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.)

Solid-State Synthesis and Structure of the Enigmatic Ammonium Octaborate: (NH4)2[B7O9(OH)5]·3/4B(OH)3·5/4H2O.

Science.gov (United States)

Neiner, Doinita; Sevryugina, Yulia V; Schubert, David M

2016-09-06

The compound known since the 19th century as ammonium octaborate was structurally characterized revealing the ammonium salt of the ribbon isomer of the heptaborate anion, [B7O9(OH)5](2-), with boric acid and water molecules. Of composition (NH4)2B7.75O12.63·4.88H2O, it approximates the classical ammonium octaborate composition (NH4)2B8O13·6H2O and has the structural formula {(NH4)2[B7O9(OH)5]}4·3B(OH)3·5H2O. It spontaneously forms at room temperature in solid-state mixtures of ammonium tetraborate and ammonium pentaborate. It crystallizes in the monoclinic space group P21/c with a = 11.4137(2) Å, b = 11.8877(2) Å, c = 23.4459(3) Å, β = 90.092(1)°, V = 3181.19(8) Å(3), and Z = 2 and contains well-ordered ammonium cations and [B7O9(OH)5](2-) anions and disordered B(OH)3 and H2O molecules linked by extensive H bonding. Expeditious solid-state formation of the heptaborate anion under ambient conditions has important implications for development of practical syntheses of industrially useful borates.

A neodymium(III)-ammonium complex involving oxalate and carbonate ligands: (NH4)2[Nd2(C2O4)3(CO3)(H2O)].H2O.

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Trombe, Jean-Christian; Galy, Jean; Enjalbert, Renée

2002-10-01

The title compound, diammonium aqua-mu-carbonato-tri-mu-oxalato-dineodymium(III) hydrate, (NH(4))(2)[Nd(2)(CO(3))(C(2)O(4))(3)(H(2)O)].H(2)O, involving the two ligands oxalate and carbonate, has been prepared hydrothermally as single crystals. The Nd atoms form a tetranuclear unit across the inversion centre at (1/2, 1/2, 1/2). Starting from this tetranuclear unit, the oxalate ligands serve to develop a three-dimensional network. The carbonate group acts as a bis-chelating ligand to two Nd atoms, and is monodentate to a third Nd atom. The oxalate groups are all bis-chelating. The two independent Nd atoms are ninefold coordinated and the coordination polyhedron of these atoms is a distorted monocapped antiprism.

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

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

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

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.

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-01

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

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

International Nuclear Information System (INIS)

Feng Meiling; Mao Jianggao

2005-01-01

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

(Acetylacetonato-κ2O,O′bis[5-methoxy-2-(naphth[1,2-d][1,3]oxazol-2-ylphenyl-κ2C1,N]iridium(III

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Yuan-Yuan Zhou

2011-10-01

Full Text Available In the title compound, [Ir(C18H12NO22(C5H7O2], the Ir atom is O,O′-chelated by the acetylacetonate group and C,N-chelated by the 2-arylnaphth[1,2-d]oxazole groups. The six-coordinate metal atom displays a distorted octahedral geometry. Intramolecular C—H...O hydrogen bonds occur. In the crystal, intermolecular C—H...O hydrogen bonds link the molecules into columns parallel to the b axis.

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

Channels with ordered water and bipyridine molecules in the porous coordination polymer {[Cu(SiF6(C10H8N22]·2C10N2H8·5H2O}n

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Emmanuel Aubert

2016-11-01

Full Text Available The coordination polymer {[Cu(SiF6(C10H8N22]·2C10H8N2·5H2O}n, systematic name: poly[[bis(μ2-4,4′-bipyridine(μ2-hexafluoridosilicatocopper(II] 4,4′-bipyridine disolvate pentahydrate], contains pores which are filled with water and 4,4′-bipyridine molecules. As a result of the presence of these ordered species, the framework changes its symmetry from P4/mmm to P21/c. The 4,4′-bipyridine guest molecules form chains inside the 6.5 × 6.9 Å pores parallel to [100] in which the molecules interact through π–π stacking. Ordered water molecules form infinite hydrogen-bonded chains inside a second pore system (1.6 × 5.3 Å free aperture perpendicular to the 4,4′-bipyridine channels.

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(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.

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.

NCI calculations for understanding a physical phase transition in (C6H14N2)[Mn(H2O)6](SeO4)2

Science.gov (United States)

Naïli, Houcine; François, Michel; Norquist, Alexander J.; Rekik, Walid

2017-12-01

An organically templated manganese selenate, (C6H14N2)[Mn(H2O)6](SeO4)2, has been synthesized by slow evaporation and crystallographically characterized. The title compound crystallizes at room temperature in the monoclinic centrosymmetric space group P21/n, with the following unit cell parameters: a = 7.2373(4) Å; b = 12.5600(7) Å; c = 10.1945(7) Å; β = 91.155(4)°, V = 926.50(10) Å3and Z = 2. Its crystal structure is built of manganese(II) cations coordinated by six water molecules in octahedral geometry, disordered dabcodiium cations and selenate anions, resulting in an extensive hydrogen-bonding network. Differential scanning calorimetry (DSC) measurement indicated that the precursor undergoes a reversible phase transition at about 216 and 218 K during the cooling and heating processes respectively. Below this temperature the title compound is noncentrosymmetric with space group P21 and lattice parameters a = 7.2033(8) Å; b = 12.4981(13) Å; c = 10.0888(11) Å; β = 91.281(2)°, V = 908.04(17) Å3 and Z = 2. The disorder-order transformation of the C atoms of (C6H14N2)2+ cation may drive the structural phase transition. The low temperature phase obtained by breaking symmetry presents a fully ordered structure. The noncovalent interaction (NCI) method was used not only to locate, quantify, and visualize intermolecular interactions in the high and low temperature phases but also to confirm the phase transition detected by DSC measurement. The thermal decomposition of this new compound proceeds through four stages giving rise to the manganese oxide as final product at 850 °C.

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.

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.

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.

(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.

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.

Crystal structure of strontium osmate (8) Sr[OsO5(H2O)]x3H2O

International Nuclear Information System (INIS)

Nevskij, N.N; Ivanov-Ehmin, B.N.; Nevskaya, N.A.; Belov, N.V.; AN SSSR, Moscow. Inst. Kristallografii)

1982-01-01

Crystal structure of the Sr[OsO 5 (H 2 O)]x3H 2 O complex is studied. Rhombic P-cell has the parameters: a=6.426(1), b=7.888(1), c=14.377(5) A, Vsub(c)=729 A 3 . The R-factor equals 0.034. The coordinates of the basis atoms and isotropic temperature corrections, as well as basic interatomic distances, are determined

Crystal structure of RbCe(SeO4)2 · 5H2O

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Ovanesyan, S.M.; Iskhakova, L.D.; Trunov, V.K.

1987-01-01

RbTR(SeO 4 ) 2 x5H 2 O TR=La-Pr are synthesized. Crystal structure of RbCe(SeO 4 ) 2 x5H 2 O is studied. Monoclinic unit parameters are: a=7,200(2), b=8,723(1), c=19,258(6) A, Β=90,88(2), ρ (calc) =3,304 sp.gr. P2 1 /c. Within the structure the Ce nine vertex cages are united by Se(1)- and Se(2)-tetrahedrons in (Ce(SeO 4 ) 2 (H 2 O) 5 ) 2 ∞ n- layers. Some crystal structure regularities of the laminated MTR(EO 4 ) 2 xnH 2 O (M=NH 4 ,K,Rb,Cs; TR=La-Ln, E=S,Se) are considered

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

Science.gov (United States)

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

2018-06-01

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

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

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Sergey Malinkin

2011-09-01

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

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

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.

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.

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

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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].

5-Fluoro-6′H,7′H,8′H-spiro[indoline-3,7′-pyrano[3,2-c:5,6-c′]di-1-benzopyran]-2,6′,8′-trione

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J. Suresh

2012-03-01

Full Text Available In the title compound, C26H12FNO6, the central pyran ring and both benzopyran systems are nonplanar, having total puckering amplitudes of 0.139 (2, 0.050 (1 and 0.112 (2 Å, respectively. The central pyran ring adopts a boat conformation. The crystal structure is stabilized by C—H...O, N—H...O, N—H...F and C—H...π interactions.

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.

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.

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

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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.

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

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Palanikumar Maniam

2011-06-01

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

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

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.

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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.

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.

(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-[Bis(2,4-di-tert-butylphenoxyphosphanyloxy-κP]-3,5-di-tert-butylphenyl-κC1}[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I toluene monosolvate

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Detlef Selent

2012-02-01

Full Text Available The reaction of (η3-allyl[(1,2,5,6-η-cycloocta-1,5-diene]rhodium(I with tris(2,4-di-tert-butylphenylphosphite in toluene produces the title compound, [Rh(C42H62O3P(C8H12]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2 and 0.190 (2.

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

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Xiao Zhen Feng

2008-05-01

Full Text Available In the title compound, [Cu(C13H13Cl2NO3(C3H7NO], the CuII atom is coordinated in a slightly distorted square-planar geometry by two O atoms and one N atom from the tridentate chiral ligand 2-[(3,5-dichloro-2-oxidobenzylideneamino]-3-methylpentanoate and by one O atom from dimethylformamide. In the crystal structure, the Cu atom forms contacts with Cl and O atoms of two units (Cu...Cl and Cu...O = 3.401 and 2.947 Å, respectively, thereby forming an approximately octahedral arrangement. A three-dimensional network is constructed through Cl...Cu, O...Cu, Cl...Cl contacts and C—H...O hydrogen bonds.

MeB5O8(Me-Li, Na, K, NH4)-H2NCONHCOCH3-H2O system at 25 deg C

International Nuclear Information System (INIS)

Skvortsov, V.G.; Fedorov, Yu.A.; Molodkin, A.K.; Tsekhanskij, R.S.

1986-01-01

Using the methods of isothermal solubility, densi- and refractometry, systems MB 5 O 8 (M-Li, Na, K, NH 4 )-acetylcarbamide - H 2 O at 25 deg C have been studied. It is ascertained, that the systems investigated are of simple eutonic type

9-{[4-(Dimethylaminobenzyl]amino}-5-(4-hydroxy-3,5-dimethoxyphenyl-5,5a,8a,9-tetrahydrofuro[3′,4′:6,7]naphtho[2,3-d][1,3]dioxol-6(8H-one methanol monosolvate

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Hong Chen

2011-11-01

Full Text Available In the title compound, C30H32N2O7·CH4O, the tetrahydrofuran ring and the six-membered ring fused to it both display envelope conformations, with the ring C atom opposite the carbonyl group and the adjacent bridgehead C atom as the flaps, respectively. In the crystal structure, intermolecular O—H...O hydrogen bonds link all moieties into ribbons along [010]. Weak intermolecular C—H...O interactions consolidate the crystal packing further.

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.

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

International Nuclear Information System (INIS)

Vaqueiro, Paz

2006-01-01

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

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

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R. Cortés

2010-03-01

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

(μ-3-Acetyl-5-carboxyl­ato-4-methyl­pyrazolido-1:2κ4 N 2,O 3:N 1,O 5)-μ-chlorido-tetra­pyridine-1κ2 N,2κ2 N-chlorido-1κCl-dicopper(II) propan-2-ol solvate

Science.gov (United States)

Malinkin, Sergey; Penkova, Larisa; Pavlenko, Vadim A.; Haukka, Matti; Fritsky, Igor O.

2009-01-01

The title compound, [Cu2(C7H6N2O3)Cl2(C5H5N)4]·C3H8O, is a binuclear pyrazolate complex, in which the two CuII atoms have different coordination numbers and are connected by a bridging Cl atom. One CuII atom has a distorted square-pyramidal coordination environment formed by two pyridine N atoms, one bridging Cl atom and an N,O-chelating pyrazolate ligand. The other CuII atom adopts an octa­hedral geometry defined by two pyridine N atoms at the axial positions, two Cl atoms and the coordinated pyrazolate ligand in the equatorial plane. An O—H⋯O hydrogen bond connects the complex mol­ecules and propan-2-ol solvent mol­ecules into pairs. These pairs form columns along the a axis. PMID:21577764

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.

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

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

Nd(BrO3)3-Yb(BrO3)3-H2O and Nd2(SeO4)3-Yb2(SeO4)3-H2O systems at 25 deg C

International Nuclear Information System (INIS)

Serebrennikov, V.V.; Batyreva, V.A.; Tsybukova, T.N.

1981-01-01

Using the methods of isothermal solubility the Nd(BrO 3 ) 3 - Yb(BrO 3 ) 3 -H 2 O and Nd 2 (SeO 4 ) 3 -Yb 2 (SeO 4 ) 3 -H 2 O systems are studied at 25 deg C. The compositions of the solid phases are determined by the method of ''residues''. The formation of two series of solid solutions in both systems is established. Besides, there is a crystallization region of Nd 2 (SeO 4 ) 3 in the system of selenates. The solubility diagrams of the systems are presented [ru

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.

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.

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

International Nuclear Information System (INIS)

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

2005-01-01

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

(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.

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.

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

N-Cyclohexyl-2-(5-fluoro-1H-indol-3-yl-2-oxoacetamide

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Dan-Li Tian

2011-07-01

Full Text Available In title compound, C16H17FN2O2, the cyclohexane ring adopts a chair conformation.. The crystal packing is stabilized by weak π–π stacking interactions [centroid–centroid distance = 3.503 (5 Å] and intermolecular C—H...O, N—H...O and N—H...F hydrogen-bond interactions.

rac-6-Hydroxy-4-(4-nitrophenyl-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

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Jian-Li Zhang

2010-11-01

Full Text Available The title compound, C16H12F3N3O5S·H2O, was prepared by reaction of 4-nitrobenzaldehyde, 4,4,4-trifluoro-1-(thiophen-2-ylbutane-1,3-dione and urea. The asymmetric unit contains two independent molecules, with essentially identical geometries and conformations. The dihydropyrimidine rings adopt a half-chair conformation. The dihedral angles between the benzene ring and the thiophene ring are 54.82 (8 and 58.72 (8° in the two molecules. The molecular conformation of one of the molecules is stabilized by two intramolecular O—H...O hydrogen bonds, generating an S(6 ring. The crystal structure is stabilized by intermolecular O—H...O and N—H...O hydrogen bonds.

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

Energy Technology Data Exchange (ETDEWEB)

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.

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.

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

Science.gov (United States)

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

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Mehmet Akkurt

2014-06-01

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

Siudaite, Na8(Mn2+ 2Na)Ca6Fe3+ 3Zr3NbSi25O74(OH)2Cl·5H2O: a new eudialyte-group mineral from the Khibiny alkaline massif, Kola Peninsula

Science.gov (United States)

Chukanov, Nikita V.; Rastsvetaeva, Ramiza K.; Kruszewski, Łukasz; Aksenov, Sergey M.; Rusakov, Vyacheslav S.; Britvin, Sergey N.; Vozchikova, Svetlana A.

2018-03-01

The new eudialyte-group mineral siudaite, ideally Na8(Mn2+ 2Na)Ca6Fe3+ 3Zr3NbSi25O74(OH)2Cl·5H2O, was discovered in a peralkaline pegmatite situated at the Eveslogchorr Mt., Khibiny alkaline massif, Kola Peninsula, Russia. The associated minerals are aegirine, albite, microcline, nepheline, astrophyllite, and loparite-(Ce). Siudaite forms yellow to brownish-yellow equant anhedral grains up to 1.5 cm across. Its lustre is vitreous, and the streak is white. Cleavage is none observed. The Mohs' hardness is 4½. Density measured by hydrostatic weighing is 2.96(1) g/cm3. Density calculated using the empirical formula is equal to 2.973 g/cm3. Siudaite is nonpleochroic, optically uniaxial, negative, with ω = 1.635(1) and ɛ = 1.626(1) (λ = 589 nm). The IR spectrum is given. The chemical composition of siudaite is (wt%; electron microprobe, H2O determined by HCN analysis): Na2O 8.40, K2O 0.62, CaO 9.81, La2O3 1.03, Ce2O3 1.62, Pr2O3 0.21, Nd2O3 0.29, MnO 6.45, Fe2O3 4.51. TiO2 0.54, ZrO2 11.67, HfO2 0.29, Nb2O5 2.76, SiO2 47.20, Cl 0.54, H2O 3.5, -O = Cl - 0.12, total 99.32. According to Mössbauer spectroscopy data, all iron is trivalent. The empirical formula (based on 24.5 Si atoms pfu, in accordance with structural data) is [Na7.57(H2O)1.43]Σ9(Mn1.11Na0.88Ce0.31La0.20Nd0.05Pr0.04K0.41)Σ3(H2O)1.8(Ca5.46Mn0.54)Σ6(Fe3+ 1.76Mn2+ 1.19)Σ2.95Nb0.65(Ti0.20Si0.50)Σ0.71(Zr2.95Hf0.04Ti0.01)Σ3Si24.00Cl0.47O70(OH)2Cl0.47·1.82H2O. The crystal structure was determined using single-crystal X-ray diffraction data. The new mineral is trigonal, space group R3m, with a = 14.1885(26) Å, c = 29.831(7) Å, V = 5200.8(23) Å3 and Z = 3. Siudaite is chemically related to georgbarsanovite and is its analogue with Fe3+-dominant M2 site. The strongest lines of the powder X-ray diffraction pattern [d, Å (I, %) (hkl)] are: 6.38 (60) (-114), 4.29 (55) (-225), 3.389 (47) (131), 3.191 (63) (-228). 2.963 (100) (4-15), 2.843 (99) (-444), 2.577 (49) (3-39). Siudaite is named after the Polish

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.

Standarization of Mn-54 by liquid scintillation counting using organic samples of (C8H15 O2)2 Mn-54

International Nuclear Information System (INIS)

1990-01-01

A new method of standardization of Mn 54 by liquid scintillation counting with an organic sample of (C 8 H 15 O 2 ) 2 Mn 54 is described. This procedure shows a good long term stability of samples, over 20 days, and counting efficiencies between 10% and 24% for PCS e INSTAGEL and 10% 32% for a toluene-based scintillator. The discrepancies between experimental and computed values are less that 0,9% for PCS and INSTAGEL and less than 1,2% for Toluene, in the 5-2,5 interval of quenching parameter. The global uncertainty on the activity concentrat-ion of a sample standardized by this method has been lower than 3% (Author)

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

Completing the series. New coordination networks of composition {sup 3}{sub ∞}[RE{sub 2}(ADC){sub 3}(H{sub 2}O){sub 6}].2H{sub 2}O with RE = Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Y and ADC{sup 2-} = acetylenedicarboxylate ({sup -}O{sub 2}C-C≡C-CO{sub 2}{sup -})

Energy Technology Data Exchange (ETDEWEB)

Gramm, Verena K.; Schuy, Andrea; Ruschewitz, Uwe [Institut fuer Anorganische Chemie, Koeln Univ. (Germany); Suta, Markus; Wickleder, Claudia [Anorganische Chemie, Universitaet Siegen (Germany); Sternemann, Christian [Fakultaet Physik / DELTA, Technische Universitaet Dortmund (Germany)

2018-02-01

The crystal structures of {sup 3}{sub ∞}[RE{sub 2}(ADC){sub 3}(H{sub 2}O){sub 6}].2H{sub 2}O (RE = Pr, Nd, Sm, Eu, Tb, Dy) were solved and refined from X-ray single crystal data. They crystallize in a structure type already known for RE = La, Ce and Gd (P1, no. 2, Z = 2), which is characterized by REO{sub 9} polyhedra forming dimeric units being the nodes of a 3D framework structure linked by ADC{sup 2-} anions ({sup -}O{sub 2}C-C≡C-CO{sub 2}{sup -} = acetylenedicarboxylate). From synchrotron powder diffraction data it was shown that isostructural coordination networks are formed for RE = Ho, Er, Y, whereas for RE = Tm, Yb, Lu a new structure type crystallizing in a highly complex crystal structure with a large orthorhombic unit cell is found. All compounds are obtained by slow evaporation of an aqueous solution containing RE(OAc){sub 3}.xH{sub 2}O and acetylenedicarboxylic acid (H{sub 2}ADC). The coordination networks of composition {sup 3}{sub ∞}[RE{sub 2}(ADC){sub 3}(H{sub 2}O){sub 6}].2H{sub 2}O were thoroughly investigated by thermal analysis and for RE = Eu, Tb, a strong red and green photoluminescence was observed and investigated by means of UV/Vis spectroscopy. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Magnesium hexafluoridozirconates MgZrF{sub 6}.5H{sub 2}O, MgZrF{sub 6}.2H{sub 2}O, and MgZrF{sub 6}. Structures, phase transitions, and internal mobility of water molecules

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Gerasimenko, Andrey V.; Gaivoronskaya, Kseniya A.; Slobodyuk, Arseny B.; Didenko, Nina A. [Institute of Chemistry, Russian Academy of Sciences, Vladivostok (Russian Federation)

2017-12-04

The MgZrF{sub 6}.nH{sub 2}O (n = 5, 2 and 0) compounds were studied by the methods of X-ray diffraction and {sup 19}F, MAS {sup 19}F, and {sup 1}H NMR spectroscopy. At room temperature, the compound MgZrF{sub 6}.5H{sub 2}O has a monoclinic C-centered unit cell and is composed of isolated chains of edge-sharing ZrF{sub 8} dodecahedra reinforced with MgF{sub 2}(H{sub 2}O){sub 4} octahedra and uncoordinated H{sub 2}O molecules and characterized by a disordered system of hydrogen bonds. In the temperature range 259 to 255 K, a reversible monoclinic <-> two-domain triclinic phase transition is observed. The phase transition is accompanied with ordering of hydrogen atoms positions and the system of hydrogen bonds. The structure of MgZrF{sub 6}.2H{sub 2}O comprises a three-dimensional framework consisting of chains of edge-sharing ZrF{sub 8} dodecahedra linked to each other through MgF{sub 4}(H{sub 2}O){sub 2} octahedra. The compound MgZrF{sub 6} belongs to the NaSbF{sub 6} type and is built from regular ZrF{sub 6} and MgF{sub 6} octahedra linked into a three-dimensional framework through linear Zr-F-Mg bridges. The peaks in {sup 19}F MAS spectra were attributed to the fluorine structural positions. The motions of structural water molecules were studied by variable-temperature {sup 1}H NMR spectroscopy. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

2-Phenyl-7-(4-pyridylmethylamino-1,2,4-triazolo[1,5-a][1,3,5]triazin-5(4H-oneFused heterocyclic systems with s-triazine ring. Part 17. For part 16, see Dolzhenko et al. (2011.

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Lip Lin Koh

2011-01-01

Full Text Available In the title compound, C16H13N7O, the 1,2,4-triazolo[1,5-a][1,3,5]triazine heterocyclic system is essentially planar (r.m.s. deviation = 0.0375 Å. The attached benzene ring lies almost in the mean plane of 1,2,4-triazolo[1,5-a][1,3,5]triazine [dihedral angle = 1.36 (23°], while the pyridine ring is turned out of this plane by the aminomethyl bridge [dihedral angle = 69.22 (9°]. The amino group H atom is involved in intramolecular hydrogen bonding with a triazole N atom. In the crystal, molecules are connected via C(=ONH...N hydrogen bonds into C(11 chains parallel to [100]. The amino group H atom acts as a hydrogen-bond donor, forming an NH...O=C hydrogen bond with the carbonyl O atom, which links the molecules into C(6 chains running along [011] and [01overline{1}].

ZrOCl2.8H2O as a green and efficient catalyst for the expeditious synthesis of substituted 3-arylpyrimido[4,5-c]pyridazines in water

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Mehdi Rimaz

2015-09-01

Full Text Available A new and simple synthetic methodology for the preparation of 3-arylpyrimido[4,5-c]pyridazine-5,7(6H,8H-diones and 3-aryl-5-oxo-7-thioxo-7,8-dihydropyrimido[4,5-c]pyridazin-5(6H-ones by a one-pot three component reaction of barbituric acid or thiobarbituric acid with arylglyoxals in the presence of catalytic amount of ZrOCl2∙8H2O as green Lewis acid and hydrazine hydrate at ambient temperature in water was reported. All of these pyrimidopyridazines derivatives have one clustered water molecule in their molecular structure. The use of ZrOCl2∙8H2O catalyst is feasible because of its easy availability, convenient handling, high stability, simple recovery, reusability, good activity and eco-friendly.

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

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Hoong-Kun Fun

2009-01-01

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

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.

Theoretical studies of the optical and EPR spectra for VO^{2+} in Na_3C_6H_5O_7·2H_2O single crystal

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Ch.-Y. Li

2015-06-01

Full Text Available On the basis of the perturbation formulas for a d^1 configuration ion in a tetragonal crystal field, the three optical absorption bands and electron paramagnetic resonance (EPR parameters (g factors g_i and hyperfine structure constants A_i for i = || and ⊥, respectively of VO^{2+} in Na_3C_6H_5O_7·2H_2O (TSCD single crystals were studied using the perturbation theory method. By simulating the calculated optical and EPR spectra to the observed values, local structure parameters and negative signs of the hyperfine structure constants A_i of the octahedral (VO_6^{8-} cluster in TSCD single crystal can be obtained.

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

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

1994-02-01

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

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.

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

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Ning-Juan Zheng

2012-04-01

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

(Dimethylformamide-κO(2-hydroxybenzoato-κ2O1,O1′[tris(1-methyl-1H-benzimidazol-2-ylmethyl-κN3amine-κN]manganese(II perchlorate dimethylformamide monosolvate

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Baoliang Qi

2010-10-01

Full Text Available In the title complex, [Mn(C7H5O3(C27H27N7(C3H7NO]ClO4·C3H7NO, the MnII ion is coordinated in a slightly distorted monocapped trigonal-prismatic geometry. The tris(1-methyl-1H-benzimidazol-2-ylmethylamine (Mentb ligand coordinates in a tetradentate mode and the coordination is completed by a bis-chelating salicylate ligand and a dimethylformamide ligand. The hydroxy group and the ortho H atoms of the salicylate ligand were refined as disordered over two sites with occupancies of 0.581 (8 and 0.419 (8. Both disorder components of the hydroxy group form intramolecular O—H...O hydrogen bonds.

Crystal structure of trans-di-chloridobis-[N-(5,5-di-methyl-4,5-di-hydro-3H-pyrrol-2-yl-κN)acetamide]palladium(II) dihydrate.

Science.gov (United States)

Lasri, Jamal; Eltayeb, Naser Eltaher; Haukka, Matti; Babgi, Bandar A

2017-04-01

The title complex, [PdCl 2 (C 8 H 14 N 2 O) 2 ]·2H 2 O, was obtained by N-O bond cleavage of the oxa-diazo-line rings of the trans -[di-chlorido-bis-(2,5,5-trimethyl-5,6,7,7a-tetra-hydro-pyrrolo-[1,2- b ][1,2,4]oxa-diazole- N 1 )]palladium(II) complex. The palladium(II) atom exhibits an almost square-planar coordination provided by two trans -arranged chloride anions and a nitro-gen 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 mol-ecules into double layers parallel to the bc plane.

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.

Dicarbonyl[2-hydroxy-3,5,7-tris(morpholinomethylcyclohepta-2,4,6-trienonato(1–-κ2O1,O2]rhodium(I

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G. Steyl

2008-12-01

Full Text Available In the title compound, [Rh(C22H32N3O5(CO2], the RhI atom is coordinated by two carbonyl ligands and two tropolonate O atoms in a distorted square-planar geometry. It is an example of a new type of tropolone derivative that has not been characterized via solid-state methods. Weak intramolecular C—H...N and intermolecular C—H...O hydrogen bonds, and π–π stacking interactions between the tropolone rings [centroid–centroid distance = 3.590 (8 Å] are observed in the crystal structure.

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

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Erik Hennings

2014-12-01

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

Theoretical characterizations of novel C2H5O+ reactions

Science.gov (United States)

Hudson, Charles E.; McAdoo, David J.

2004-03-01

Assorted reactions of C2H5O+ isomers are characterized by theory, including tracing their courses by means of intrinsic reaction coordinate computations. We establish that CH3CH=OH+ eliminates methane by transferring H from oxygen to a methyl hydrogen and then to the CC bond to produce CHO++CH4. This adds to the limited knowledge of the involvement of hypervalent structures in the reactions of cations in the gas phase. Second, we characterized the course of CH3CH=OH+-->H3O++HC[triple bond; length as m-dash]CH. In this dissociation, H first migrates from the methyl to the oxygen to give O-protonated vinyl alcohol, a stable intermediate. Then the H2O swings outward to over the middle of the CC bond while one of the two hydrogens on the non-O-bearing carbon revolves to between the oxygen and the two carbons, leading to formation of a [H3O+ HC[triple bond; length as m-dash]CH] complex. This complex contains sufficient energy to dissociate its partners because a high barrier is crossed in its formation. Third, we found that methane elimination from CH3O+=CH2 involves stretching of the CH3---O bond and then rotation of the methyl so that a methyl hydrogen is pointed directly toward the oxygen. This reaction is completed by further rotation of the methyl to abstract a methylene hydrogen to the opposite side of the methyl from that initially bonded to oxygen. This clearly establishes that this dissociation takes place through an ion-neutral complex. Each of the reaction coordinates for the three preceding reactions traverses a novel bonding stage involving H, evidence that such are not unusual in gas phase ion chemistry. Finally, we showed that in the rearrangement CH3O+=CH2-->CH2=O+CH3, before Ht is transferred CH2 rotates around the C=C bond from being in the skeletal plane to being perpendicular to it, and Ht remains in the skeletal plane throughout its transfer. This pathway appears to balance avoiding an orbital symmetry-forbidden suprafacial transition state with

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

African Journals Online (AJOL)

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

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.

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.

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)

Carbonate hydrates of the heavy alkali metals: preparation and structure of Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O und Cs{sub 2}CO{sub 3} . 3 H{sub 2}O; Carbonat-Hydrate der schweren Alkalimetalle: Darstellung und Struktur von Rb{sub 2}CO{sub 3} . 1,5 H{sub 2}O und Cs{sub 2}CO{sub 3} . 3 H{sub 2}O

Energy Technology Data Exchange (ETDEWEB)

Cirpus, V.; Wittrock, J.; Adam, A. [Koeln Univ. (Germany). Inst. fuer Anorganische Chemie

2001-03-01

Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O and Cs{sub 2}CO{sub 3} . 3 H{sub 2}O were prepared from aqueous solution and by means of the reaction of dialkylcarbonates with RbOH and CsOH resp. in hydrous alcoholes. Based on four-circle diffractometer data, the crystal structures were determined (Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O: C2/c (no. 15), Z = 8, a = 1237.7(2) pm, b = 1385.94(7) pm, c = 747.7(4) pm, {beta} = 120.133(8) , V{sub EZ} = 1109.3(6) . 10{sup 6} pm{sup 3}; Cs{sub 2}CO{sub 3} . 3 H{sub 2}O: P2/c (no. 13), Z = 2, a = 654.5(2) pm, b = 679.06(6) pm, c = 886.4(2) pm, {beta} = 90.708(14) , V{sub EZ} = 393.9(2) . 10{sup 6} pm{sup 3}). Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O is isostructural with K{sub 2}CO{sub 3} . 1.5 H{sub 2}O. In case of Cs{sub 2}CO{sub 3} . 3 H{sub 2}O no comparable structure is known. Both structures show {sub {infinity}}{sup 1}[(CO{sub 3}{sup 2-})(H{sub 2}O)]-chains, being connected via additional H{sub 2}O forming columns (Rb{sub 2}CO{sub 3} . 1.5 H{sub 2}O) and layers (Cs{sub 2}CO{sub 3} . 3 H{sub 2}O), respectively. (orig.)

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-05-15

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

2-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.

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

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Vahan Martirosyan

2008-03-01

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

Redetermination of Ce[B5O8(OH(H2O]NO3·2H2O

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Ya-Xi Huang

2012-05-01

Full Text Available The crystal structure of Ce[B5O8(OH(H2O]NO3·2H2O, cerium(III aquahydroxidooctaoxidopentaborate nitrate dihydrate, has been redetermined from single-crystal X-ray diffraction data. In contrast to the previous determination [Li et al. (2003. Chem. Mater. 15, 2253–2260], the present study reveals the location of all H atoms, slightly different fundamental building blocks (FBBs of the polyborate anions, more reasonable displacement ellipsoids for all non-H atoms, as well as a model without disorder of the nitrate anion. The crystal structure is built from corrugated polyborate layers parallel to (010. These layers, consisting of [B5O8(OH(H2O]2− anions as FBBs, stack along [010] and are linked by Ce3+ ions, which exhibit a distorted CeO10 coordination sphere. The layers are additionally stabilized via O—H...O hydrogen bonds between water molecules and nitrate anions, located at the interlayer space. The [BO3(H2O]-group shows a [3 + 1] coordination and is considerably distorted from a tetrahedral configuration. Bond-valence-sum calculation shows that the valence sum of boron is only 2.63 valence units (v.u. when the contribution of the water molecule (0.49 v.u. is neglected.

1-[3-(4-Chlorophenyl-5-(4-methoxyphenyl-4,5-dihydro-1H-pyrazol-1-yl]ethanone

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Hoong-Kun Fun

2012-04-01

Full Text Available In the title compound, C18H17ClN2O2, the benzene rings form dihedral angles of 6.69 (6 and 74.88 (5° with the 4,5-dihydro-1H-pyrazole ring. The benzene rings form a dihedral angle of 76.67 (5° with each other. In the crystal, molecules are linked via bifurcated (C,C–H...O hydrogen bonds into chains along [010]. The crystal structure is further consolidated by C—H...π interactions.

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.

Di-μ-chlorido-bis({4-[bis(trimethylsilylamino]-6-chloro-2,2,8,8-tetramethyl-5,7-bis(trimethylsilyl-3,5,7-triaza-4,6-diphospha-2,8-disilanon-3-en-4-ido-κ2P,P′}palladium(II diethyl ether disolvate

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Martha Höhne

2016-06-01

Full Text Available The title compound, [Pd2(C18H54Cl2N4P2Si62Cl2]·2C4H10O, features a dinuclear chloride-bridged palladium complex bearing two equivalents of the novel monoanionic mixed valent (λ3-P—N—(λ5-P ligand. A metal catalyzed coupling of two aminoiminophosphines and a shift of one chlorine from the metal to the phosphorus results in the (λ3-P—N—(λ5-P ligand. The molecule contains a planar bimetallic Pd2Cl2 core with a crystallographic centre of inversion at the mid-point of the Pd...Pd line. The Pd atoms are in a distorted square-planar arrangement, where the P/Pd/P and Cl/Pd/Cl planes are twisted with respect to each other by a dihedral angle of 7.57 (4°. The P—Pd—P bite angle is 71.380 (18°. Intramolecular C—H...Cl interactions are observed. In the crystal, the diethyl ether solvent molecule is disordered over two sites, with an occupancy ratio of 0.788 (5:0.212 (5.

Aquachloridobis[5-(2-pyridyl-1H-tetrazolato-κN1]iron(III

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Bo Wang

2009-08-01

Full Text Available The title compound, [Fe(C6H4N52Cl(H2O], was synthesized by hydrothermal reaction of FeCl3 with 2-(1H-tetrazol-5-ylpyridine. The iron(III metal centre exhibits a distorted octahedral coordination geometry provided by four N atoms from two bidentate organic ligands, one water O atom and one chloride anion. The pyridine and tetrazole rings are nearly coplanar [dihedral angles = 4.32 (15 and 5.04 (14°]. In the crystal structure, intermolecular O—H...N hydrogen bonds link the complex molecules into a two-dimensional network parallel to (100.

N-{2-[2-(5-Methyl-1H-pyrazol-3-ylacetamido]phenyl}benzamide monohydrate

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Karim Chkirate

2017-02-01

Full Text Available The asymmetric unit of the title compound, C19H18N4O2·H2O, comprises the U-shaped pyrazole derivative and a solvent water molecule. The molecular conformation is partly determined by an intramolecular N—H...O hydrogen bond. The crystal packing is directed by an extensive network of O—H...O, N—H...O, N—H...N and C—H...O hydrogen bonds together with C—H...π(ring contacts that generate a three-dimensional network.

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.

Photodissociation of van der Waals clusters of isoprene with oxygen, C{sub 5}H{sub 8}-O{sub 2}, in the wavelength range 213-277 nm

Energy Technology Data Exchange (ETDEWEB)

Vidma, Konstantin V.; Frederix, Pim W. J. M.; Parker, David H. [Institute for Molecules and Materials, Radboud University Nijmegen, Heyendaalseweg 135, 6525 ED Nijmegen (Netherlands); Baklanov, Alexey V. [Institute of Chemical Kinetics and Combustion, Institutskaja Street 3, Novosibirsk 630090 (Russian Federation) and Novosibirsk State University, Pirogova street 2, Novosibirsk 630090 (Russian Federation)

2012-08-07

The speed and angular distribution of O atoms arising from the photofragmentation of C{sub 5}H{sub 8}-O{sub 2}, the isoprene-oxygen van der Waals complex, in the wavelength region of 213-277 nm has been studied with the use of a two-color dissociation-probe method and the velocity map imaging technique. Dramatic enhancement in the O atoms photo-generation cross section in comparison with the photodissociation of individual O{sub 2} molecules has been observed. Velocity map images of these 'enhanced' O atoms consisted of five channels, different in their kinetic energy, angular distribution, and wavelength dependence. Three channels are deduced to be due to the one-quantum excitation of the C{sub 5}H{sub 8}-O{sub 2} complex into the perturbed Herzberg III state ({sup 3}{Delta}{sub u}) of O{sub 2}. This excitation results in the prompt dissociation of the complex giving rise to products C{sub 5}H{sub 8}+O+O when the energy of exciting quantum is higher than the complex photodissociation threshold, which is found to be 41740 {+-} 200 cm{sup -1} (239.6{+-}1.2 nm). This last threshold corresponds to the photodissociation giving rise to an unexcited isoprene molecule. The second channel, with threshold shifted to the blue by 1480 {+-} 280 cm{sup -1}, corresponds to dissociation with formation of rovibrationally excited isoprene. A third channel was observed at wavelengths up to 243 nm with excitation below the upper photodissociation threshold. This channel is attributed to dissociation with the formation of a bound O atom C{sub 5}H{sub 8}-O{sub 2}+hv{yields} C{sub 5}H{sub 8}-O{sub 2}({sup 3}{Delta}{sub u}) {yields} C{sub 5}H{sub 8}O + O and/or to dissociation of O{sub 2} with borrowing of the lacking energy from incompletely cooled complex internal degrees of freedom C{sub 5}H{sub 8}{sup *}-O{sub 2}+hv{yields} C{sub 5}H{sub 8}{sup *}-O{sub 2}({sup 3}{Delta}{sub u}) {yields} C{sub 5}H{sub 8}+ O + O. The kinetic energy of the O atoms arising in two other

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

Science.gov (United States)

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.

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

Energy Technology Data Exchange (ETDEWEB)

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

Methyl 2-(1a,4a-dimethyl-2,8-dioxo-2,3,4,4a,5,6,7,8-octahydro-1aH-1-oxacyclopropa[d]naphthalen-7-ylacrylate

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Mohamed Tebbaa

2012-02-01

Full Text Available The title compound, C16H20O5, was synthesized from ilicic acid [2-(8-hydroxy-4a,8-dimethyldecahydronaphthalen-2-ylacrylic acid], which was isolated from the chloroform extract of the aerial part of Inula viscose (L Aiton [or Dittrichia viscosa (L Greuter]. The molecule is built up from two fused six-membered rings, the epoxidized six-membered ring adopts a half-chair conformation while the other ring displays a perfect chair conformation. The crystal structure features C—H...O hydrogen bonds.

Solubility of NaNd(CO3)2.6H2O(c) in concentrated Na2CO3 and NaHCO3 solutions

International Nuclear Information System (INIS)

Rao, L.; Rai, D.; Felmy, A.R.; Fulton, R.W.; Novak, C.F.

1996-01-01

NaNd(CO 3 ) 2 x 6 H 2 O(c) was identified to be the final equilibrium solid phase in suspensions containing concentrated sodium carbonate (0.1 to 2.0 M) and sodium bicarbonate (0.1 to 1.0 M), with either NaNd(CO 3 ) 2 x 6 H 2 O(c) or Nd 2 (CO 3 ) 3 x xH 2 O(s) as initial solids. A thermodynamic model, based on Pitzer's specific into-interaction approach, was developed to interpret the solubility of NaNd(CO 3 ) 2 x 6 H 2 O(c) as functions of sodium carbonate and sodium bicarbonate concentrations. In this model, the solubility data of NaNd(CO 3 ) 2 x 6 H 2 O(c) were explained by assuming the formation of NdCO 3 + , Nd(CO 3 ) 2 - and Nd(CO 3 ) 3 3- species and invoking the specific ion interactions between Na + and Nd(CO 3 ) 3 3- . Ion interaction parameters for Na + -Nd(CO 3 ) 3 3- were developed to fit the solubility data. Based on the model calculations, Nd(CO 3 ) 3 3- was the predominant aqueous neodymium species in 0.1 to 2 M sodium carbonate and 0.1 to 1 M sodium bicarbonate solutions. The logarithm of the NaNd(CO 3 ) 2 x 6 H 2 O solubility product (NaNd(CO 3 ) 2 x 6 H 2 O(c)=Na + +Nd 3+ +2 CO 3 2- +6 H 2 O) was calculated to be -21.39. This model also provided satisfactory interpretation of the solubility data of the analogous Am(III) system in less concentrated carbonate and bicarbonate solutions. (orig.)

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.

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

4-(4-Chlorophenyl-6-hydroxy-5-(2-thienylcarbonyl-6-(trifluoromethyl-3,4,5,6-tetrahydropyrimidin-2(1H-one monohydrate

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Mohammad Hossein Mosslemin

2009-06-01

Full Text Available The asymmetric unit of the title compound, C16H12ClF3N2O3S·H2O, contains two crystallographically independent organic molecules and two water molecules. The organic species are linked by an intermolecular O—H...O hydrogen bond, while the water molecules are connected to them through intermolecular O—H...N hydrogen bonds. The thiophene and phenyl rings are oriented at dihedral angles of 62.35 (4 in the first independent molecule and 60.74 (5° in the second, while the pyrimidine rings adopt twisted conformations in both molecules. Intramolecular N—H...F interactions result in the formation of two five-membered rings having envelope conformations. In the crystal structure, further intermolecular O—H...O and N—H...O hydrogen bonds link the molecules into chains.

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

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

Science.gov (United States)

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

2008-10-18

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

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

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

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Michael J. Ferguson

2008-10-01

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

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

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Hoong-Kun Fun

2010-07-01

Full Text Available The title Schiff base compound, C22H24IN3O2, adopts an E configuration about the central C=N bond. The pyrazolone ring makes a dihedral angle of 49.68 (10° with its attached phenyl ring. The phenolate plane makes dihedral angles of 16.78 (9 and 50.54 (9°, respectively, with the pyrazolone ring and the terminal phenyl ring. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, an intermolecular C—H...O hydrogen bond is also observed.

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.

A novel fluffy nanostructured 3D network of Ni(C7H4O5) for supercapacitors

International Nuclear Information System (INIS)

Chen, Qiulin; Lei, Shuijin; Chen, Lianfu; Deng, Peiqin; Xiao, Yanhe; Cheng, Baochang

2017-01-01

Highlights: • The fluffy 3D network of Ni(C 7 H 4 O 5 ) complex is firstly prepared on Ni foam. • The fluffy 3D network shows high areal capacitance and excellent cycle stability. • The fluffy network has large superior pseudocapacitive performance than the powder. • An asymmetric supercapacitor with high capacitance and energy density is assembled. - Abstract: Supercapacitors have raised considerable research interest in recent years due to their extensive potential application in next-generation energy storage. It is always of great importance to develop new electrode materials for supercapacitors so far. In this research, nickel gallate complex (Ni(C 7 H 4 O 5 )) nanostructures are successfully grown on nickel foam by a facile hydrothermal route, which can be directly used as the electrodes for supercapacitors. X-ray diffraction patterns show that the sample is amorphous. The scanning electron microscopy images reveal that the products consist of novel fluffy 3D network with a mass of fibers. The electrochemical measurements demonstrate that the prepared Ni(C 7 H 4 O 5 ) electrode possesses the specific capacitance of 3.688 F cm −2 (1229.3 F g −1 ) at a current density of 9 mA cm −2 (3 A g −1 ). It presents an excellent cycling stability with a capacitance retention of 87.9% after 5000 cycles even at a very high current density of 40 mA cm −2 . An asymmetric supercapacitor device is assembled using the Ni(C 7 H 4 O 5 ) sample as positive electrode and activated carbon as negative one. A high gravimetric capacitance of 71.4 F g −1 at a current density of 0.5 A g −1 can be achieved. The fabricated device delivers the highest energy density of 23.8 W h kg −1 at a power density of 388.2 W kg −1 with a voltage window of 1.55 V. This strategy should be extended to other organometallic compounds for supercapacitors.

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

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Ying-Ying Liu

2011-11-01

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

(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.

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

International Nuclear Information System (INIS)

Jagannatha Swamy, S.

2002-01-01

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

Competition between weak OH···π and CH··O hydrogen bonds: THz spectroscopy of the C2H2—H2O and C2H4—H2O complexes

DEFF Research Database (Denmark)

Andersen, Jonas; Heimdal, Jimmy; Nelander, B.

2017-01-01

an intermolecular CH⋯O hydrogen-bonded configuration of C2v symmetry with the H2O subunit acting as the hydrogen bond acceptor. The observation and assignment of two large-amplitude donor OH librational modes of the C2H4—H2O complex at 255.0 and 187.5 cm−1, respectively, confirms an intermolecular OH⋯π hydrogen...

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

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Mehmet Karakus

2012-04-01

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

3-Ethyl-5-(4-methoxyphenoxy-2-(pyridin-4-yl-3H-imidazo[4,5-b]pyridine

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S. Ranjith

2011-07-01

Full Text Available In the title compound, C20H18N4O2, the imidazopyridine fused ring system is almost perpendicular to the benzene ring [dihedral angle = 87.6 (5°]. The pyridine ring makes a dihedral angle of 35.5 (5° with the mean plane of the imidazopyridine fragment. The crystal structure is stabilized by an aromatic π–π stacking interaction between the phenyl rings of neighbouring molecules [centroid–centroid distance = 3.772 (2 Å, interplanar distance = 3.546 (2 Å and slippage = 1.286 (2 Å].

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-03-15

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

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

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Andya Nemati

2008-10-01

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

[2,6-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.

A two-dimensional CdII coordination polymer: poly[diaqua[μ3-5,6-bis(pyridin-2-ylpyrazine-2,3-dicarboxylato-κ5O2:O3:O3,N4,N5]cadmium

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Monserrat Alfonso

2016-09-01

Full Text Available The reaction of 5,6-bis(pyridin-2-ylpyrazine-2,3-dicarboxylic acid with cadmium dichloride leads to the formation of the title two-dimensional coordination polymer, [Cd(C16H8N4O4(H2O2]n. The metal atom is sevenfold coordinated by one pyrazine and one pyridine N atom, two water O atoms, and by two carboxylate O atoms, one of which bridges two CdII atoms to form a Cd2O2 unit situated about a centre of inversion. Hence, the ligand coordinates to the cadmium atom in an N,N′,O-tridentate and an O-monodentate manner. Within the polymer network, there are a number of O—H...O hydrogen bonds present, involving the water molecules and the carboxylate O atoms. There are also C—H...N and C—H...O hydrogen bonds present. In the crystal, the polymer networks lie parallel to the bc plane. They are aligned back-to-back along the a axis with the non-coordinating pyridine rings directed into the space between the networks.

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

MeB/sub 5/O/sub 8/(Me-Li, Na, K, NH/sub 4/)-H/sub 2/NCONHCOCH/sub 3/-H/sub 2/O system at 25 deg C

Energy Technology Data Exchange (ETDEWEB)

Skvortsov, V G; Fedorov, Yu A; Molodkin, A K; Tsekhanskij, R S

1986-06-01

Using the methods of isothermal solubility, densi- and refractometry, systems MB/sub 5/O/sub 8/ (M-Li, Na, K, NH/sub 4/)-acetylcarbamide - H/sub 2/O at 25 deg C have been studied. It is ascertained, that the systems investigated are of simple eutonic type.

2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

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YuanQi Yu

2011-10-01

Full Text Available The asymmetric unit of the title compound, C8H9N2+·C8H5O4−, contains two independent ion pairs. In each 2-methyl-1H-benzimidazolium ion, an intramolecular O—H...O bond forms an S(7 graph-set motif. In the crystal, the components are linked by N—H...O hydrogen bonds, forming chains along [210]. Further stabilization is provided by weak C—H...O hydrogen bonds.

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.

Synthesis and investigation of aluminium uranium-containing compounds of Al[B5UO6]2[OH]·nH2O (B5=P, As) composition

International Nuclear Information System (INIS)

Chernorukov, N.G.; Sulejmanov, E.V.; Barch, S.V.

2001-01-01

The technique of synthesis of hydroxyuranophosphate and hydroxyuranoarsenate of aluminium is developed. Hydroxyuranophosphates and hydroxyuranoarsenates of aluminium are prepared by reaction of interaction of aqueous solutions of orthophosphoric (orthoarsenic) acid (0.05 mol/l), uranyl nitrate (0.05 mol/l) and aluminium nitrate (0.1 mol/l) at 20 Deg C. Peculiarities of the structure and thermal degradation reactions are studied by the methods of x-ray diffraction, IR spectroscopy, thermography. It is shown that in dependence on outer conditions in the systems Al[PUO 6 ] 2 ·[OH]·nH 2 O and Al[AsUO 6 ] 2 ·[OH]·nH 2 O crystal hydrates with hydrate numbers n=3-11(13) and anhydrous compounds form. The compounds have laminated type of lattice. Two-dimensional layers of [P(As)UO 6 ] ∞ n- are the basis of anion sublattice of these compounds. Aluminium in coordination surrounding of hydroxy groups and water molecules forms cationic sublattice [ru

Crystallization of rare earth germanates in the K2O-Ln2O3-GeO2-H2O at 280 deg C

International Nuclear Information System (INIS)

Panasenko, E.B.; Begunova, R.G.; Sklokina, N.F.

1980-01-01

Crystallization of rare earth germanates in potassium hydroxide solutions is studied at 280 deg C. Stability limits for different crystalline phases are established. Diorthogermanates Ln 2 O 3 x2GeO 3 (three structural modifications) are formed with all lanthanides except lanthanum. Germanates-apatites 7Ln 2 O 3 x9GeO 2 are characteristic for ''large'' lanthanides La-Nd. Alkali germanate of the composition 0.5 K 2 OxLn 2 O 3 xGeO 2 xnH 2 O is realized with the elements of the end of rare earth series, i.e., Tm-Lu. Some properties of the germanates synthesized are considered [ru

3,4-Dibromo-2,2,5,5-tetraphenyl-2,5-dihydrofuran

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Nadine Seidel

2018-04-01

Full Text Available The crystal structure of the title compound, C28H20Br2O, was solved in the orthorhombic space group P212121 with one molecule in the asymmetric unit. The phenyl rings are nearly planar and inclined at angles of 67.7 (1, 68.8 (1, 79.3 (1 and 62.3 (1° to the plane of the 2,5-dihydrofuran ring. The crystal structure features C—H...π and Br...Br interactions, which connect the molecules to a three-dimensional supramolecular network.

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,...

Total scattering cross-sections for the systems nH2 + nH2, pH2 + pH2, nD2 + nD2, oD2 + oD2 and HD + HD for relative energies below ten milli-electron volts

International Nuclear Information System (INIS)

Johnson, D.L.

1979-01-01

Relative total scattering cross sections for nH 2 + nH 2 , pH 2 + pH 2 , nD 2 + nD 2 , oD 2 + oD 2 , and HD + HD were measured with inclined nozzle beams derived from nozzle sources and intersecting at 21 0 . Both nozzles could be varied in temperature from 4.2K to 300K to provide the velocity range for the cross sections. The use of a parahydrogen converter allowed the measurement of the pH 2 + pH 2 and oD 2 + oD 2 cross sections. Cross sections for the H 2 + H 2 were measured over a relative velocity range of 200 m/s to 1450 m/s. The nH 2 + nH 2 results show an undulation in the velocity range between 350 m/s and 400 m/s that corresponds to a l = 3 orbiting resonance. Analysis of the pH 2 + pH 2 cross section indicates a l = 4 orbiting resonance near 586 m/s. This resonance has a peak energy of 1.79 meV and a measured energy width of 1.05 meV, both which agree well with theoretical predictions. The D 2 + D 2 cross sections have been measured in the velocity range between 190 m/s and 1000 m/s. No orbiting resonances have been observed, but in the oD 2 + oD 2 cross section a deep minimum between the l = 4 and the l = 5 resonances at low velocities is clearly suggested. Initial measurements of the HD + HD cross section suggests the presence of the l = 4 orbiting resonance near a relative velocity of 300 m/s. The experimental results for each system were normalized to the total cross sections, which were convoluted to account for experimental velocity and angular dispersions. Three different potentials were considered, but a chi-square fit of the data indicates that the Schaefer and Meyer potential, which has been theoretically obtained from first principles, provides the best overall description of the hydrogen systems in the low collisional energy range

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

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Maxym O. Plutenko

2012-12-01

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

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

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

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Şamil Işık

2009-12-01

Full Text Available All the non-H atoms of the title compound, C10H10N4O3, are almost coplanar, the maximum deviation from planarity being 0.065 (3 Å. The dihedral angle between the aromatic rings is 1.66 (6°. The molecule adopts the enol–imine tautomeric form with an intramolecular hydrogen-bonding interaction between the Schiff base N atom and the hydroxy group. In the crystal, intermolecular N—H...O and O—H...O hydrogen bonds link the molecules into a three-dimensional network.

catena-Poly[[[diaqua(2-fluorobenzoato-κ2O,O′strontium]-μ3-2-fluorobenzoato-κ5O:O,O′:O′,F] monohydrate

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Zhu-Nian Jin

2011-04-01

Full Text Available In the title compound, {[Sr(C7H4FO22(H2O2]·H2O}n, the SrII atom is coordinated by six O atoms and one F atom from four 2-fluorobenzoate ligands and two water molecules, resulting in an irregular SrFO8 coordination environment. The μ3-2-fluorobenzoate ligand bridges three symmetry-related SrII atoms, giving rise to a chain structure extending along [010]. The polymeric chains are connected via O—H...O hydrogen bonds into a two-dimensional supramolecular structure parallel to (100.

(Acetato-κO(aqua-κO(2-{bis[(3,5-dimethyl-1H-pyrazol-1-yl-κN2methyl]amino-κN}ethanol-κOnickel(II perchlorate monohydrate

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Jia Zhou

2012-04-01

Full Text Available In the structure of the title complex, [Ni(CH3CO2(C14H23N5O(H2O]ClO4·H2O, the NiII centre has a distorted octahedral environment defined by one O and three N atoms derived from the tetradentate ligand, and two O atoms, one from a water molecule and the other from an acetate anion. The molecules are connected into a three-dimensional architecture by O—H...O hydrogen bonds. The perchlorate anion is disordered over two positions; the major component has a site-occupancy factor of 0.525 (19.

The MgSeO4-UO2SeO4-H2O system at 25 deg C

International Nuclear Information System (INIS)

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

1984-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

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Hualing Zhu

2011-07-01

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

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.

Poly[aqua-μ-bromido-(μ2-5-methylpyrazine-2-carboxylato-κ4N1,O2:O2,O2′lead(II

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Pan Yang

2012-09-01

Full Text Available In the title coordination polymer, [PbBr(C6H5N2O2(H2O]n, the PbII atom is coordinated by one pyrazine N atom, two bridging Br atoms, a water molecule and three carboxylate O atoms. Bridging by the two anions generates a layer structure parallel to (001; the layers are linked by O—H...N and O—H...Br hydrogen bonds, forming a three-dimensional network. The lone pair is stereochemically active, resulting in a Ψ-dodecahedral coordination environment for PbII.

Subsolidus phase relations of Bi2O3-Nd2O3-CuO

International Nuclear Information System (INIS)

Sun Yezhou

1997-01-01

The subsolidus phase relations of the Bi 2 O 3 -Nd 2 O 3 -CuO ternary system and its binary systems along with crystallographic parameters of the compounds were investigated by X-ray powder diffraction and differential thermal analysis. The room temperature section of the phase diagram of the Bi 2 O 3 -Nd 2 O 3 -CuO system can be divided into two diphase regions and six triphase regions. No ternary compound was found. There exist two solid solutions (α, β) and a compound Bi 0.55 Nd 0.45 O 1.5 in the (Bi 2 O 2 ) 1-x (Nd 2 O 3 ) x system. Both solid solution α (0.05≤x≤0.30) and β (0.53≤x≤0.73) belong to the rhombohedral system (R3m). The lattice parameters represented by a hexagonal cell are a=3.9832(4), c=27.536(5) A for Bi 0.8 Nd 0.2 O 1.5 (α phase) and a=3.8826(3), c=9.727(1) A for Bi 0.4 Nd 0.8 O 1.5 (β phase). The Bi 0.55 Nd 0.45 O 1.5 compound crystallizes in a face-centered cubic (f.c.c.) lattice with a=5.5480(2) A. (orig.)