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

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Krzysztof Lyczko

2013-01-01

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

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

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Zilu Chen

2008-09-01

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

Clean to dirty limit and T c suppression in NdFeAsO0.7F0.3 studied by H c2 analysis

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Pallecchi, I.; Tarantini, C.; Shen, Y.; Singh, R. K.; Newman, N.; Cheng, P.; Jia, Y.; Wen, H.-H.; Putti, M.

2018-07-01

In this work, we investigate the temperature dependence of the upper critical field, dH c2/dT, in an increasingly disordered NdFeAsO0.7F0.3 (NdFeAs(O,F)) single crystal that has been progressively irradiated up to a 5.25 × 1016 cm- 2 total α-particle dose. For the H∣∣ab-plane, dH c2/dT does not vary remarkably with irradiation, while for the H∣∣c-axis it increases sharply after the first irradiation of 3.60 × 1015 cm-2 and then more gradually with further irradiation doses. Focusing on the H∣∣c-axis, we develop a phenomenological analysis of the H c2 slope which allows us to inspect the crossover from the clean to the dirty regime. From the H c2 slope normalized to the critical temperature and to its clean limit value, we extract the ratio of the coherence length ξ BCS to the mean free path {\\ell } and we find that when T c is reduced by a factor of four from its pristine value, ξ BCS/{\\ell } becomes as large as ˜7 and {\\ell } reaches values of ˜1.8 nm, indicating that NdFeAs(O,F) is well into the dirty regime. Our analysis of the H c2 slope also allows us to compare the pair-breaking effectiveness of scattering in different superconductors, showing similarity between unconventional NdFeAs(O,F) and moderate-T c phonon-mediated devices, such as MgB2 and A15 compounds, but much a stronger difference with YBa2Cu3O7-δ . This work thus shows that dH c2/dT is a reliable parameter, providing an alternative to residual resistivity, for investigating the pair-breaking mechanism induced by impurity scattering in superconductors.

Tris(dibenzoylmethanido-κ2O,O′[(6S,8S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-κ2N,N′]gadolinium(III

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Xi-Li Li

2009-09-01

Full Text Available In the title compound, [Gd(C15H11O23(C17H18N2], the GdIII atom is coordinated by six O atoms from three β-diketonate ligands and two N atoms from a chiral ligand LS,S-(+-7,7-dimethyl-3-(2-pyridyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline, in a coordination geometry best described as distorted square-antiprismatic.

(3-Benzoyl-1,7,7-trimethylbicyclo[2.2.1]heptan-2-olato-κ2O,Obis[2-(2-pyridylphenyl-κ2C1,N]iridium(III

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Kaijun Luo

2011-11-01

Full Text Available The title compound, [Ir(C11H8N2(C17H19O2], has an octahedral coordination geometry around the IrIII atom, retaining the cis-C,C,trans–N,N chelate disposition of the two 2-phenylpyridine ligands. The chelate rings are nearly mutually perpendicular [the interplanar angles range from 85.48 (17 to 89.17 (19°]. The two 2-(2-pyridylphenyl ligands are approximately planar, with the plane of the phenyl ring being inclined to that of the pyridine ring by 2.3 (3 and 5.1 (3° in the two ligands. The interplanar angle between the phenyl ring in 3-benzoyl-camphor and the IrO2C3 chelate ring is 35.5 (2°.

[2,6-Difluoro-3-(pyridin-2-yl-κNpyridin-4-yl-κC4](pentane-2,4-dionato-κ2O,O′iridium(III

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Kaijun Luo

2013-11-01

Full Text Available The title compound, [Ir(C10H5F2N22(C5H7O2], has a distorted octahedral coordination geometry around the IrIII atom, retaining the cis-C,C/trans-N,N chelate disposition in two 2,6-difluoro-3-(pyridin-2-yl-κNpyridin-4-yl ligands which are nearly mutually perpendicular [dihedral angle = 82.75 (15°]. The molecular structure is stabilized by weak C—H...O and C—H...F hydrogen-bond interactions. The crystal structure is stabilized by π–π stacking interactions (centroid–centroid distance = 3.951 Å.

Molecular and crystal structure of nido-9-C5H5N-11-I-7,8-C2B9H10: supramolecular architecture via hydrogen bonding X-H...I (X = B, C)

International Nuclear Information System (INIS)

Polyanskaya, T.M.

2006-01-01

A monocrystal X-ray diffraction study of a new iodine-containing cluster compound 9-(pyridine)-11-iodo-decahydro-7,8-dicarba-nido-undecaborane [9-C 5 H 5 N-11-I-7,8-C 2 B 9 H 10 ] has been performed. Crystal data: C 7 H 15 B 9 NI, M = 337.39, monoclinic, space group P2 1 /c, unit cell parameters: a=9.348(1) A, b=11.159(1) A, c=13.442(2) A, β=98.13(1) deg, V=1388.1(5) A 3 , Z=4, d calc = 1.614 g/cm 3 , T = 295 K, F(000)=648, μ=2.276 mm -1 . The structure was solved by a direct method and refined in the full-matrix anisotropic approximation (isotropic for hydrogen atoms) to final agreement factors R 1 = 0.0254, wR 2 = 0.0454 for 2437 I hkl >2σ I from 3590 measured I hkl (an Enraf-Nonius CAD-4 diffractometer, λMoK α , graphite monochromator, θ/2θ-scanning). The molecules are joined into a supramolecular assembly by hydrogen bonds X-H...I (X = B, C) [ru

Propane-1,2-diammonium bis(pyridine-2,6-dicarboxylato-κ3O,N,O′nickelate(II tetrahydrate

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Mohammad Ghadermazi

2008-07-01

Full Text Available The reaction of nickel(II nitrate hexahydrate, propane-1,2-diamine and pyridine-2,6-dicarboxylic acid in a 1:2:2 molar ratio in aqueous solution resulted in the formation of the title compound, (C3H12N2[Ni(C7H3NO42]·4H2O or (p-1,2-daH2[Ni(pydc2]·4H2O (where p-1,2-da is propane-1,2-diamine and pydcH2 is pyridine-2,6-dicarboxylic acid. The geometry of the resulting NiN2O4 coordination can be described as distorted octahedral. Considerable C=O...π stacking interactions are observed between the carboxylate C=O groups and the pyridine rings of the (pydc2− fragments, with O...π distances of 3.1563 (12 and 3.2523 (12 Å and C=O...π angles of 95.14 (8 and 94.64 (8°. In the crystal structure, a wide range of non-covalent interactions, consisting of hydrogen bonding [O—H...O, N—H...O and C—H...O, with D...A distances ranging from 2.712 (2 to 3.484 (2 Å], ion pairing, π–π [centroid-to-centroid distance = 3.4825 (8 Å] and C=O...π stacking, connect the various components to form a supramolecular structure.

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

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Tara Shahani

2010-01-01

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

Synthesis and crystal structure of a new neodymium(III) selenate-selenite: Nd2(SeO4)(SeO3)2(H2O)2

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Feng Meiling; Mao Jianggao

2005-01-01

The title new neodymium(III) selenate-selenite was obtained by hydrothermal reactions of neodymium(III) oxide, H 2 SeO 4 and 1,10-phenanthroline at 140 o C. Its structure was established by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group C2/c with cell parameters of a = 12.258(2) A, b 7.1024(15) A, c = 13.391(3) A, β = 104.250(2) o . The structure of Nd 2 (SeO 4 )(SeO 3 ) 2 (H 2 O) 2 is isomorphous with that of Er 2 (SeO 4 )(SeO 3 ) 2 (H 2 O) 2 , which was refined in the monoclinic space group C2 with the disordered selenate group. It features an ordered 3D network with channels along b-axis. The selenate or selenite groups alone can form a 2D layer with the Nd(III) ions. IR spectrum, TGA and luminescent studies have also been performed

(Carbonato-κ(2)O,O')bis-(5,5'-dimethyl-2,2'-bipyridyl-κ(2)N,N')cobalt(III) bromide trihydrate.

Science.gov (United States)

Arun Kumar, Kannan; Meera, Parthsarathi; Amutha Selvi, Madhavan; Dayalan, Arunachalam

2012-04-01

In the title complex, [Co(CO(3))(C(12)H(12)N(2))(2)]Br·3H(2)O, the Co(III) cation has a distorted octa-hedral coordination environment. It is chelated by four N atoms of two different 5,5'-dimethyl-2,2'-bipyridyl (dmbpy) ligands in axial and equatorial positions, and by two O atoms of a carbonate anion completing the equatorial positions. Although the water mol-ecules are disordered and their H atoms were not located, there are typical O⋯O distances between 2.8 and 3.0 Å, indicating O-H⋯O hydrogen bonding. The crystal packing is consolidated by C-H⋯O and C-H⋯Br hydrogen bonds, as well as π-π stacking inter-actions between adjacent pyridine rings of the dmbpy ligands, with centroid-centroid distances of 3.694 (3) and 3.7053 (3) Å.

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)

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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.

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

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Andrii I. Buvailo

2008-01-01

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

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

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Lin Chen

2011-01-01

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

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

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Andya Nemati

2008-10-01

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

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.

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.

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

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Alain Igau

2013-12-01

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

Standard Molar Enthalpy of Formation of RE(C5H8NS2)3(o-phen)

Institute of Scientific and Technical Information of China (English)

MENG Xiang-Xin; GAO Sheng-Li; CHEN San-Ping; YANG Xu-Wu; XIE Gang; SHI Qi-Zhen

2005-01-01

Five solid ternary complexes of RE(C5H8NS2)3(o-phen) (RE=Ho, Er, Tm, Yb, Lu) have been synthesized in absolute ethanol by rare earth chloride low hydrate reacting with the mixed ligands of ammonium pyrrolidinedithiocarbamate (APDC) and 1,10-phenanthroline·H2O (o-phen·H2O) in the ordinary laboratory atmosphere without any cautions against moisture or air. IR spectra of the complexes showed that the RE3+ coordinated with six sulfur atoms of three PDC- and two nitrogen atoms of o-phen·H2O. It was assumed that the coordination number of RE3+was eight. The constant-volume combustion energies of the complexes, △cU, were determined as (-16788.46±7.74), (- 15434.53± 8.28), (- 15287.807.31), (- 15200.50±7.22) and (- 15254.34±6.61) kJ·mol-1, respectively, by a precise rotating-bomb calorimeter at 298.15 K. Its standard molar enthalpies of combustion, △cH m,and standard molar enthalpies of formation, △fH m, were calculated as (-16803.95 ±7.74), (-15450.02±8.28),(-15303.29±9.28), (-15215.99±7.22), (-15269.83±6.61) kJ·mol-1 and (-1115.42±8.94), (-2477.80±9.15), (-2619.95 ±10.44), (-2670.17 ± 8.22), ( -2650.06± 8.49) kJ·mol-1, respectively.

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

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Lin Li

2008-01-01

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

One-Step Synthesis of Cu–ZnO@C from a 1D Complex [Cu0.02Zn0.98(C8H3NO6(C12H8N2]n for Catalytic Hydroxylation of Benzene to Phenol

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Guanghui Wang

2018-05-01

Full Text Available A novel one-dimensional bimetallic complex [Cu0.02Zn0.98(C8H3NO6(C12H8N2]n (“Complex” has been synthesized by a hydrothermal method. A Cu–ZnO@C composite was obtained by a one-step pyrolysis of Complex. Correlated with the characterization results, it is confirmed that both metallic Cu0 and ZnO nanoparticles were highly dispersed on/in the carbon substrate. This simple one-step pyrolysis method avoids the high-temperature pretreatment under H2 commonly required for preparation of such Cu–ZnO catalysts. The Cu–ZnO@C composite was tested with respect to its catalytic activities for the hydroxylation of benzene to phenol with H2O2. The results indicate that the benzene conversion, phenol yield, and phenol selectivity reached the maximum values (55.7%, 32%, and 57.5%, respectively at Complex carbonized at 600 °C, and were higher than those of the commercial mixed sample. Compared with the other candidate catalysts, the turnover frequency (TOF of our Cu–ZnO@C catalyst (117.9 mmol mol−1 s−1 can be ranked at the top. The higher catalytic activities should be due to the highly dispersed metallic Cu0 and ZnO particles as well as their synergistic interaction.

N-{4-[4-(4-Fluorophenyl-1-(2-methoxyethyl-2-methylsulfanyl-1H-imidazol-5-yl]-2-pyridyl}-2-methyl-3-phenylpropionamide

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Stefan Laufer

2009-12-01

Full Text Available In the crystal structure of the title compound, C28H29FN4O2S, the imidazole ring makes dihedral angles of 11.85 (7, 73.33 (7 and 22.83 (8° with the 4-fluorophenyl, pyridine and phenyl rings, respectively. The 4-fluorophenyl ring makes dihedral angles of 77.91 (7 and 26.93 (8° with the pyridine and phenyl rings, respectively. The phenyl and pyridine rings are nearly perpendicular, making a dihedral angle of 86.47 (9°. The crystal packing shows an intermolecular N—H...O hydrogen-bonding interaction between the N—H and carbonyl groups of the amide functions.

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

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Zukhra Ch. Kadirova

2009-07-01

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

3′,7′,7′-Trimethyl-1′-phenyl-5′,6′,7′,8′-tetrahydrospiro[indoline-3,4′-(1H,4H-pyrazolo[3,4-b]chromene]-2,5′-dione

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Li-Qin Zhao

2010-12-01

Full Text Available The title spirooxindole compound, C26H23N3O3, was prepared by the reaction of isatin, 3-methyl-1-phenyl-2-pyrazolin-5-one and 5,5-dimethylcyclohexane-1,3-dione in an ethanol solution. The fused cyclohexene ring adopts an envelope conformation. The dihedral angle between the aromatic and pyrazoline rings is 23.70 (8°. An intramolecular C—H...O interaction occurs. The crystal structure is stabilized by N—H...N hydrogen-bonding interactions, leading to a zigzag chain along the b axis.

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.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Keggin type polyoxometalate H4[αSiW12O40].nH2O as intercalant for hydrotalcite

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Neza Rahayu Palapa

2017-06-01

Full Text Available The synthesis of hydrotalcite and polyoxometalate H4[αSiW12O40].nH2O with the ratio (2:1, (1:1, (1:2 and (1:3 has been done. The product of intercalation was characterized using FT-IR spectrophotometer, XRD, and TG-DTA. Polyoxometalate H4[αSiW12O40].nH2O intercalated layered double hydroxide was optimised to use as adsorbent Congo red dye. Characterization using FT-IR was not showing the optimal insertion process. The result using XRD characterization was showed successful of polyoxometalate H4[αSiW12O40].nH2O inserted layered double hydroxide with a ratio (1:1 which the basal spacing was expanded from 7,8 Ȧ to 9,81 Ȧ. Furthermore, the thermal analysis was performed using TG-DTA. The result show that the decomposition of polyoxometalate H4[αSiW12O40].nH2O intercalated  hydrotalcite with ratio (1:1 was occured at 80oC to 400oC with a loss of OH in the layer at 150oC to 220oC, and then the decomposition of the compound polyoxometalate H4[αSiW12O40].nH2O at 350oC to 420oC. Keywords: Hydrotalcite, Layered Double Hydroxide, Polyoxometalate, Intercalation

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

International Nuclear Information System (INIS)

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

1991-01-01

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

Synthesis 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

Modelling of phase equilibria in CH4–C2H6–C3H8–nC4H10–NaCl–H2O systems

International Nuclear Information System (INIS)

Li, Jun; Zhang, Zhigang; Luo, Xiaorong; Li, Xiaochun

2015-01-01

Highlights: • A new model was established for the phase equilibria of C1–C2–C3–nC4–brine systems. • The model can reproduce of hydrocarbon–brine equilibria to high T&P and salinity. • The model can well predict H 2 O solubility in light hydrocarbon rich phases. - Abstract: A thermodynamic model is presented for the mutual solubility of CH 4 –C 2 H 6 –C 3 H 8 –nC 4 H 10 –brine systems up to high temperature, pressure and salinity. The Peng–Robinson model is used for non-aqueous phase fugacity calculations, and the Pitzer model is used for aqueous phase activity calculations. The model can accurately reproduce the experimental solubilities of CH 4 , C 2 H 6 , C 3 H 8 and nC 4 H 10 in water or NaCl solutions and H 2 O solubility in the non-aqueous phase. The experimental data of mutual solubility for the CH 4 –brine subsystem are sufficient for temperatures exceeding 250 °C, pressures exceeding 1000 bar and NaCl molalities greater than 6 molal. Compared to the CH 4 –brine system, the mutual solubility data of C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine are not sufficient. Based on the comparison with the experimental data of H 2 O solubility in C 2 H 6 -, C 3 H 8 - or nC 4 H 10 -rich phases, the model has an excellent capability for the prediction of H 2 O solubility in hydrocarbon-rich phases, as these experimental data were not used in the modelling. Predictions of hydrocarbon solubility (at temperatures up to 200 °C, pressures up to 1000 bar and NaCl molalities greater than 6 molal) were made for the C 2 H 6 –brine, C 3 H 8 –brine and nC 4 H 10 –brine systems. The predictions suggest that increasing pressure generally increases the hydrocarbon solubility in water or brine, especially in the lower-pressure region. Increasing temperature usually decreases the hydrocarbon solubility at lower temperatures but increases the hydrocarbon solubility at higher temperatures. Increasing water salinity dramatically decreases

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

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Evgeny Bulatov

2014-02-01

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

Tinnunculite, C5H4N4O3 · 2H2O: Occurrences on the Kola Peninsula and Redefinition and Validation as a Mineral Species

Science.gov (United States)

Pekov, I. V.; Chukanov, N. V.; Yapaskurt, V. O.; Belakovskiy, D. I.; Lykova, I. S.; Zubkova, N. V.; Shcherbakova, E. P.; Britvin, S. N.; Chervonnyi, A. D.

2017-12-01

Based on a study of samples found in the Khibiny (Mt. Rasvumchorr: the holotype) and Lovozero (Mts Alluaiv and Vavnbed) alkaline complexes on the Kola Peninsula, Russia, tinnunculite was approved by the IMA Commission on New Minerals, Nomenclature, and Classification as a valid mineral species (IMA no. 2015-02la) and, taking into account a revisory examination of the original material from burnt dumps of coal mines in the southern Urals, it was redefined as crystalline uric acid dihydrate (UAD), C5H4N4O3 · 2H2O. Tinnunculite is poultry manure mineralized in biogeochemical systems, which could be defined as "guano microdeposits." The mineral occurs as prismatic or tabular crystals up to 0.01 × 0.1 × 0.2 mm in size and clusters of them, as well as crystalline or microglobular crusts. Tinnunculite is transparent or translucent, colorless, white, yellowish, reddish or pale lilac. Crystals show vitreous luster. The mineral is soft and brittle, with a distinct (010) cleavage. D calc = 1.68 g/cm3 (holotype). Tinnunculite is optically biaxial (-), α = 1.503(3), β = 1.712(3), γ = 1.74(1), 2 V obs = 40(10)°. The IR spectrum is given. The chemical composition of the holotype sample (electron microprobe data, content of H is calculated by UAD stoichiometry) is as follows, wt %: 37.5 O, 28.4 C, 27.0 N, 3.8 Hcalc, total 96.7. The empirical formula calculated on the basis of (C + N+ O) = 14 apfu is: C4.99H8N4.07O4.94. Tinnunculite is monoclinic, space group (by analogy with synthetic UAD) P21/ c. The unit cell parameters of the holotype sample (single crystal XRD data) are a = 7.37(4), b = 6.326(16), c = 17.59(4) Å, β = 90(1)°, V = 820(5) Å3, Z = 4. The strongest reflections in the XRD pattern ( d, Å- I[ hkl]) are 8.82-84[002], 5.97-15[011], 5.63-24[102̅, 102], 4.22-22[112], 3.24-27[114̅,114], 3.18-100[210], 3.12-44[211̅, 211], 2.576-14[024].

Hydrothermal synthesis and crystal structures of new uranyl oxalate hydroxides: α- and β-[(UO2)2(C2O4)(OH)2(H2O)2] and [(UO2)2(C2O4)(OH)2(H2O)2].H2O

International Nuclear Information System (INIS)

Duvieubourg, Laurence; Nowogrocki, Guy; Abraham, Francis; Grandjean, Stephane

2005-01-01

Two modifications of the new uranyl oxalate hydroxide dihydrate [UO 2 ) 2 (C 2 O 4 )(OH) 2 (H 2 O) 2 ] (1 and 2) and one form of the new uranyl oxalate hydroxide trihydrate [(UO 2 ) 2 (C 2 O 4 )(OH) 2 (H 2 O) 2 ].H 2 O (3) were synthesized by hydrothermal methods and their structures determined from single-crystal X-ray diffraction data. The crystal structures were refined by full-matrix least-squares methods to agreement indices R(wR)=0.0372(0.0842) and 0.0267(0.0671) calculated for 1096 and 1167 unique observed reflections (I>2σ(I)), for α (1) and β (2) forms, respectively and to R(wR)=0.0301(0.0737) calculated for 2471 unique observed reflections (I>2σ(I)), for 3. The α-form of the dihydrate is triclinic, space group P1-bar , Z=1, a=6.097(2), b=5.548(2), c=7.806(3)A, α=89.353(5), β=94.387(5), γ=97.646(5) o , V=260.88(15)A 3 , β-form is monoclinic, space group C2/c, Z=4, a=12.180(3), b=8.223(2), c=10.777(3)A, β=95.817(4), V=1073.8(5)A 3 . The trihydrate is monoclinic, space group P2 1 /c, Z=4, a=5.5095(12), b=15.195(3), c=13.398(3)A, β=93.927(3), V=1119.0(4)A 3 . In the three structures, the coordination of uranium atom is a pentagonal bipyramid composed of dioxo UO 2 2+ cation perpendicular to five equatorial oxygen atoms belonging to one bidentate oxalate ion, one water molecule and two hydroxyl ions in trans configuration in 2 and in cis configuration in 1 and 3. The UO 7 polyhedra are linked through hydroxyl oxygen atoms to form different structural building units, dimers [U 2 O 10 ] obtained by edge-sharing in 1, chains [UO 6 ] ∼ and tetramers [U 4 O 26 ] built by corner-sharing in 2 and 3, respectively. These units are further connected by oxalate entities that act as bis-bidentate to form one-dimensional chains in 1 and bi-dimensional network in 2 and 3. These chains or layers are connected in frameworks by hydrogen-bond arrays

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].

Propane-1,3-diaminium–2-carboxypyridine-6-carboxylate–pyridine-2,6-dicarboxylic acid–water (1/2/2/8

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Hossein Aghabozorg

2008-01-01

Full Text Available The title proton-transfer compound, C3H12N22+·2C7H4NO4−·2C7H5NO4·8H2O or (pnH2(pydcH2.2(pydcH2·8H2O, was obtained by the reaction of pyridine-2,6-dicarboxylic acid (pydcH2 and propane-1,3-diamine (pn in aqueous solution. Both neutral and monoanionic forms of the diacid are observed in the crystal structure. The negative charge of two monoanions is balanced by the dicationic propane-1,3-diaminium species. In addition, considerable π–π stacking interactions between the aromatic rings of the (pydcH− and (pydcH2 fragments [with centroid–centroid distances of 3.5108 (11–3.5949 (11 Å] are observed. The most important feature of this crystal structure is the presence of a large number of O—H...O, O—H...N, N—H...O, N—H...N, C—H...O and C—H...N hydrogen bonds, with D...A ranging from 2.445 (2 to 3.485 (3 Å. These interactions as well as ion pairing and π–π stacking connect the various fragments into a supramolecular structure.

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

Science.gov (United States)

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.

Di-?-cyanido-tetra?cyanido(5,5,7,12,12,14-hexa?methyl-1,4,8,11-tetra?aza?cyclo?tetra?decane)[N-(quinolin-8-yl)quinoline-2-carboxamidato]diiron(III)nickel(II) 2.07-hydrate

OpenAIRE

Yang, Yuqi; Zhou, Hongbo; Shen, Xiaoping

2013-01-01

The asymmetric unit of the title complex, [Fe2Ni(C19H12N3O)2(CN)6(C16H36N4)]?2.07H2O, contains one [Fe(qcq)(CN)3]? anion, half a [Ni(teta)]2+ cation and two partially occupied inter?stitial water mol?ecules [qcq? is the N-(quinolin-8-yl)quinoline-2-carboxamidate anion and teta is 5,5,7,12,12,14-hexa?methyl-1,4,8,11-tetra?aza?cyclo?tetra?deca?ne]. In the complex mol?ecule, two [Fe(qcq)(CN)3]? anions additionally coordinate the central [Ni(teta)]2+ cation through cyanide groups in a trans mode,...

Supramolecular architecture in a co-crystal of the N(7—H tautomeric form of N6-benzoyladenine with adipic acid (1/0.5

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Robert Swinton Darious

2016-06-01

Full Text Available The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one molecule of N6-benzoyladenine (BA and one half-molecule of adipic acid (AA, the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7°. The N6-benzoyladenine molecule crystallizes in the N(7—H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intramolecular N—H...O hydrogen bonding between the carbonyl (C=O group and the N(7—H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7 ring motif. The two carboxyl groups of adipic acid interact with the Watson–Crick face of the BA molecules through O—H...N and N—H...O hydrogen bonds, generating an R22(8 ring motif. The latter units are linked by N—H...N hydrogen bonds, forming layers parallel to (10-5. A weak C—H...O hydrogen bond is also present, linking adipic acid molecules in neighbouring layers, enclosing R22(10 ring motifs and forming a three-dimensional structure. C=O...π and C—H...π interactions are also present in the structure.

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

Science.gov (United States)

Bouzidia, Nabaa; Salah, Najet; Hamdi, Besma; Ben Salah, Abdelhamid

2017-04-01

The study of metal phosphate has been a proactive field of research thanks to its applied and scientific importance, especially in terms of the development of optical devices such as solid state lasers as well as optical fibers. The present paper seeks to investigate the synthesis, crystal structure, elemental analysis and properties of FeAlF2(C10H8N2)(HPO4)2(H2O) compound investigated by spectroscopic studies (FT-IR and FT-Raman), thermal behavior and luminescence. The Hirshfeld surface analysis and 2-D fingerprint plot have been performed to explore the behavior of these weak interactions and crystal cohesion. This investigation shows that the molecules are connected by hydrogen bonds of the type Osbnd H⋯O and Osbnd H⋯F. In addition, the 2,2'‒bipyridine ligand plays a significant role in the construction of 3-D supramolecular framework via π‒π stacking. FT‒IR and FT‒Raman spectra were used so as to ease the responsibilities of the vibration modes of the title compound. The thermal analysis (TGA) study shows a mass loss evolution as a temperature function. Finally, the optical properties were evaluated by photoluminescence spectroscopy.

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

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M. N. Ponnuswamy

2008-10-01

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

Crystal structure of ethyl (2S-9-methoxy-2-methyl-4-oxo-3,4,5,6-tetrahydro-2H- 2,6-methanobenzo[g][1,3,5]oxadiazocine-11-carboxylate

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A. Dhandapani

2015-02-01

Full Text Available In the title compound, C15H18N2O5, the methoxyphenyl ring makes a dihedral angle of 84.70 (12° with the mean plane of the tetrahydropyrimidin-2(1H-one ring. Both the pyran and tetrahydropyrimidin-2(1H-one rings have distorted envelope conformations with the carboxylate-substituted C atom as the flap. In the crystal, molecules are linked via pairs of N—H...O hydrogen bonds, forming zigzag chains propagating along [010], which enclose R22(8 ring motifs. The chains are linked by C—H...π interactions, forming a two-dimensional network parallel to (100.

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

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Naki Çolak

2013-07-01

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

2,2′-Bis{8-[(benzylaminomethylidene]-1,6-dihydroxy-5-isopropyl-3-methylnaphthalen-7(8H-one}

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Shukhrat M. Hakberdiev

2013-11-01

Full Text Available The asymmetric unit of the title compound, C44H44N2O6, contains two independent molecules with similar conformations. The dihydronaphthalene ring systems are approximately planar [maximum deviations = 0.036 (2, 0.128 (2, 0.0.24 (2 and 0.075 (2 Å]. The dihedral angle between two dihydronaphthalene ring systems is 83.37 (4° in one molecule and 88.99 (4° in the other. The carbonyl O atom is linked with the adjacent hydroxy and imino groups via intramolecular O—H...O and N—H...O hydrogen bonds. In the crystal, molecules are linked through O—H...O hydrogen bonds into layers parallel to (001, and adjacent layers are further stacked by π–π interactions between dihydronaphthalene and phenyl rings into a three-dimensional supramolecular architecture. In the crystal, one of the isopropyl groups is disordered over two positions with an occupancy ratio of 0.684 (8:0.316 (8.

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

International Nuclear Information System (INIS)

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

1994-01-01

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

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

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S. Smaoui

2018-02-01

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

Crystal-field energy level analysis for Nd3+ ions at the low symmetry C1 site in [Nd(hfa)4(H2O)](N(C2H5)4) single crystals

International Nuclear Information System (INIS)

Mech, Agnieszka; Gajek, Zbigniew; Karbowiak, Miroslaw; Rudowicz, Czeslaw

2008-01-01

Optical absorption measurements of Nd 3+ ions in single crystals of [Nd(hfa) 4 (H 2 O)](N(C 2 H 5 ) 4 ) (hfa = hexafluoroacetyloacetonate), denoted Nd(hfa) for short, have been carried out at 4.2 and 298 K. This compound crystallizes in the monoclinic system (space group P 2 1 /n). Each Nd ion is coordinated to eight oxygen atoms that originate from the hexafluoroacetylacetonate ligands and one oxygen atom from the water molecule. A total of 85 experimental crystal-field (CF) energy levels arising from the Nd 3+ (4f 3 ) electronic configuration were identified in the optical spectra and assigned. A three-step CF analysis was carried out in terms of a parametric Hamiltonian for the actual C 1 symmetry at the Nd 3+ ion sites. In the first step, a total of 27 CF parameters (CFPs) in the Wybourne notation B kq , admissible by group theory, were determined in a preliminary fitting constrained by the angular overlap model predictions. The resulting CFP set was reduced to 24 specific independent CFPs using appropriate standardization transformations. Optimizations of the second-rank CFPs and extended scanning of the parameter space were employed in the second step to improve reliability of the CFP sets, which is rather a difficult task in the case of no site symmetry. Finally, seven free-ion parameters and 24 CFPs were freely varied, yielding an rms deviation between the calculated energy levels and the 85 observed ones of 11.1 cm -1 . Our approach also allows prediction of the energy levels of Nd 3+ ions that are hidden in the spectral range overlapping with strong ligand absorption, which is essential for understanding the inter-ionic energy transfer. The orientation of the axis system associated with the fitted CF parameters w.r.t. the crystallographic axes is established. The procedure adopted in our calculations may be considered as a general framework for analysis of CF levels of lanthanide ions at low (triclinic) symmetry sites

Crystal-field energy level analysis for Nd(3+) ions at the low symmetry C(1) site in [Nd(hfa)(4)(H(2)O)](N(C(2)H(5))(4)) single crystals.

Science.gov (United States)

Mech, Agnieszka; Gajek, Zbigniew; Karbowiak, Mirosław; Rudowicz, Czesław

2008-09-24

Optical absorption measurements of Nd(3+) ions in single crystals of [Nd(hfa)(4)(H(2)O)](N(C(2)H(5))(4)) (hfa = hexafluoroacetyloacetonate), denoted Nd(hfa) for short, have been carried out at 4.2 and 298 K. This compound crystallizes in the monoclinic system (space group P 2(1)/n). Each Nd ion is coordinated to eight oxygen atoms that originate from the hexafluoroacetylacetonate ligands and one oxygen atom from the water molecule. A total of 85 experimental crystal-field (CF) energy levels arising from the Nd(3+) (4f(3)) electronic configuration were identified in the optical spectra and assigned. A three-step CF analysis was carried out in terms of a parametric Hamiltonian for the actual C(1) symmetry at the Nd(3+) ion sites. In the first step, a total of 27 CF parameters (CFPs) in the Wybourne notation B(kq), admissible by group theory, were determined in a preliminary fitting constrained by the angular overlap model predictions. The resulting CFP set was reduced to 24 specific independent CFPs using appropriate standardization transformations. Optimizations of the second-rank CFPs and extended scanning of the parameter space were employed in the second step to improve reliability of the CFP sets, which is rather a difficult task in the case of no site symmetry. Finally, seven free-ion parameters and 24 CFPs were freely varied, yielding an rms deviation between the calculated energy levels and the 85 observed ones of 11.1 cm(-1). Our approach also allows prediction of the energy levels of Nd(3+) ions that are hidden in the spectral range overlapping with strong ligand absorption, which is essential for understanding the inter-ionic energy transfer. The orientation of the axis system associated with the fitted CF parameters w.r.t. the crystallographic axes is established. The procedure adopted in our calculations may be considered as a general framework for analysis of CF levels of lanthanide ions at low (triclinic) symmetry sites.

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.

Experimental and Theoretical Studies of the Factors Affecting the Cycloplatination of the Chiral Ferrocenylaldimine (SC-[(η5-C5H5Fe{(η5-C5H4–C(H=N–CH(Me(C6H5}

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Concepción López

2014-11-01

Full Text Available The study of the reactivity of the enantiopure ferrocenyl Schiff base (SC-[FcCH=N–CH(Me(C6H5] (1 (Fc = (η5-C5H5Fe(η5-C5H4 with cis-[PtCl2(dmso2] under different experimental conditions is reported. Four different types of chiral Pt(II have been isolated and characterized. One of them is the enantiomerically pure trans-(SC-[Pt{κ1-N[FcCH=N–CH(Me(C6H5]}Cl2(dmso] (2a in which the imine acts as a neutral N-donor ligand; while the other three are the cycloplatinated complexes: [Pt{κ2-C,N [(C6H4–N=CHFc]}Cl(dmso] (7a and the two diastereomers {(Sp,SC and (Rp,SC} of [Pt{κ2-C,N[(η5-C5H3–CH=N–{CH(Me(C6H5}]Fe(η5-C5H5}Cl(dmso] (8a and 9a, respectively. Isomers 7a-9a, differ in the nature of the metallated carbon atom [CPh (in 7a or CFc (in 8a and 9a] or the planar chirality of the 1,2-disubstituted ferrocenyl unit (8a and 9a. Reactions of 7a–9a with PPh3 gave [Pt{κ2-C,N[(C6H4–N=CHFc]}Cl(PPh3] (in 7b and the diastereomers (Sp,SC and (Rp,SC of [Pt{κ2-C,N[(η5-C5H3–CH=N–{CH(Me(C6H5}] Fe(η5-C5H5}Cl(PPh3] (8b and 9b, respectively. Comparative studies of the electrochemical properties and cytotoxic activities on MCF7 and MDA-MB231 breast cancer cell lines of 2a and cycloplatinated complexes 7b-9b are also reported. Theoretical studies based on DFT calculations have also been carried out in order to rationalize the results obtained from the cycloplatination of 1, the stability of the Pt(II complexes and their electrochemical properties.

Crystal-field energy level analysis for Nd3+ ions at the low symmetry C1 site in [Nd(hfa)4(H2O)](N(C2H5)4) single crystals

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Mech, Agnieszka; Gajek, Zbigniew; Karbowiak, Mirosław; Rudowicz, Czesław

2008-09-01

Optical absorption measurements of Nd3+ ions in single crystals of [Nd(hfa)4(H2O)](N(C2H5)4) (hfa = hexafluoroacetyloacetonate), denoted Nd(hfa) for short, have been carried out at 4.2 and 298 K. This compound crystallizes in the monoclinic system (space group P 21/n). Each Nd ion is coordinated to eight oxygen atoms that originate from the hexafluoroacetylacetonate ligands and one oxygen atom from the water molecule. A total of 85 experimental crystal-field (CF) energy levels arising from the Nd3+ (4f3) electronic configuration were identified in the optical spectra and assigned. A three-step CF analysis was carried out in terms of a parametric Hamiltonian for the actual C1 symmetry at the Nd3+ ion sites. In the first step, a total of 27 CF parameters (CFPs) in the Wybourne notation Bkq, admissible by group theory, were determined in a preliminary fitting constrained by the angular overlap model predictions. The resulting CFP set was reduced to 24 specific independent CFPs using appropriate standardization transformations. Optimizations of the second-rank CFPs and extended scanning of the parameter space were employed in the second step to improve reliability of the CFP sets, which is rather a difficult task in the case of no site symmetry. Finally, seven free-ion parameters and 24 CFPs were freely varied, yielding an rms deviation between the calculated energy levels and the 85 observed ones of 11.1 cm-1. Our approach also allows prediction of the energy levels of Nd3+ ions that are hidden in the spectral range overlapping with strong ligand absorption, which is essential for understanding the inter-ionic energy transfer. The orientation of the axis system associated with the fitted CF parameters w.r.t. the crystallographic axes is established. The procedure adopted in our calculations may be considered as a general framework for analysis of CF levels of lanthanide ions at low (triclinic) symmetry sites.

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.

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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.

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.

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 and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).

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Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B

2016-08-01

Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms.

Crystal structure of methyl 2-(2H-1,3-benzodioxol-5-yl-7,9-dibromo-8-oxo-1-oxaspiro[4.5]deca-2,6,9-triene-3-carboxylate

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Lucimara Julio Martins

2014-12-01

Full Text Available The title compound, C18H12Br2O6, was synthesized from Morita–Baylis–Hillman adducts. It incorporates the brominated spiro-hexadienone moiety typically exhibited by compounds of this class that exhibit biological activity. Both the brominated cyclohexadienone and the central five-membered rings are nearly planar (r.m.s. deviations of 0.044 and 0.016 Å, respectively, being almost perpendicularly oriented [interplanar angle = 89.47 (5°]. With respect to the central five-membered ring, the brominated cyclohexadienone ring, the benzodioxol ring and the carboxylate fragment make C—O—C—C, O—C—C—C and C—C—C—O dihedral angles of −122.11 (8, −27.20 (11 and −8.40 (12°, respectively. An intramolecular C—H...O hydrogen bond occurs. In the crystal, molecules are linked by non-classical C—H...O and C—H...Br hydrogen bonds resulting in a molecular packing in which the brominated rings are in a head-to-head orientation, forming well marked planes parallel to the b axis.

Aquachlorido{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolato-κ2O1,N,N′,O1′}cobalt(III dimethylformamide monosolvate

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Yun Wei

2012-04-01

Full Text Available In the title compound, [Co(C18H18N2O4Cl(H2O]·C3H7NO, the CoIII ion is six-coordinated by a tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethanylylidene]diphenolate ligand, with a chloride ion and an aqua ligand in the apical positions. The compound crystallized as a dimethylformamide (DMF monosolvate. In the crystal, complex molecules are linked via O—Hwater...O hydrogen bonds to form a dimer-like arrangement. These dimers are linked via a C—H...Cl interaction, and the DMF molecule is linked to the complex molecule by C—H...O interactions.

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

International Nuclear Information System (INIS)

Mandal, Sukhendu; Natarajan, Srinivasan

2005-01-01

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

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

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Yan-Lin Zhang

2011-10-01

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

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

International Nuclear Information System (INIS)

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

1996-01-01

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

Structure, ferroelectric ordering, and semiempirical quantum calculations of lanthanide based metal-organic framework: [Nd(C4H5O6)(C4H4O6)][3H2O

Science.gov (United States)

Ahmad, Bhat Zahoor; Want, Basharat

2016-04-01

We investigate the structure and ferroelectric behavior of a lanthanide based metal-organic framework (MOF), [Nd(C4H5O6)(C4H4O6)][3H2O]. X-ray crystal structure analyses reveal that it crystallizes in the P41212 space group with Nd centres, coordinated by nine oxygen atoms, forming a distorted capped square antiprismatic geometry. The molecules, bridged by tartrate ligands, form a 2D chiral structure. The 2D sheets are further linked into a 3D porous framework via strong hydrogen-bonding scheme (O-H…O ≈ 2.113 Å). Dielectric studies reveal two anomalies at 295 K and 185 K. The former is a paraelectric-ferroelectric transition, and the later is attributed to the freezing down of the motion of the hydroxyl groups. The phase transition is of second order, and the spontaneous polarization in low temperature phase is attributed to the ordering of protons of hydroxyl groups. The dielectric nonlinearity parameters have been calculated using Landau- Devonshire phenomenological theory. In addition, the most recent semiempirical models, Sparkle/PM7, Sparkle/RM1, and Sparkle/AM1, are tested on the present system to assay the accuracy of semiempirical quantum approaches to predict the geometries of solid MOFs. Our results show that Sparkle/PM7 model is the most accurate to predict the unit cell structure and coordination polyhedron geometry. The semiempirical methods are also used to calculate different ground state molecular properties.

Structuring effects of [Ln6O(OH)8(NO3)6(H2O)12]2+ entities

International Nuclear Information System (INIS)

Guillou, O.; Daiguebonne, C.; Calvez, G.; Le Dret, F.; Car, P.-E.

2008-01-01

In order to obtain highly porous lanthanide-based coordination polymers we are currently investigating reactions between [Ln 6 O(OH) 8 (NO 3 ) 6 (H 2 O) 12 ] 2+ di-cationic hexanuclear entities and sodium salts of benzene-poly-carboxylic acids. Two new coordination polymers obtained during this study are reported here. In both cases, the hexanuclear entity has been destroyed during the reaction. However the resulting compounds are original thanks to a structuring effect of the poly-metallic complex. The first compound of chemical formula [Y 2 (C 8 H 4 O 4 ) 3 (DMF)(H 2 O)],2DMF crystallizes in the monoclinic system, space group P121/n (n o 14) with a = 16.0975(3) A, b = 14.4605(3) A, c = 17.7197(4) A, β = 92.8504(9) o and Z = 4. The second compound of chemical formula Y 2 (NO 3 ) 2 (C 10 H 2 O 8 )(DMF) 4 crystallizes in the triclinic system, space group P-1 (n o 2) with a = 7.5312(3) A, b = 9.0288(3) A, c = 13.1144(6) A, α = 92.6008(14) o , β = 94.9180(14) o , γ = 112.1824(16) o and Z = 2. Both crystal structures are 2D. Both crystal structures are described and the original structural features are highlighted and related to a potential structuring effect of the hexanuclear precursor

Bis{μ-2,2′-[1,1′-(ethane-1,2-diyldinitrilodiethylidyne]diphenolato-κ5O,N,N′,O′:O}bis[chloridomanganese(III

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Robert D. Pike

2008-02-01

Full Text Available The title compound, [Mn2(C18H18N2O22Cl2], was synthesized by the reaction between manganese(II o-chlorobenzoate and the Schiff base generated in situ by the condensation of ethane-1,2-diamine and o-hydroxyacetophenone. The centrosymmetric dimer contains two Jahn–Teller-distorted manganese(III ions, each in an octahedral geometry, connected through two phenoxy bridges from two ligands.

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.

Bis(2,6-dihydroxybenzoato-κ2O1,O1′(nitrato-κ2O,O′bis(1,10-phenanthroline-κ2N,N′cerium(III

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Hongxiao Jin

2011-01-01

Full Text Available The mononuclear title complex, [Ce(C7H5O32(NO3(C12H8N22], is isostructural to other related lanthanide structures. The Ce atom is in a pseudo-bicapped square-antiprismatic geometry formed by four N atoms from two chelating 1,10-phenanthroline (phen ligands and by six O atoms, four from two 2,6-dihydroxybenzoate (DHB ligands and the other two from a nitrate anion. π–π stacking interactions between phen and DHB ligands [centroid–centroid distances = 3.513 (3 and 3.762 (2 Å] and phen and phen ligands [face-to-face separation = 3.423 (7 Å] of adjacent complexes stabilize the crystal structure. Intramolecular O—H...O hydrogen bonds are observed in the DHB ligands.

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

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Huichun Zhu

2010-01-01

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

Neutron diffraction analysis of HRh[P(C6H5)3]4

International Nuclear Information System (INIS)

Bau, R.; Stevens, R.C.; McLean, M.; Koetzle, T.F.

1987-01-01

We have collected neutron diffraction data on a large single crystal of the title compound. The most surprising result is an extremely short Rh-H distance of 1.31(8) A, presumably caused by steric interactions involving the bulky triphenyl phosphine ligands. Crystallographic details: HRh[P(C 6 H 5 ) 3 ] 4 . 1 / 2 C 6 H 6 crystallizes in the space group Pa3, with a = b = c = 22.776(3) A, Z = 8. Data were collected at the Brookhaven High Flux Beam reactor at a temperature of -23 0 C, λ = 1.15882(7) A -1 . Least-squares refinement (in which the phenyl rings were treated as rigid groups) resulted in an R factor [based on data with f > 4σ(F)] of 0.12 for 914 reflections and 95 parameters. 10 refs

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

Science.gov (United States)

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

2017-01-03

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

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

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Hong-Mian Wu

2008-05-01

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

Diaqua{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolato-κ2O,N,N′,O′}manganese(III perchlorate 18-crown-6 hemisolvate monohydrate

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Ming-Ming Yu

2009-02-01

Full Text Available In the cation of the title compound, [Mn(C18H18N2O4(H2O2]ClO4·0.5C12H24O6·H2O, the MnIII ion is coordinated by two water O atoms, and two O atoms and two N atoms from the tetradentate 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilomethylidyne]diphenolate ligand, completing a distorted octahedral geometry. One O atom of the 18-crown-6-ether is disordered over two positions with occupancies of 0.70 (2 and 0.30 (2.

Structure, ferroelectric ordering, and semiempirical quantum calculations of lanthanide based metal-organic framework: [Nd(C4H5O6)(C4H4O6)][3H2O

International Nuclear Information System (INIS)

Ahmad, Bhat Zahoor; Want, Basharat

2016-01-01

We investigate the structure and ferroelectric behavior of a lanthanide based metal-organic framework (MOF), [Nd(C 4 H 5 O 6 )(C 4 H 4 O 6 )][3H 2 O]. X-ray crystal structure analyses reveal that it crystallizes in the P4 1 2 1 2 space group with Nd centres, coordinated by nine oxygen atoms, forming a distorted capped square antiprismatic geometry. The molecules, bridged by tartrate ligands, form a 2D chiral structure. The 2D sheets are further linked into a 3D porous framework via strong hydrogen-bonding scheme (O-H…O ≈ 2.113 Å). Dielectric studies reveal two anomalies at 295 K and 185 K. The former is a paraelectric-ferroelectric transition, and the later is attributed to the freezing down of the motion of the hydroxyl groups. The phase transition is of second order, and the spontaneous polarization in low temperature phase is attributed to the ordering of protons of hydroxyl groups. The dielectric nonlinearity parameters have been calculated using Landau– Devonshire phenomenological theory. In addition, the most recent semiempirical models, Sparkle/PM7, Sparkle/RM1, and Sparkle/AM1, are tested on the present system to assay the accuracy of semiempirical quantum approaches to predict the geometries of solid MOFs. Our results show that Sparkle/PM7 model is the most accurate to predict the unit cell structure and coordination polyhedron geometry. The semiempirical methods are also used to calculate different ground state molecular properties.

Measurements of Ay(θ) for 12C(n,n)12C from En=2.2 to 8.5 MeV

International Nuclear Information System (INIS)

Roper, C.D.; Tornow, W.; Braun, R.T.; Chen, Q.; Crowell, A.; Trotter, D. Gonzalez; Howell, C.R.; Salinas, F.; Setze, R.; Walter, R.L.; Chen Zemin; Tang Hongqing; Zhou Zuying

2005-01-01

The analyzing power A y (θ) for neutron elastic scattering from 12 C has been measured for 33 neutron energies between E n =2.2 and 8.5 MeV in the angular range from 25 deg. to 145 deg. in the laboratory system. The primary motivation for these measurements is the need for an accurate knowledge of A y (θ) for 12 C(n,n) 12 C elastic scattering to enable corrections to high-precision neutron-proton and neutron-deuteron A y (θ) data in the neutron-energy range below E n =30 MeV. In their own right, 12 C(n,n) 12 C A y (θ) data are of crucial importance for improving both the parametrization of n- 12 C scattering and our knowledge of the level scheme of 13 C. The present A y (θ) data are compared with published data and previous phase-shift-analysis results

Ethane-1,2-diaminium 4,5-dichlorophthalate

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Graham Smith

2010-01-01

Full Text Available In the structure of the title compound, C2H10N22+·C8H2Cl2O42−, the dications and dianions form hydrogen-bonded ribbon substructures which enclose conjoint cyclic R21(7, R12(7 and R42(8 associations and extend down the c-axis direction. These ribbons inter-associate down b, giving a two-dimensional sheet structure. In the dianions, one of the carboxylate groups is essentially coplanar with the benzene ring, while the other is normal to it [C—C—C—O torsion angles = 177.67 (12 and 81.94 (17°, respectively].

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

Science.gov (United States)

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

2016-05-01

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

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.

C=C bond cleavage on neutral VO3(V2O5)n clusters.

Science.gov (United States)

Dong, Feng; Heinbuch, Scott; Xie, Yan; Bernstein, Elliot R; Rocca, Jorge J; Wang, Zhe-Chen; Ding, Xun-Lei; He, Sheng-Gui

2009-01-28

The reactions of neutral vanadium oxide clusters with alkenes (ethylene, propylene, 1-butene, and 1,3-butadiene) are investigated by experiments and density function theory (DFT) calculations. Single photon ionization through extreme ultraviolet radiation (EUV, 46.9 nm, 26.5 eV) is used to detect neutral cluster distributions and reaction products. In the experiments, we observe products (V(2)O(5))(n)VO(2)CH(2), (V(2)O(5))(n)VO(2)C(2)H(4), (V(2)O(5))(n)VO(2)C(3)H(4), and (V(2)O(5))(n)VO(2)C(3)H(6), for neural V(m)O(n) clusters in reactions with C(2)H(4), C(3)H(6), C(4)H(6), and C(4)H(8), respectively. The observation of these products indicates that the C=C bonds of alkenes can be broken on neutral oxygen rich vanadium oxide clusters with the general structure VO(3)(V(2)O(5))(n=0,1,2...). DFT calculations demonstrate that the reaction VO(3) + C(3)H(6) --> VO(2)C(2)H(4) + H(2)CO is thermodynamically favorable and overall barrierless at room temperature. They also provide a mechanistic explanation for the general reaction in which the C=C double bond of alkenes is broken on VO(3)(V(2)O(5))(n=0,1,2...) clusters. A catalytic cycle for alkene oxidation on vanadium oxide is suggested based on our experimental and theoretical investigations. The reactions of V(m)O(n) with C(6)H(6) and C(2)F(4) are also investigated by experiments. The products VO(2)(V(2)O(5))(n)C(6)H(4) are observed for dehydration reactions between V(m)O(n) clusters and C(6)H(6). No product is detected for V(m)O(n) clusters reacting with C(2)F(4). The mechanisms of the reactions between VO(3) and C(2)F(4)/C(6)H(6) are also investigated by calculations at the B3LYP/TZVP level.

Structure, ferroelectric ordering, and semiempirical quantum calculations of lanthanide based metal-organic framework: [Nd(C{sub 4}H{sub 5}O{sub 6})(C{sub 4}H{sub 4}O{sub 6})][3H{sub 2}O

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Ahmad, Bhat Zahoor; Want, Basharat, E-mail: bawant@kashmiruniversity.ac.in [Solid State Research Laboratory, Department of Physics, University of Kashmir, Srinagar 190006 (India)

2016-04-14

We investigate the structure and ferroelectric behavior of a lanthanide based metal-organic framework (MOF), [Nd(C{sub 4}H{sub 5}O{sub 6})(C{sub 4}H{sub 4}O{sub 6})][3H{sub 2}O]. X-ray crystal structure analyses reveal that it crystallizes in the P4{sub 1}2{sub 1}2 space group with Nd centres, coordinated by nine oxygen atoms, forming a distorted capped square antiprismatic geometry. The molecules, bridged by tartrate ligands, form a 2D chiral structure. The 2D sheets are further linked into a 3D porous framework via strong hydrogen-bonding scheme (O-H…O ≈ 2.113 Å). Dielectric studies reveal two anomalies at 295 K and 185 K. The former is a paraelectric-ferroelectric transition, and the later is attributed to the freezing down of the motion of the hydroxyl groups. The phase transition is of second order, and the spontaneous polarization in low temperature phase is attributed to the ordering of protons of hydroxyl groups. The dielectric nonlinearity parameters have been calculated using Landau– Devonshire phenomenological theory. In addition, the most recent semiempirical models, Sparkle/PM7, Sparkle/RM1, and Sparkle/AM1, are tested on the present system to assay the accuracy of semiempirical quantum approaches to predict the geometries of solid MOFs. Our results show that Sparkle/PM7 model is the most accurate to predict the unit cell structure and coordination polyhedron geometry. The semiempirical methods are also used to calculate different ground state molecular properties.

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

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Goverdhan Mehta

2012-12-01

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

(3-Methylbenzonitrile-1κN-cis-tetrakis(μ-N-phenylacetamidato-1:2κ4N:O;1:2κ4O:N-dirhodium(II(Rh—Rh

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Cassandra T. Eagle

2014-08-01

Full Text Available The complex molecule of the title compound, [Rh2{N(C6H5COCH3}4(NCC7H7], has crystallographically-imposed mirror symmetry. The four acetamide ligands bridging the dirhodium core are arranged in a 2,2-cis manner with two N atoms and two O atoms coordinating to the unique RhII atom cis to one another. The Neq—Rh—Rh—Oeq torsion angles on the acetamide bridge are 0.75 (7 and 1.99 (9°. The axial nitrile ligand completes the distorted octahedral coordination sphere of one RhII atom and shows a nonlinear coordination, with an Rh—N—C bond angle of 162.8 (5°; the N—C bond length is 1.154 (7 Å.

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.

Aqua(4-hydroxypyridine-2,6-dicarboxylato(1,10-phenanothrolinecopper(II 4.5-hydrate

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Hossein Aghabozorg

2008-01-01

Full Text Available The title compound, [Cu(C7H3NO5(C12H8N2(H2O]·4.5H2O or [Cu(hypydc(phen(H2O]·4.5H2O (phen is 1,10-phenanthroline and hypydcH2 is 4-hydroxypyridine-2,6-dicarboxylic acid, was obtained by the reaction of copper(II nitrate hexahydrate with the proton-transfer compound (phenH2(hypydc in aqueous solution. Both the cationic and the anionic fragments of the proton-transfer compound are involved in complexation. Each CuII atom has a distorted octahedral geometry. It is hexacoordinated by three O atoms and three N atoms, from one phen fragment (as bidentate ligand, one (hypydc2− unit (as tridentate ligand and a water molecule. In the crystal structure, O—H...O and C—H...O hydrogen bonds, and π–π stacking interactions [centroid-to-centroid distance 3.5642 (11 Å] between the phen ring systems, contribute to the formation of a three-dimensional supramolecular structure.

Lanthanite-(Nd), Nd2(CO3)3·8H2O

Science.gov (United States)

Morrison, Shaunna M.; Andrade, Marcelo B.; Wenz, Michelle D.; Domanik, Kenneth J.; Downs, Robert T.

2013-01-01

Lanthanite-(Nd), ideally Nd2(CO3)3·8H2O [dineodymium(III) tricarbonate octa­hydrate], is a member of the lanthanite mineral group characterized by the general formula REE 2(CO3)3·8H2O, where REE is a 10-coordinated rare earth element. Based on single-crystal X-ray diffraction of a natural sample from Mitsukoshi, Hizen-cho, Karatsu City, Saga Prefecture, Japan, this study presents the first structure determination of lanthanite-(Nd). Its structure is very similar to that of other members of the lanthanite group. It is composed of infinite sheets made up of corner- and edge-sharing of two NdO10-polyhedra (both with site symmetry ..2) and two carbonate triangles (site symmetries ..2 and 1) parallel to the ab plane, and stacked perpendicular to c. These layers are linked to one another only through hydrogen bonding involving the water mol­ecules. PMID:23476479

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

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Shu-Shen Zhang

2011-10-01

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

(3R,6S,7aS-3-Phenyl-6-(phenylsulfanylperhydropyrrolo[1,2-c]oxazol-5-one

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Anthony D. Woolhouse

2009-05-01

Full Text Available Molecules of the title compound [systematic name: (2R,5S,7S-2-phenyl-7-phenylsulfanyl-1-aza-3-oxabicyclo[3.3.0]octan-8-one], C18H17NO2S, form high quality crystals even though they are only packed using C—H...O(carbonyl and weak C—H...S interactions. The dihedral angle between the aromatic rings is 85.53 (5°. The fused rings adopt envelope and twist conformations.

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....

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.

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.

Bis{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(iminomethylene]diphenolato(1.5−-κ4O,N,N′,O′}praeseodymium(III

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Da-Qi Wang

2009-02-01

Full Text Available The title compound, [Pr(C18H22.5N2O42], is isotypic with its Er and Tb analogues. All interatomic distances, angles and the hydrogen bond geometry are very similar for the three structures..

(μ-3-Acetyl-5-carboxylato-4-methylpyrazolido-1:2κ4N2,O3:N1,O5-μ-chlorido-tetrapyridine-1κ2N,2κ2N-chlorido-1κCl-dicopper(II propan-2-ol solvate

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Sergey Malinkin

2009-10-01

Full Text Available The title compound, [Cu2(C7H6N2O3Cl2(C5H5N4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octahedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H...O hydrogen bond connects the complex molecules and propan-2-ol solvent molecules into pairs. These pairs form columns along the a axis.

Supra-molecular architecture in a co-crystal of the N(7)-H tautomeric form of N (6)-benzoyl-adenine with adipic acid (1/0.5).

Science.gov (United States)

Swinton Darious, Robert; Thomas Muthiah, Packianathan; Perdih, Franc

2016-06-01

The asymmetric unit of the title co-crystal, C12H9N5O·0.5C6H10O4, consists of one mol-ecule of N (6)-benzoyl-adenine (BA) and one half-mol-ecule of adipic acid (AA), the other half being generated by inversion symmetry. The dihedral angle between the adenine and phenyl ring planes is 26.71 (7)°. The N (6)-benzoyl-adenine mol-ecule crystallizes in the N(7)-H tautomeric form with three non-protonated N atoms. This tautomeric form is stabilized by intra-molecular N-H⋯O hydrogen bonding between the carbonyl (C=O) group and the N(7)-H hydrogen atom on the Hoogsteen face of the purine ring, forming an S(7) ring motif. The two carboxyl groups of adipic acid inter-act with the Watson-Crick face of the BA mol-ecules through O-H⋯N and N-H⋯O hydrogen bonds, generating an R 2 (2)(8) ring motif. The latter units are linked by N-H⋯N hydrogen bonds, forming layers parallel to (10-5). A weak C-H⋯O hydrogen bond is also present, linking adipic acid mol-ecules in neighbouring layers, enclosing R (2) 2(10) ring motifs and forming a three-dimensional structure. C=O⋯π and C-H⋯π inter-actions are also present in the structure.

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

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.

Aquachlorido{6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolato-κ2O1,N,N′,O1′}cobalt(III monohydrate

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Jianxin Xing

2009-04-01

Full Text Available The title compound, [Co(C18H18N2O4Cl(H2O]·H2O, contains a distorted octahedral cobalt(III complex with a 6,6′-dimethoxy-2,2′-[ethane-1,2-diylbis(nitrilodimethylidyne]diphenolate ligand, a chloride and an aqua ligand, and also a disordered water solvent molecule (half-occupancy. The CoIII ion is coordinated in an N2O3Cl manner. Weak O—H...O hydrogen bonds may help to stabilize the crystal packing.

Thermal stability of polyoxometalate compound of Keggin K8[2-SiW11O39]∙nH2O supported with SiO2

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Yunita Sari M A

2017-06-01

Full Text Available Synthesis through sol-gel method and characterization of polyoxometalate compound of K8[b2-SiW11O39]∙nH2O supported with SiO2 have been done. The functional groups of polyoxometalate compound  was characterized by FT-IR spectrophotometer for the fungtional groups and the degree’s of crystalinity  using XRD. The acidity of K8[b2-SiW11O39]∙nH2O/SiO2 was determined qualitative analysis using ammonia and pyridine adsorption and the quantitative analysis using potentiometric titration method. The results of FT-IR spectrum of K8[b2-SiW11O39]∙nH2O appeared at  wavenumber 987.55 cm-1 (W=O, 864.11 cm-1 (W-Oe-W, 756.1 cm-1 (W-Oc-W, 3425.58 cm-1 (O-H, respectively and spectrum of  K8[b2-SiW11O39]SiO2 appeared at wavenumber  956.69 cm-1 (W=O, 864.11 cm-1 (W-Oe-W, 3448.72 cm-1 (O-H, respectively. The diffraction of XRD pattern of K8[b2-SiW11O39]∙nH2O and K8[b2-SiW11O39]∙nH2O/SiO2 compounds show high crystalinity. The acidic properties showed K8[b2-SiW11O39]∙nH2O/SiO2 more acidic compared to K8[b2-The SiW11O39]∙nH2O. The qualitative analysis showed pyridine compound adsorbed more of polyoxometalate compound of K8[b2-SiW11O39]∙nH2O/SiO2. Analysis of stability showed that the K8[b2-SiW11O39]∙nH2O/SiO2 at temperature 500°C has structural changes compare to 200-400oC which was indicated from vibration at wavenumber 800-1000 cm-1. Keywords : K8[b2-SiW11O39]∙nH2O, polyoxometalate, SiO2.

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.

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

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Augusto Rivera

2011-11-01

Full Text Available The title compound, C25H30N2O6, has the imidazolidine ring in an envelope conformation. There are two intramolecular O—H...N hydrogen-bond interactions with graph-set motif S(6. The cyclohexane ring adopts a slightly distorted chair conformation. One methyl carboxylate substituent forms a dihedral angle of 12.00 (5° with the plane of the benzene ring, while the other methyl carboxylate group is almost coplanar, making a dihedral angle of 2.26 (9°. In the crystal, pairs of intermolecular C—H...O hydrogen bonds form racemic dimers, corresponding to an R22(18 graph-set motif. Further weak C—H...O interactions generate a chain running along the c axis.

1-Methoxy-3-o-tolylbicyclo[2.2.2]oct-5-ene-2,2-dicarbonitrile

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Orhan Büyükgüngör

2009-09-01

Full Text Available In the title compound, C18H18N2O, the cyclohexene and cyclohexane rings of the bicyclo[2.2.2]oct-5-ene unit adopt distorted boat conformations. In the crystal, molecules exist as C—H...N hydrogen-bonded centrosymmetric R22(14 dimers, which are further linked by C—H...π interactions.

Bis[2-(2-aminoethyl-1H-benzimidazole-κ2N2,N3](nitrato-κ2O,O′cobalt(II chloride trihydrate

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Jing Zhao

2012-06-01

Full Text Available In the title compound, [Co(NO3(C9H11N32]Cl·3H2O, the CoII atom is coordinated by four N atoms from two chelating 2-(2-aminoethyl-1H-benzimidazole ligands and two O atoms from one nitrate anion in a distorted octahedral coordination environment. In the crystal, N—H...Cl, N—H...O, O—H...Cl and O—H...O hydrogen bonds link the complex cations, chloride anions and solvent water molecules into a three-dimensional network. π–π interactions between the imidazole and benzene rings and between the benzene rings are observed [centroid–centroid distances = 3.903 (3, 3.720 (3, 3.774 (3 and 3.926 (3 Å].

Crystal structure of (1S,2R,6R,7R,8S,12S-4,10,17-triphenyl-15-thia-4,10-diazapentacyclo[5.5.5.01,16.02,6.08,12]heptadeca-13,16-diene-3,5,9,11-tetrone p-xylene hemisolvate

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Wayland E. Noland

2014-12-01

Full Text Available The title tetrone compound, C32H22N2O4S· 0.5C8H10, is the major product (50% yield of an attempted Diels–Alder reaction of 2-(α-styrylthiophene with N-phenylmaleimide (2 equivalents in toluene. Recrystallization of the resulting powder from p-xylene gave the title hemisolvate; the p-xylene molecule is located about an inversion center. In the crystal, the primary tetrone contacts are between a carbonyl O atom and the four flagpole H atoms of the bicyclo[2.2.2]octene core, forming chains along [001].

Triaquabis(1H-imidazolebis[μ2-2-(oxaloaminobenzoato(3−]dicopper(IIcalcium(II heptahydrate

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Peng Zhang

2008-02-01

Full Text Available In the title heterotrinuclear coordination compound, [CaCu2(C9H4NO52(C3H4N22(H2O3]·7H2O, the Ca2+ cation is in a pentagonal–bipyramidal geometry and bridges two (1H-imidazole[2-(oxaloaminobenzoato(3−]copper(II units in its equatorial plane. Each CuII atom has a normal square-planar geometry. The molecule has approximate local (non-crystallographic mirror symmetry and 23 classical hydrogen bonds are found in the crystal structure.

(2,3,7,8,12,13,17,18-Octaethylporphyrinato-κ4Ncobalt(II–2-nitrobenzaldehyde (1/2

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Anissa Mansour

2012-09-01

Full Text Available The asymmetric unit of the title compound, [Co(C36H44N4]·2C7H5NO3, is composed of one half of the complex, arranged about an inversion center, and a complete 2-nitrobenzaldehyde (NBA molecule. The structure consists of columns that contain interleaved molecules of NBA and [CoII(OEP] (OEP is 2,3,7,8,12,13,17,18-octaethylporphyrin, which are stacked along the a axis. The CoII atom is involved in a π interaction with the ring of the NBA molecule with a centroid–metal distance of 3.508 (6 Å. There is an intramolecular C—H...O hydrogen bond in the NBA molecule.

Ethyl 2-(3,4-dimethyl-5,5-dioxo-1H,4H-benzo[e]pyrazolo[4,3-c][1,2]thiazin-1-ylacetate

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Sana Aslam

2012-10-01

Full Text Available In the title molecule, C15H17N3O4S, the heterocyclic thiazine ring adopts a twist-boat conformation, which differs from that in related compounds, with adjacent S and C atoms displaced by 0.981 (4 and 0.413 (5 Å, respectively, on the same side of the mean plane formed by the remaining ring atoms. The mean plane of the benzene ring makes a dihedral angle of 23.43 (14° with the mean plane of the pyrazole ring. In the crystal, molecules are connected by weak C—H...O hydrogen bonds to form a three-dimensional network. The H atoms of the methyl group attached to the pyrazole ring were refined over six sites with equal occupancies.

trans-Bis(5,5-diphenylhydantoinato-κN3bis(propane-1,2-diamine-κ2N,N′nickel(II

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Xiaojiao Li

2008-12-01

Full Text Available The asymmetric unit of the title complex, [Ni(pht2(pn2] (pht is 5,5-diphenylhydantoinate and pn is propane-1,2-diamine or [Ni(C15H11N2O22(C3H10N22], contains one-half [Ni(pht2(pn2] molecule. The NiII atom is situated on a crystallographic center of inversion and shows a distorted octahedral coordination geometry. A three-dimensional network structure is assembled by inter- and intramolecular N—H...O=C interactions.

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

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

2017-03-01

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

Sandwich iridium complexes with the monoanionic carborane ligand [9-SMe2-7,8-C2B9H10]-

International Nuclear Information System (INIS)

Loginov, D.A.; Vinogradov, M.M.; Perekalin, D.S.; Starikova, Z.A.; Lysenko, K.A.; Petrovskij, P.V.; Kudinov, A.R.

2006-01-01

The reaction of the [(η-9-SMe 2 -7,8-C 2 B 9 H 10 )IrBr 2 ] 2 complex with Tl[Tl(η-7,8-C 2 B 9 H 11 )] afforded the iridacarborane compound (η-9-SMe 2 -7,8-C 2 B 9 H 10 )Ir(η-7,8-C 2 B 9 H 11 ). The cationic complex [Cp*Ir(η-9-SMe 2 -7,8-C 2 B 9 H 10 )] + PF 6 - (Cp* is pentamethylcyclopentadienyl) was synthesized by the reaction of [Cp*IrCl 2 ] 2 with Na[9-SMe 2 -7,8-C 2 B 9 H 10 ]. The structures of (η-9-SMe 2 -7,8-C 2 B 9 H 10 )Ir(η-cod) (cod is 1,5-cyclooctadiene) and [Cp*Ir(η-9-SMe 2 -7,8-C 2 B 9 H 10 ]PF 6 were established by X-ray diffraction [ru

Chlorogenic acid analogues from Gynura nepalensis protect H9c2 cardiomyoblasts against H2O2-induced apoptosis.

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Yu, Bang-Wei; Li, Jin-Long; Guo, Bin-Bin; Fan, Hui-Min; Zhao, Wei-Min; Wang, He-Yao

2016-11-01

Chlorogenic acid has shown protective effect on cardiomyocytes against oxidative stress-induced damage. Herein, we evaluated nine caffeoylquinic acid analogues (1-9) isolated from the leaves of Gynura nepalensis for their protective effect against H 2 O 2 -induced H9c2 cardiomyoblast damage and explored the underlying mechanisms. H9c2 cardiomyoblasts were exposed to H 2 O 2 (0.3 mmol/L) for 3 h, and cell viability was detected with MTT assay. Hoechst 33342 staining was performed to evaluate cell apoptosis. MMPs (mitochondrial membrane potentials) were measured using a JC-1 assay kit, and ROS (reactive oxygen species) generation was measured using CM-H 2 DCFDA. The expression levels of relevant proteins were detected using Western blot analysis. Exposure to H 2 O 2 markedly decreased the viability of H9c2 cells and catalase activity, and increased LDH release and intracellular ROS production; accompanied by a loss of MMP and increased apoptotic rate. Among the 9 chlorogenic acid analogues as well as the positive control drug epigallocatechin gallate (EGCG) tested, compound 6 (3,5-dicaffeoylquinic acid ethyl ester) was the most effective in protecting H9c2 cells from H 2 O 2 -induced cell death. Pretreatment with compound 6 (1.56-100 μmol/L) dose-dependently alleviated all the H 2 O 2 -induced detrimental effects. Moreover, exposure to H 2 O 2 significantly increased the levels of Bax, p53, cleaved caspase-8, and cleaved caspase-9, and decreased the level of Bcl-2, resulting in cell apoptosis. Exposure to H 2 O 2 also significantly increased the phosphorylation of p38, JNK and ERK in the H9c2 cells. Pretreatment with compound 6 (12.5 and 25 μmol/L) dose-dependently inhibited the H 2 O 2 -induced increase in the level of cleaved caspase-9 but not of cleaved caspase-8. It also dose-dependently suppressed the H 2 O 2 -induced phosphorylation of JNK and ERK but not that of p38. Compound 6 isolated from the leaves of Gynura nepalensis potently protects H9c2

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

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Khusnutdin M. Shakhidoyatov

2010-03-01

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

Di-μ-cyanido-tetra-cyanido(5,5,7,12,12,14-hexa-methyl-1,4,8,11-tetra-aza-cyclo-tetra-decane)[N-(quinolin-8-yl)quinoline-2-carboxamidato]diiron(III)nickel(II) 2.07-hydrate.

Science.gov (United States)

Yang, Yuqi; Zhou, Hongbo; Shen, Xiaoping

2013-05-01

The asymmetric unit of the title complex, [Fe2Ni(C19H12N3O)2(CN)6(C16H36N4)]·2.07H2O, contains one [Fe(qcq)(CN)3](-) anion, half a [Ni(teta)](2+) cation and two partially occupied inter-stitial water mol-ecules [qcq(-) is the N-(quinolin-8-yl)quinoline-2-carboxamidate anion and teta is 5,5,7,12,12,14-hexa-methyl-1,4,8,11-tetra-aza-cyclo-tetra-deca-ne]. In the complex mol-ecule, two [Fe(qcq)(CN)3](-) anions additionally coordinate the central [Ni(teta)](2+) cation through cyanide groups in a trans mode, resulting in a trinuclear structure with the Ni(2+) cation lying on an inversion centre. The two inter-stitial water mol-ecules are partially occupied, with occupancy factors of 0.528 (10) and 0.506 (9). O-H⋯O and O-H⋯N hydrogen bonding involving the two lattice water molecules and the carbonyl function and a teta N atom in an adjacent cluster leads to the formation of layers extending parallel to (010).

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

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Rajamani Raja

2015-09-01

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

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

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Nada Kheira Sebbar

2016-06-01

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

Crystal-field energy level analysis for Nd{sup 3+} ions at the low symmetry C{sub 1} site in [Nd(hfa){sub 4}(H{sub 2}O)](N(C{sub 2}H{sub 5}){sub 4}) single crystals

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Mech, Agnieszka; Gajek, Zbigniew [Institute of Low Temperature and Structure Research, Polish Academy Of Sciences, ulica Okolna 2, 54-422 Wroclaw (Poland); Karbowiak, Miroslaw [Faculty of Chemistry, University of Wroclaw, ulica F Joliot-Curie 14, 50-383 Wroclaw (Poland); Rudowicz, Czeslaw [Institute of Physics, Szczecin University of Technology, Aleja Piastow 17, 70-310 Szczecin (Poland)], E-mail: karb@wchuwr.pl

2008-09-24

Optical absorption measurements of Nd{sup 3+} ions in single crystals of [Nd(hfa){sub 4}(H{sub 2}O)](N(C{sub 2}H{sub 5}){sub 4}) (hfa = hexafluoroacetyloacetonate), denoted Nd(hfa) for short, have been carried out at 4.2 and 298 K. This compound crystallizes in the monoclinic system (space group P 2{sub 1}/n). Each Nd ion is coordinated to eight oxygen atoms that originate from the hexafluoroacetylacetonate ligands and one oxygen atom from the water molecule. A total of 85 experimental crystal-field (CF) energy levels arising from the Nd{sup 3+} (4f{sup 3}) electronic configuration were identified in the optical spectra and assigned. A three-step CF analysis was carried out in terms of a parametric Hamiltonian for the actual C{sub 1} symmetry at the Nd{sup 3+} ion sites. In the first step, a total of 27 CF parameters (CFPs) in the Wybourne notation B{sub kq}, admissible by group theory, were determined in a preliminary fitting constrained by the angular overlap model predictions. The resulting CFP set was reduced to 24 specific independent CFPs using appropriate standardization transformations. Optimizations of the second-rank CFPs and extended scanning of the parameter space were employed in the second step to improve reliability of the CFP sets, which is rather a difficult task in the case of no site symmetry. Finally, seven free-ion parameters and 24 CFPs were freely varied, yielding an rms deviation between the calculated energy levels and the 85 observed ones of 11.1 cm{sup -1}. Our approach also allows prediction of the energy levels of Nd{sup 3+} ions that are hidden in the spectral range overlapping with strong ligand absorption, which is essential for understanding the inter-ionic energy transfer. The orientation of the axis system associated with the fitted CF parameters w.r.t. the crystallographic axes is established. The procedure adopted in our calculations may be considered as a general framework for analysis of CF levels of lanthanide ions at low

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

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Zhensheng Li

2013-07-01

Full Text Available The title compound, C26H24BF2N3O, comprises a boron–dipyrromethene (BODIPY framework and a phenolic Schiff base substituent group. The BODIPY unit is close to planar [maximum deviation from the least-squares plane = 0.040 (3 Å], and forms a dihedral angle of 80.38 (13° with the meso-substituent phenyl ring and an angle of 56.57 (13° with the phenolic ring in the extended substituent chain. An intramolecular O—H...N hydrogen bond is formed between the phenolic hydroxyl group and the Schiff base N-atom. The crystal studied was a non-merohedral twin with a BASF factor of 0.447 (3 for the two components.

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

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Qiu-qi Ye

2012-09-01

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

1,4-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.

12C(n , 2 n )11C cross section from threshold to 26.5 MeV

Science.gov (United States)

Yuly, M.; Eckert, T.; Hartshaw, G.; Padalino, S. J.; Polsin, D. N.; Russ, M.; Simone, A. T.; Brune, C. R.; Massey, T. N.; Parker, C. E.; Fitzgerald, R.; Sangster, T. C.; Regan, S. P.

2018-02-01

The 12C(n ,2 n )11C cross section was measured from just below threshold to 26.5 MeV using the Pelletron accelerator at Ohio University. Monoenergetic neutrons, produced via the 3H(d ,n )4He reaction, were allowed to strike targets of polyethylene and graphite. Activation of both targets was measured by counting positron annihilations resulting from the β+ decay of 11C. Annihilation gamma rays were detected, both in coincidence and singly, using back-to-back NaI detectors. The incident neutron flux was determined indirectly via 1H(n ,p ) protons elastically scattered from the polyethylene target. Previous measurements fall into upper and lower bands; the results of the present measurement are consistent with the upper band.

Syntheses and Thermal Behaviors of Rb(FOX-7)·H2O and Cs(FOX-7)·H2O

International Nuclear Information System (INIS)

Luo, Jinan; Xu, Kangzhen; Wang, Min; Ren, Xiaolei; Chen, Yongshun; Song, Jirong; Zhao, Fengqi

2010-01-01

Two new energetic organic alkali metal salts, 1,1-diamino-2,2-dinitroethylene rubidium salt [Rb(FOX-7)·H 2 O] and 1,1- diamino-2,2-dinitroethylene cesium salt [Cs(FOX-7)·H 2 O], were synthesized by reacting of 1,1-diamino-2,2-dinitroethylene (FOX-7) and rubidium chloride or cesium chloride in alkali methanol aqueous solution, respectively. The thermal behaviors of Rb(FOX-7)·H 2 O and Cs(FOX-7)·H 2 O were studied with DSC and TG methods. The critical temperatures of thermal explosion of the two compounds are 216.22 and 223.73 .deg. C, respectively. Specific heat capacities of the two compounds were determined with a micro-DSC method, and the molar heat capacities are 217.46 and 199.47 J mol -1 K -1 at 298.15 K, respectively. The adiabatic times-to-explosion were also calculated to be a certain value of 5.81 - 6.36 s for Rb(FOX-7)·H 2 O, and 9.92 - 10.54 s for Cs(FOX-7)·H 2 O. After FOX-7 becoming alkali metal salts, thermal decomposition temperatures of the compounds heighten with the rise of element period, but thermal decomposition processes become intense

Crystal structure of trans-dichloridobis[N-(5,5-dimethyl-4,5-dihydro-3H-pyrrol-2-yl-κNacetamide]palladium(II dihydrate

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Jamal Lasri

2017-04-01

Full Text Available The title complex, [PdCl2(C8H14N2O2]·2H2O, was obtained by N–O bond cleavage of the oxadiazoline rings of the trans-[dichlorido-bis(2,5,5-trimethyl-5,6,7,7a-tetrahydropyrrolo[1,2-b][1,2,4]oxadiazole-N1]palladium(II complex. The palladium(II atom exhibits an almost square-planar coordination provided by two trans-arranged chloride anions and a nitrogen atom from each of the two neutral organic ligands. In the crystal, N—H...O, O—H...O and O—H...Cl hydrogen bonds link complex molecules into double layers parallel to the bc plane.

(meso-5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II dibromide dihydrate

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Yonghong Lu

2010-10-01

Full Text Available The asymmetric unit of the title compound, [Ni(C16H32N4]Br2·2H2O, consists of one half [Ni(C16H32N4]2+ cation, one Br− anion and one water molecule of crystallization. The NiII ion lies on an inversion centre in a square-planar environment formed by the four macrocyclic ligand N atoms. In the crystal structure, the cations, anions and water molecules are linked via intermolecular N—H...Br and O—H...Br hydrogen bonds, forming discrete chains with set-graph motif D(2D22(7D21(3D32(8. The water molecules and Br− ions are linked with set-graph motif R42(8.

catena-Poly[[[bis[aquanickel(II]bis(μ-pyridine-2,6-dicarboxylato N-oxide]-μ-1,2-di-4-pyridylethane] tetrahydrate

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Ming-Hua Yang

2008-11-01

Full Text Available In the title compound, {[Ni2(C7H3NO52(C12H12N2(H2O2]·4H2O}n, two NiII ions, two tridentate pyridine-2,6-dicarboxylate N-oxide ligands and two coordinated water molecules form centrosymmetric dinuclear units, which are further bridged by centrosymmetric 1,2-di-4-pyridylethane ligands into polymeric chains along [210]. Each NiII ion has a distorted square-pyramidal environment, with the basal plane formed by three O [Ni—O = 1.9290 (16–1.9588 (10 Å] and one N [Ni—N = 1.9828 (18 Å] atoms and the apical position occupied by the water molecule [Ni—O = 2.2643 (11 Å]. The water molecules are involved in the formation of O—H...O hydrogen bonds.

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

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

2-(6-Bromobenzo[d]thiazol-2-yl-5,5-dimethylthiazol-4(5H-one

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Rainer Beckert

2013-12-01

Full Text Available The title compound, C12H9BrN2OS2, was obtained by reacting 6-bromobenzo[d]thiazole-2-carbonitrile in iso-propanol with ethyl 2-mercapto-2-methylpropanoate at reflux temperature for several hours. The resulting dimethyloxyluciferin derivative shows partial double-bond character of the carbon–carbon bond between the two heterocyclic moieties [C—C = 1.461 (3 Å]. This double bond restricts rotation around this C—C axis, therefore leading to an almost planar molecular structure [N—C—C—S torsion angle = 9.7 (3°]. The five-membered thiazoline ring is not completely planar as a result of the bulky S atom [C—S—C—C torsion angle = 5.17 (12°].

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

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Yuan-Yuan Liu

2012-08-01

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

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

International Nuclear Information System (INIS)

Wickleder, M.S.

2005-01-01

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

2,2′-(Diselane-1,2-diyldinicotinamide N,N′-dimethylformamide disolvate

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Aixia Feng

2010-05-01

Full Text Available The asymmetric unit of the title compound, C12H10N4O2Se2·2C3H7NO, contains two solvent molecules and two half molecules of the dinicotinamide, each of which sits on a center of symmetry passing through the middle of the Se—Se bond. In each molecule, the two pyridyl groups and diseleno group are approximately coplanar (r.m.s. deviations from planarity for all non-H atoms = 0.011 and 0.008 Å in the two molecules. Intermolecular N—H...O hydrogen bonds stablilize the crystal packing.

Structural, thermal, spectroscopic and magnetic studies of the (C2N2H10)0.5[Fe xV1-x(HPO3)2] (x = 0.26, 0.52, 0.74) solid solution

International Nuclear Information System (INIS)

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

2006-01-01

The (C 2 N 2 H 10 ) 0.5 [Fe x V 1-x (HPO 3 ) 2 ] (x = 0.26, 0.52 0.74) compounds have been obtained by mild solvothermal conditions in the form of micro-crystalline powder with brown color. The crystal structures were refined by X-ray powder diffraction data using the Rietveld method. The compounds crystallize in the monoclinic system, space group P2/c with the unit-cell parameters, a = 9.262(5) A, b = 8.823(5) A, c = 9.714(6) A, β = 120.84(3) o ; a = 9.245(1) A, b = 8.823(1) A, c = 9.698(1)A, β = 120.80(1) o and, a = 9.254(4)A, b = 8.822(4)A, c = 9.702(4)A, β = 120.73(3) o for (C 2 N 2 H 10 ) 0.5 [Fe 0.26 V 0.74 (HPO 3 ) 2 ] (1) (C 2 N 2 H 10 ) 0.5 [Fe 0.52 V 0.48 (HPO 3 ) 2 ] (2), and (C 2 N 2 H 10 ) 0.5 [Fe 0.74 V 0.26 (HPO 3 ) 2 ] (3). The compounds show an open crystalline structure with three-dimensional character, whose formula for the anionic inorganic skeleton is [M(HPO 3 ) 2 ] 2- . The inorganic framework is formed by [MO 6 ] octahedra inter-connected by phosphite groups. The structure of the compounds exhibits channels extended along the [1 0 0] and [0 0 1] directions and the ethylendiammonium cations are located inside these channels, linked through hydrogen bonds and ionic interactions. The infrared spectra show the bands corresponding to the stretching (P-H) vibration of the phosphite group and the band corresponding to the deformation mode of the ethylendiammonium cation, δ(NH 3 + ). The thermal and thermodiffractometric behavior show that the compounds are stable up to approximately 300 deg. C, at higher temperatures the decomposition of the crystal structure by calcination of the organic cation starts. The diffuse reflectance spectra show bands of the V 3+ ion (d 2 ), and a band of the Fe 3+ ion (d 5 ), in a slightly distorted octahedral symmetry. The values of the Dq and Racah parameters (B and C) have been calculated for the V(III) cation. Magnetic measurements were performed on a powdered sample from 5 to 300 K at magnetic fields 1000, 500

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

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Garima Sharma

2012-09-01

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

Syntheses, crystal structures, and properties of the isotypic pair [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O

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Van, Nguyen-Duc; Kleeberg, Fabian M.; Schleid, Thomas [Institut fuer Anorganische Chemie, Universitaet Stuttgart, Pfaffenwaldring 55, 70569 Stuttgart (Germany)

2015-11-15

Single crystals of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O and [In(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O were obtained by reactions of aqueous solutions of the acid (H{sub 3}O){sub 2}[B{sub 12}H{sub 12}] with chromium(III) hydroxide and indium metal shot, respectively. The title compounds crystallize isotypically in the trigonal system with space group R anti 3c (a = 1157.62(3), c = 6730.48(9) pm for the chromium, a = 1171.71(3), c = 6740.04(9) pm for the indium compound, Z = 6). The arrangement of the quasi-icosahedral [B{sub 12}H{sub 12}]{sup 2-} dianions can be considered as stacking of two times nine layers with the sequence..ABCCABBCA.. and the metal trications arrange in a cubic closest packed..abc.. stacking sequence. The metal trications are octahedrally coordinated by six water molecules of hydration, while another fifteen H{sub 2}O molecules fill up the structures as zeolitic crystal water or second-sphere hydrating species. Between these free and the metal-bonded water molecules, bridging hydrogen bonds are found. Furthermore, there is also evidence of hydrogen bonding between the anionic [B{sub 12}H{sub 12}]{sup 2-} clusters and the free zeolitic water molecules according to B-H{sup δ-}..{sup δ+}H-O interactions. Vibrational spectroscopy studies prove the presence of these hydrogen bonds and also show slight distortions of the dodecahydro-closo-dodecaborate anions from their ideal icosahedral symmetry (I{sub h}). Thermal decomposition studies for the example of [Cr(H{sub 2}O){sub 6}]{sub 2}[B{sub 12}H{sub 12}]{sub 3}.15H{sub 2}O gave no hints for just a simple multi-stepwise dehydration process. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

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Qun Qian

2008-07-01

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

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.

Study of the unimolecular decompositions of the (C3H6)+2 and (c-C3H6)+2 complexes

International Nuclear Information System (INIS)

Tzeng, W.; Ono, Y.; Linn, S.H.; Ng, C.Y.

1985-01-01

The major product channels identified in the unimolecular decompositions ofC 3 H + 6 xC 3 H 6 and c-C 3 H + 6 xc-C 3 H 6 in the total energy [neutral (C 3 H 6 ) 2 or (c-C 3 H 6 ) 2 heat of formation plus excitation energy] range of approx.230--450 kcal/mol are C 3 H + 7 +C 3 H 5 , C 4 H + 7 +C 2 H 5 , C 4 H + 8 +C 2 H 4 , and C 5 H + 9 +CH 3 . The measured appearance energy for C 4 H + 7 (9.54 +- 0.04 eV) from (C 3 H 6 ) 2 is equal to the thermochemical threshold for the formation of C 4 H + 7 +C 2 H 5 from (C 3 H 6 ) 2 , indicating that the exit potential energy barrier for the ion--molecule reaction C 3 H + 6 +C 3 H 6 →C 4 H + 7 +C 2 H 5 is negligible. There is evidence that the formations of C 4 H + 7 +C 2 H 4 +H from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 also proceed with high probabilities when they are energetically allowed. The variations of the relative abundances for C 4 H + 7 ,C 4 H + 8 , and C 5 H + 9 from (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 as a function of ionizing photon energy are in qualitative agreement, suggesting that (C 3 H 6 ) + 2 and (c-C 3 H 6 ) + 2 rearrange to similar C 6 H + 12 isomers prior to fragmentation. The fact that C 6 H + 11 is found to be a primary ion from the unimolecular decomposition of (c-C 3 H 6 ) + 2 but not (C 3 H 6 ) + 2 supports the conclusion that the distribution of C 6 H + 12 collision complexes involved in the C 3 H + 6 +C 3 H 6 reactions is different from that in the cyclopropane ion--molecule reactions

Bis{(E-3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropan-1-aminium} bis[μ-(E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamido(2−]bis{[(E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide]copper(II} bis((E-{3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropyl}carbamate acetonitrile disolvate

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Andrii I. Buvailo

2012-12-01

Full Text Available The reaction between copper(II nitrate and (E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide led to the formation of the dinuclear centrosymmetric copper(II title complex, (C8H18N3O22[Cu2(C8H15N3O22(C8H17N3O22](C9H16N3O42·2CH3CN, in which an inversion center is located at the midpoint of the Cu2 unit in the center of the neutral [Cu2(C8H15N3O22(C8H17N3O22] complex fragment. The Cu2+ ions are connected by two N—O bridging groups [Cu...Cu separation = 4.0608 (5 Å] while the CuII ions are five-coordinated in a square-pyramidal N4O coordination environment. The complex molecule co-crystallizes with two molecules of acetonitrile, two molecules of the protonated ligand (E-3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropan-1-aminium and two negatively charged (E-{3-[2-(hydroxyiminopropanamido]-2,2-dimethylpropyl}carbamate anions, which were probably formed as a result of condensation between (E-N-(3-amino-2,2-dimethylpropyl-2-(hydroxyiminopropanamide and hydrogencarbonate anions. In the crystal, the complex fragment [Cu2(C8H15N3O22(C8H17N3O22] and the ion pair C8H18N3O2+.C9H16N3O4− are connected via an extended system of hydrogen bonds.

(Carbonato-κ2 O,O′)bis­(5,5′-dimethyl-2,2′-bipyridyl-κ2 N,N′)cobalt(III) bromide trihydrate

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Arun Kumar, Kannan; Meera, Parthsarathi; Amutha Selvi, Madhavan; Dayalan, Arunachalam

2012-01-01

In the title complex, [Co(CO3)(C12H12N2)2]Br·3H2O, the CoIII cation has a distorted octa­hedral coordination environment. It is chelated by four N atoms of two different 5,5′-dimethyl-2,2′-bipyridyl (dmbpy) ligands in axial and equatorial positions, and by two O atoms of a carbonate anion completing the equatorial positions. Although the water mol­ecules are disordered and their H atoms were not located, there are typical O⋯O distances between 2.8 and 3.0 Å, indicating O—H⋯O hydrogen bonding. The crystal packing is consolidated by C—H⋯O and C—H⋯Br hydrogen bonds, as well as π–π stacking inter­actions between adjacent pyridine rings of the dmbpy ligands, with centroid–centroid distances of 3.694 (3) and 3.7053 (3) Å. PMID:22589773

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

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Hong-Mei Wang

2009-12-01

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

Structural and spectral analyses of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide)

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Yıldırım, Sema Öztürk; Büyükmumcu, Zeki; Pekdur, Özlem Savaş; Butcher, Ray J.; Doǧan, Şengül Dilem

2018-02-01

In this study we report structure determination of N,N'-(2,2'-dithiodi-o-phenylene)bis-(furan-2-carboxamide). 2,2'-Dithiobis(benzamide) derivatives have been reported to possess important biological properties such as antibacterial, antifungal activities and inhibition of blood platelet aggregation and redeterrmined at 100(2)K from the data published by Raftery, Lallbeeharry, Bhowon, Laulloo & Joulea [Acta Cryst. 2009, E65, o16]. 2,2'-Dithiobis(N-butyl-benzamide) has been reported to be useful as an antiseptic for cosmetics. The structural properties of the compound have been characterized by using 1H NMR and the structure were determined by single-crystal X-ray diffraction. Molecular structure crystallizes in triclinic form, space group with a = 9.6396(7) Å, b = 9.9115(7) Å, c = 12.0026(8) Å, α = 109.743(6)°, β = 103.653(6)°, γ = 104.633(6)° and V = 977.15(13) Å3. In the solid state of the molecular structure N-H…S, N-H…O and C-H…O, type interactions provide for stabilization. The geometries of the title compound have been optimized using density functional theory (DFT) method. The calculated values were found to be in agreement with the experimental data.

Simple preparations of Pd6Cl12, Pt6Cl12, and Qn[Pt2Cl8+n], n=1, 2 (Q=TBA+, PPN+) and structural characterization of [TBA][Pt2Cl9] and [PPN]2[Pt2Cl10].C7H8.

Science.gov (United States)

Dell'Amico, Daniela Belli; Calderazzo, Fausto; Marchetti, Fabio; Ramello, Stefano; Samaritani, Simona

2008-02-04

The hexanuclear Pd6Cl12, i.e., the crystal phase classified as beta-PdCl2, was obtained by reacting [TBA]2[Pd2Cl6] with AlCl3 (or FeCl3) in CH2Cl2. The action of AlCl3 on PtCl42-, followed by digestion of the resulting solid in 1,2-C2H4Cl2 (DCE), CHCl3, or benzene, produced Pt6Cl12.DCE, Pt6Cl12.CHCl3, or Pt6Cl12.C6H6, respectively. Treating [TBA]2[PtCl6] with a slight excess of AlCl3 afforded [TBA][Pt2Cl9], whose anion was established crystallographically to be constituted by two "PtCl6" octahedra sharing a face. Dehydration of H2PtCl6.nH2O with SOCl2 gave an amorphous compound closely analyzing as PtCl4, reactive with [Q]Cl in SOCl2 to yield [Q][Pt2Cl9] or [Q]2[Pt2Cl10], depending on the [Q]Cl/Pt molar ratio (Q=TBA+, PPN+). A single-crystal X-ray diffraction study has shown [PPN]2[Pt2Cl10].C7H8 to contain dinuclear anions formed by two edge-sharing PtCl6 octahedra.

Hydrothermal synthesis and characterization of the praseodymium borate-nitrate Pr[B{sub 5}O{sub 8}(OH)(H{sub 2}O){sub 0.87}]NO{sub 3}.2H{sub 2}O

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Ortner, Teresa S.; Huppertz, Hubert [Innsbruck Univ. (Austria). Inst. fuer Allgemeine, Anorganische und Theoretische Chemie

2017-10-01

The praseodymium borate-nitrate Pr[B{sub 5}O{sub 8}(OH)(H{sub 2}O){sub 0.87}]NO{sub 3}.2H{sub 2}O was obtained in a hydrothermal synthesis. It crystallizes monoclinically in the space group P2{sub 1}/n (no. 14) with four formula units (Z=4) and unit cell parameters of a=641.9(3), b=1551.8(7), c=1068.4(5) pm, with β=90.54(2) yielding V=1.0643(8) nm{sup 3}. The defect variant constitutes the missing member in the series of isostructural, early rare earth borate-nitrates of the composition RE[B{sub 5}O{sub 8}(OH)(H{sub 2}O){sub x}]NO{sub 3}.2H{sub 2}O [RE=La (x=0; 1), Ce (x=1), Nd (x=0.85), Sm (x=0)]. In addition to powder and single-crystal X-ray diffraction data, the novel borate-nitrate was characterized through IR and Raman spectroscopy.

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

Science.gov (United States)

Bulatov, Evgeny; Chulkova, Tatiana; Haukka, Matti

2014-01-01

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

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

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Najat Abbassi

2013-04-01

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

Proton-transfer compounds of 8-hydroxy-7-iodoquinoline-5-sulfonic acid (ferron) with 4-chloroaniline and 4-bromoaniline.

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Smith, Graham; Wermuth, Urs D; Healy, Peter C

2007-07-01

The crystal structures of the proton-transfer compounds of ferron (8-hydroxy-7-iodoquinoline-5-sulfonic acid) with 4-chloroaniline and 4-bromoaniline, namely 4-chloroanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)ClN(+) x C(9)H(5)INO(4)S(-) x H(2)O, and 4-bromoanilinium 8-hydroxy-7-iodoquinoline-5-sulfonate monohydrate, C(6)H(7)BrN(+) x C(9)H(5)INO(4)S(-) x H(2)O, have been determined. The compounds are isomorphous and comprise sheets of hydrogen-bonded cations, anions and water molecules which are extended into a three-dimensional framework structure through centrosymmetric R(2)(2)(10) O-H...N hydrogen-bonded ferron dimer interactions.

The 12C(n, 2n)11C cross section from threshold to 26.5 MeV.

Science.gov (United States)

Yuly, M; Eckert, T; Hartshaw, G; Padalino, S J; Polsin, D N; Russ, M; Simone, A T; Brune, C R; Massey, T N; Parker, C E; Fitzgerald, R; Sangster, T C; Regan, S P

2018-02-01

The 12 C(n, 2n) 11 C cross section was measured from just below threshold to 26.5 MeV using the Pelletron accelerator at Ohio University. Monoenergetic neutrons, produced via the 3 H(d,n) 4 He reaction, were allowed to strike targets of polyethylene and graphite. Activation of both targets was measured by counting positron annihilations resulting from the β + decay of 11 C. Annihilation gamma rays were detected, both in coincidence and singly, using back-to-back NaI detectors. The incident neutron flux was determined indirectly via 1 H(n,p) protons elastically scattered from the polyethylene target. Previous measurements fall into upper and lower bands; the results of the present measurement are consistent with the upper band.

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

Directory of Open Access Journals (Sweden)

Sibi Narayanan

2012-12-01

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

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

International Nuclear Information System (INIS)

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

1979-01-01

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

Synthesis, structure and magnetic behavior of a new three-dimensional Manganese phosphite-oxalate: [C2N2H10][Mn2II(OH2)2(HPO3)2(C2O4)

International Nuclear Information System (INIS)

Ramaswamy, Padmini; Mandal, Sukhendu; Natarajan, Srinivasan

2009-01-01

A novel manganese phosphite-oxalate, [C 2 N 2 H 10 ][Mn 2 II (OH 2 ) 2 (HPO 3 ) 2 (C 2 O 4 )] has been hydothermally synthesized and its structure determined by single-crystal X-ray diffraction. The structure consists of neutral manganese phosphite layers, [Mn(HPO 3 )] ∞ , formed by MnO 6 octahedra and HPO 3 units, cross-linked by the oxalate moieties. The organic cations occupy the middle of the 8-membered one-dimensional channels. Magnetic studies indicate weak antiferromagnetic interactions between the Mn 2+ ions. - Abstract: A new antiferromagnetic three-dimensional inorganic-organic hybrid compound, [C 2 N 2 H 10 ][Mn 2 II (OH 2 ) 2 (HPO 3 ) 2 (C 2 O 4 )] has been prepared hydrothermally. The compound has neutral manganese layers pillared by oxalate units. The neutral manganese layers are shown here. Display Omitted

Structurally characterized 1,1,3,3-tetramethylguanidine solvated magnesium aryloxide complexes: [Mg(mu-OEt)(DBP)(H-TMG)]2, [Mg(mu-OBc)(DBP)(H-TMG)]2, [Mg(mu-TMBA)(DBP)(H-TMG)]2, [Mg(mu-DPP)(DBP)(H-TMG)]2, [Mg(BMP)2(H-TMG)2], [Mg(O-2,6-Ph2C6H3)2 (H-TMG)2].

Science.gov (United States)

Monegan, Jessie D; Bunge, Scott D

2009-04-06

The synthesis and structural characterization of several 1,1,3,3-tetramethylguanidine (H-TMG) solvated magnesium aryloxide complexes are reported. Bu(2)Mg was successfully reacted with H-TMG, HOC(6)H(3)(CMe(3))(2)-2,6 (H-DBP), and either ethanol, a carboxylic acid, or diphenyl phosphate in a 1:1 ratio to yield the corresponding [Mg(mu-L)(DBP)(H-TMG)](2) where L = OCH(2)CH(3) (OEt, 1), O(2)CC(CH(3))(3) (OBc, 2), O(2)C(C(6)H(2)-2,4,6-(CH(3))(3)) (TMBA, 3), or O(2)P(OC(6)H(5))(2) (DPP, 4). Bu(2)Mg was also reacted with two equivalents of H-TMG and HOC(6)H(3)(CMe(3))-2-(CH(3))-6 (BMP) or HO-2,6-Ph(2)C(6)H(3) to yield [Mg(BMP)(2)(H-TMG)(2)] (5) and [Mg(O-2,6-Ph(2)C(6)H(3))(2)(H-TMG)(2)] (6). Compounds 1-6 were characterized by single-crystal X-ray diffraction. Polymerization of l- and rac-lactide with 1 was found to generate polylactide (PLA). A discussion concerning the relevance of compounds 2 - 4 to the structure of Mg-activated phosphatase enzymes is also provided. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, FT-IR spectroscopy, and (1)H, (13)C and (31)P NMR studies.