acetyl-1-naphthol with 1,4-bis(aminooxybutane in ethanol. The molecule, which lies about an inversion centre, adopts a linear structure, in which the oxime groups and naphthalene ring systems assume an anti conformation. The intramolecular interplanar distance between parallel naphthalene rings is 1.054 (3 Å. Intramolecular O—H...N hydrogen bonds are formed between the oxime nitrogen and hydroxy groups.

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

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

2017-12-01

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆F₂N₄S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆ClFN₄S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group$P\\bar 1$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) ųof compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) ųof compound (2). Structural analyses reveal that the title compounds are isostructural.