Rahman ML, Mohd Yusoff M, Ismail J
… +2 more, Kwong HC, Quah CK
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552976
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The title compound, C16H14N2O3, has an E conformation about the azo-benzene [-N=N- = 1.2481 (16) Å] linkage. The benzene rings are almost coplanar [dihedral angle = 1.36 (7)°]. The O atoms of the carb-oxy-lic acid group...The title compound, C16H14N2O3, has an E conformation about the azo-benzene [-N=N- = 1.2481 (16) Å] linkage. The benzene rings are almost coplanar [dihedral angle = 1.36 (7)°]. The O atoms of the carb-oxy-lic acid group are disordered over two sets of sites and were refined with an occupancy ratio of 0.5:0.5. The two disordered components of the carb-oxy-lic acid group make dihedral angles of 1.5 (14) and 3.8 (12)° with the benzene ring to which they are attached. In the crystal, mol-ecules are linked via pairs of O-H⋯O hydrogen bonds, forming inversion dimers. The dimers are connected via C-H⋯O hydrogen bonds, forming ribbons lying parallel to [120]. These ribbons are linked via C-H⋯π inter-actions, forming slabs parallel to (001).
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552975
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The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hy...The synthesis, crystal structure, and FT-IR data for the title compound, [Na2Mn4(C2H2ClO2)2(C7H4NO3)4(C3H7NO)6]·2C3H7NO or Na2(O2CCH2Cl)2[12-MCMn(III) N(shi)-4](DMF)6·2DMF, where MC is metallacrown, shi(3-) is salicyl-hydroximate, and DMF is N,N-di-methyl-formamide, is reported. The macrocyclic metallacrown consists of an -[Mn(III)-N-O]4- ring repeat unit and the metallacrown captures two Na(+) ions in the central cavity above and below the plane of the metallacrown. Each Na(+) ion is seven-coordinate and is bridged to two ring Mn(III) ions, through either a coordinating DMF mol-ecule or a chloro-acetate anion. The ring Mn(III) ions have either a tetra-gonally distorted octa-hedral geometry or a distorted square-pyramidal geometry. Weak C-H⋯O inter-actions, in addition to pure van der Waals forces, contribute to the overall packing of the mol-ecules. The complete molecule has inversion symmetry and is disordered over two sets of sites with an occupancy ratio of 0.8783 (7):0.1217 (7). The solvent molecule is also disordered over two sets of sites, with an occupancy ratio of 0.615 (5):0.385 (5).
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552974
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The title compounds, calcium perchlorate tetra-hydrate and calcium perchlorate hexa-hydrate, were crystallized at low temperatures according to the solid-liquid phase diagram. The structure of the tetra-hydrate consists...The title compounds, calcium perchlorate tetra-hydrate and calcium perchlorate hexa-hydrate, were crystallized at low temperatures according to the solid-liquid phase diagram. The structure of the tetra-hydrate consists of one Ca(2+) cation eightfold coordinated in a square-anti-prismatic fashion by four water mol-ecules and four O atoms of four perchlorate tetra-hedra, forming chains parallel to [01-1] by sharing corners of the ClO4 tetra-hedra. The structure of the hexa-hydrate contains two different Ca(2+) cations, each coordinated by six water mol-ecules and two O atoms of two perchlorate tetra-hedra, forming [Ca(H2O)6(ClO4)]2 dimers by sharing two ClO4 tetra-hedra. The dimers are arranged in sheets parallel (001) and alternate with layers of non-coordinating ClO4 tetra-hedra. O-H⋯O hydrogen bonds between the water mol-ecules as donor and ClO4 tetra-hedra and water mol-ecules as acceptor groups lead to the formation of a three-dimensional network in the two structures. Ca(ClO4)2·6H2O was refined as a two-component inversion twin, with an approximate twin component ratio of 1:1 in each of the two structures.
Wagner T, Christiansen N, Hrib CG
… +2 more, Kaufmann DE, Edelmann FT
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552973
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The title salt, [Pd(C3H4N2)4]Cl2, was obtained unexpectedly by the reaction of palladium(II) dichloride with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris-(pyrazol-yl)ethane in methanol solution. The Pd(2+) cation is...The title salt, [Pd(C3H4N2)4]Cl2, was obtained unexpectedly by the reaction of palladium(II) dichloride with equimolar amounts of 1-chloro-1-nitro-2,2,2-tris-(pyrazol-yl)ethane in methanol solution. The Pd(2+) cation is located on an inversion centre and has a square-planar coordination sphere defined by four N atoms of four neutral pyrazole ligands. The average Pd-N distance is 2.000 (2) Å. The two chloride anions are not coordinating to Pd(2+). They are connected to the complex cations through N-H⋯Cl hydrogen bonds. In addition, C-H⋯Cl hydrogen bonds are observed, leading to a three-dimensional linkage of cations and anions.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552972
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The title complex, systematic name hexa-kis-(μ2-4-tert-but-oxy-4-oxobut-2-en-2-olato)-1:2κ(9) O (2),O (4):O (2);2:3κ(9) O (2),O (4):O (2)-trizinc, [Zn3(C8H13O3)6], syn-the-sized from tert-butyl aceto-acetate and di-ethyl...The title complex, systematic name hexa-kis-(μ2-4-tert-but-oxy-4-oxobut-2-en-2-olato)-1:2κ(9) O (2),O (4):O (2);2:3κ(9) O (2),O (4):O (2)-trizinc, [Zn3(C8H13O3)6], syn-the-sized from tert-butyl aceto-acetate and di-ethyl-zinc, consists of trinuclear centrosymmetric mol-ecules of an approximate C 3i symmetry. The three metal cations are arranged in a linear fashion, with the central Zn(II) atom located on a centre of symmetry. All three metal cations exhibit a distorted octa-hedral coordination geometry. The terminal Zn(II) cations are chelated by three tert-butyl aceto-acetate ligands and these units are connected to the central Zn(II) atom by the bridging enolate O atoms.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552971
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The title compound, [SnCl4(H2O)2]·6H2O, was crystallized according to the solid-liquid phase diagram at lower temperatures. It is built-up of SnCl4(H2O)2 octa-hedral units (point group symmetry 2) and lattice water mol-e...The title compound, [SnCl4(H2O)2]·6H2O, was crystallized according to the solid-liquid phase diagram at lower temperatures. It is built-up of SnCl4(H2O)2 octa-hedral units (point group symmetry 2) and lattice water mol-ecules. An intricate three-dimensional network of O-H⋯O and O-H⋯Cl hydrogen bonds between the complex molecules and the lattice water molecules is formed in the crystal structure.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552970
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Since the discovery of perchlorate salts on Mars and the known occurrence of ferric salts in the regolith, there is a distinct possibility that the title compound could form on the surface of Mars. [Fe(H2O)6](ClO4)3·3H2O...Since the discovery of perchlorate salts on Mars and the known occurrence of ferric salts in the regolith, there is a distinct possibility that the title compound could form on the surface of Mars. [Fe(H2O)6](ClO4)3·3H2O was crystallized from aqueous solutions at low temperatures according to the solid-liquid phase diagram. It consists of Fe(H2O)6 octa-hedra (point group symmetry -3.) and perchlorate anions (point group symmetry .2) as well as non-coordinating water mol-ecules, as part of a second hydrogen-bonded coordination sphere around the cation. The perchlorate appears to be slightly disordered, with major-minor component occupancies of 0.773 (9):0.227 (9).
Hennings E, Schmidt H, Köhler M
… +1 more, Voigt W
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552969
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The title compound, [Sn(H2O)3](ClO4)2, was synthesized by the redox reaction of copper(II) perchlorate hexa-hydrate and metallic tin in perchloric acid. Both the trigonal-pyramidal [Sn(H2O)3](2+) cations and tetra-hedral...The title compound, [Sn(H2O)3](ClO4)2, was synthesized by the redox reaction of copper(II) perchlorate hexa-hydrate and metallic tin in perchloric acid. Both the trigonal-pyramidal [Sn(H2O)3](2+) cations and tetra-hedral perchlorate anions lie on crystallographic threefold axes. In the crystal, the cations are linked to the anions by O-H⋯O hydrogen bonds, generating (001) sheets.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552968
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The title compound, (C3H12N2)2[AlF6][AlF4(H2O)2]·4H2O, was obtained by a solvothermal method in ethanol as solvent and with aluminium hydroxide, HF and 1,3-di-amino-propane as educts. The asymmetric unit contains a quart...The title compound, (C3H12N2)2[AlF6][AlF4(H2O)2]·4H2O, was obtained by a solvothermal method in ethanol as solvent and with aluminium hydroxide, HF and 1,3-di-amino-propane as educts. The asymmetric unit contains a quarter each of two crystallographically independent propane-1,3-di-ammonium dicat-ions, [AlF6](3-) and [AlF4(H2O)2](-) anions and four water mol-ecules. The cations, anions and three of the independent water mol-ecules are situated on special positions mm, while the fourth water mol-ecule is disordered about a mirror plane. In the crystal, inter-molecular N-H⋯F and O-H⋯F hydrogen bonds link the cations and anions into a three-dimensional framework with the voids filled by water mol-ecules, which generate O-H⋯O hydrogen bonds and further consolidate the packing.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552967
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A single crystal of the title compound, the ternary silicide digadolinium trirhenium penta-silicide, Gd2Re3Si5, was isolated from an alloy of nominal composition Gd20Re30Si50 synthesized by arc melting and investigated b...A single crystal of the title compound, the ternary silicide digadolinium trirhenium penta-silicide, Gd2Re3Si5, was isolated from an alloy of nominal composition Gd20Re30Si50 synthesized by arc melting and investigated by X-ray single-crystal diffraction. Its crystal structure belongs to the U2Mn3Si5 structure type. All atoms in the asymmetric lie on special positions. The Gd site has site symmetry m..; the two Mn atoms have site symmetries m.. and 2.22; the three Si atoms have site symmetries m.., ..2 and 4.. . The coordination polyhedra of the Gd atoms have 21 vertices, while those of the Re atoms are cubo-octa-hedra and 13-vertex polyhedra. The Si atoms are arranged as tricapped trigonal prisms, bicapped square anti-prisms, or 11-vertex polyhedra. The crystal structure of the title compound is also related to the structure types CaBe2Ge2 and W5Si3. It can be represented as a stacking of Gd-centred polyhedra of composition [GdSi9]. The Re atoms form infinite chains with an Re-Re distance of 2.78163 (5) Å and isolated squares with an Re-Re distance of 2.9683 (6) Å.
Umadevi M, Ramalingam BM, Yamuna R
… +2 more, Mohanakrishnan AK, Chakkaravarthi G
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552966
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In the title compound, C25H15Cl2NO4S, the di-chloro-phenyl ring is twisted by 68.69 (11)° from the mean plane of the carbazole ring system [r.m.s. deviation = 0.084 (2)°]. The hy-droxy group is involved in an intra-molec...In the title compound, C25H15Cl2NO4S, the di-chloro-phenyl ring is twisted by 68.69 (11)° from the mean plane of the carbazole ring system [r.m.s. deviation = 0.084 (2)°]. The hy-droxy group is involved in an intra-molecular O-H⋯O hydrogen bond, which generates an S(6) graph-set motif. In the crystal, pairs of C-H⋯Cl hydrogen bonds link mol-ecules into inversion dimers with an R (2) 2(26) motif. Weak C-H⋯O inter-actions further link these dimers into ribbons propagating in [100].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552965
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In the title compound, C4H22B20, the two {1,2-closo-C2B10H11} cages are linked across a centre of inversion with a C-C distance of 1.5339 (11) Å. By careful analysis of the structure, it is established that the non-linki...In the title compound, C4H22B20, the two {1,2-closo-C2B10H11} cages are linked across a centre of inversion with a C-C distance of 1.5339 (11) Å. By careful analysis of the structure, it is established that the non-linking cage C atom is equally disordered over cage vertices 2 and 3.
Ezemobi F, North H, Scott KR
… +2 more, Wutoh AK, Butcher RJ
Acta Crystallogr Sect E Struct Rep Online
· 2014 Dec · PMID 25552964
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The title compounds, C9H7NO3, (1), C10H7NO5, (2), and C14H9NO5, (3), are three potentially anti-convulsant compounds. Compounds (1) and (2) are isoindoline derivatives and (3) is an iso-quinoline derivative. Compounds (2...The title compounds, C9H7NO3, (1), C10H7NO5, (2), and C14H9NO5, (3), are three potentially anti-convulsant compounds. Compounds (1) and (2) are isoindoline derivatives and (3) is an iso-quinoline derivative. Compounds (2) and (3) crystallize with two independent mol-ecules (A and B) in their asymmetric units. In all three cases, the isoindoline and benzoiso-quinoline moieties are planar [r.m.s. deviations are 0.021 Å for (1), 0.04 and 0.018 Å for (2), and 0.033 and 0.041 Å for (3)]. The substituents attached to the N atom are almost perpendicular to the mean planes of the heterocycles, with dihedral angles of 89.7 (3)° for the N-O-Cmeth-yl group in (1), 71.01 (4) and 80.00 (4)° for the N-O-C(=O)O-Cmeth-yl groups in (2), and 75.62 (14) and 74.13 (4)° for the same groups in (3). In the crystal of (1), there are unusual inter-molecular C=O⋯C contacts of 2.794 (1) and 2.873 (1) Å present in mol-ecules A and B, respectively. There are also C-H⋯O hydrogen bonds and π-π inter-actions [inter-centroid distance = 3.407 (3) Å] present, forming slabs lying parallel to (001). In the crystal of (2), the A and B mol-ecules are linked by C-H⋯O hydrogen bonds, forming slabs parallel to (10-1), which are in turn linked via a number of π-π inter-actions [the most significant centroid-centroid distances are 3.4202 (7) and 3.5445 (7) Å], forming a three-dimensional structure. In the crystal of (3), the A and B mol-ecules are linked via C-H⋯O hydrogen bonds, forming a three-dimensional structure, which is consolidated by π-π inter-actions [the most significant inter-centroid distances are 3.575 (3) and 3.578 (3) Å].
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484840
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In the crystal of the title hydrated salt, C6H7N4 (+)·C4H5O6 (-)·0.5H2O, the bi-imidazole monocation, 1H,1'H-[2,2'-biimidazol]-3-ium, is hydrogen bonded, via N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds, to the hydrogen tartrat...In the crystal of the title hydrated salt, C6H7N4 (+)·C4H5O6 (-)·0.5H2O, the bi-imidazole monocation, 1H,1'H-[2,2'-biimidazol]-3-ium, is hydrogen bonded, via N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds, to the hydrogen tartrate anion and the water mol-ecule, which is located on a twofold rotation axis, forming sheets parallel to (001). The sheets are linked via C-H⋯O hydrogen bonds, forming a three-dimensional structure. There are also C=O⋯π inter-actions present [O⋯π distances are 3.00 (9) and 3.21 (7) Å], involving the carbonyl O atoms and the imidazolium ring, which may help to consolidate the structure. In the cation, the dihedral angle between the rings is 11.6 (2)°.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484839
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The title compound, C9H7BrO2, displays a trans configuration with respect to the C=C double bond and is essentially planar [maximum deviation from the least-squares plane through all non-H atoms = 0.056 (4) Å]. The vinyl...The title compound, C9H7BrO2, displays a trans configuration with respect to the C=C double bond and is essentially planar [maximum deviation from the least-squares plane through all non-H atoms = 0.056 (4) Å]. The vinyl-aldehyde group adopts an extended conformation wih a C-C-C-C torsion angle of 179.7 (4)°. In the crystal, mol-ecules are linked by classical O-H⋯O and weak C-H⋯O hydrogen bonds into a three-dimensional supra-molecular network.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484838
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The title compound, C8H12S2 (trivial name DTCDD), was obtained as a side product of the reaction between cis-1,4-di-chloro-but-2-ene and sodium sulfide. The asymmetric unit consists of one-quarter of the mol-ecule (S sit...The title compound, C8H12S2 (trivial name DTCDD), was obtained as a side product of the reaction between cis-1,4-di-chloro-but-2-ene and sodium sulfide. The asymmetric unit consists of one-quarter of the mol-ecule (S site symmetry 2) and the complete mol-ecule has 2/m (C 2h ) point symmetry with the C=C bond in an E conformation. The geometry of the title compound is compared to those of a chloro derivative and a mercury complex.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484837
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The title compound, C15H14N4O, crystallizes with two mol-ecules in the asymmetric unit with similar conformations (r.m.s. overlay fit for the 20 non-H atoms = 0.175 Å). In the first mol-ecule, the dihedral angles between...The title compound, C15H14N4O, crystallizes with two mol-ecules in the asymmetric unit with similar conformations (r.m.s. overlay fit for the 20 non-H atoms = 0.175 Å). In the first mol-ecule, the dihedral angles between the planes of the central pyrazole ring and the pendant phenyl and pyrrole rings are 42.69 (8) and 51.88 (6)°, respectively, with corresponding angles of 54.49 (7) and 49.61 (9)°, respectively, in the second mol-ecule. In the crystal, the two mol-ecules, together with their inversion-symmetry counterparts, are linked into tetra-mers by O-H⋯N hydrogen bonds. The tetra-mers form layers parallel to (211) through pairwise C-H⋯π inter-actions.
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484836
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The title compound, C16H16N4O2, crystallizes with two mol-ecules in the asymmetric unit, one of which shows disorder of the acetate group over two sets of sites in a 0.799 (2):0.201 (2) ratio. The phenyl group has a simi...The title compound, C16H16N4O2, crystallizes with two mol-ecules in the asymmetric unit, one of which shows disorder of the acetate group over two sets of sites in a 0.799 (2):0.201 (2) ratio. The phenyl group has a similar but opposite sense of twist relative to the pyrazole ring in the two mol-ecules, as indicated by the syn N-N-Car-Car (ar = aromatic) torsion angles of 39.7 (2) and -36.9 (2)°. Each mol-ecule features an intra-molecular N-H⋯O hydrogen bond, which closes an S(6) ring. In the crystal, C-H⋯O and C-H⋯N inter-actions direct the packing into a layered structure parallel to (110).
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484835
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In the title compound, C15H15N7, the phenyl ring is inclined by 19.86 (5)° to the mean plane of the pyrazolo-[3,4-b]pyrazine core. In the crystal, N-H⋯N and C-H⋯N hydrogen bonds form [010] chains, which stack via π-π int...In the title compound, C15H15N7, the phenyl ring is inclined by 19.86 (5)° to the mean plane of the pyrazolo-[3,4-b]pyrazine core. In the crystal, N-H⋯N and C-H⋯N hydrogen bonds form [010] chains, which stack via π-π inter-actions [centroid-centroid distance between the pyrazole rings = 3.4322 (7) Å].
Kavitha CN, Jasinski JP, Kaur M
… +2 more, Anderson BJ, Yathirajan HS
Acta Crystallogr Sect E Struct Rep Online
· 2014 Nov · PMID 25484834
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The title salt {systematic name: bis-[1-(3-chloro-phen-yl)piperazinium 2,4,6-tri-nitro-phenolate]-picric acid (2/1)}, 2C10H14ClN2 (+)·2C6H5N3O7 (-)·C6H6N3O7, crystallized with two independent 1-(3-chloro-phen-yl)piperazi...The title salt {systematic name: bis-[1-(3-chloro-phen-yl)piperazinium 2,4,6-tri-nitro-phenolate]-picric acid (2/1)}, 2C10H14ClN2 (+)·2C6H5N3O7 (-)·C6H6N3O7, crystallized with two independent 1-(3-chloro-phen-yl)piperazinium cations, two picrate anions and a picric acid mol-ecule in the asymmetric unit. The six-membered piperazine ring in each cation adopts a slightly distorted chair conformation and contains a protonated N atom. In the picric acid mol-ecule, the mean planes of the nitro groups in the ortho-, meta-, and para-positions are twisted from the benzene ring by 31.5 (3), 7.7 (1), and 3.8 (2)°, respectively. In the anions, the dihedral angles between the benzene ring and the ortho-, meta-, and para-nitro groups are 36.7 (1), 5.0 (6), 4.8 (2)°, and 34.4 (9), 15.3 (8), 4.5 (1)°, respectively. The nitro group in one anion is disordered and was modeled with two sites for one O atom with an occupancy ratio of 0.627 (7):0.373 (7). In the crystal, the picric acid mol-ecule inter-acts with the picrate anion through a trifurcated O-H⋯O four-centre hydrogen bond involving an intra-molecular O-H⋯O hydrogen bond and a weak C-H⋯O inter-action. Weak inter-molecular C-H⋯O inter-actions are responsible for the formation of cation-anion-cation trimers resulting in a chain along [010]. In addition, weak C-H⋯Cl and weak π-π inter-actions [centroid-centroid distances of 3.532 (3), 3.756 (4) and 3.705 (3) Å] are observed and contribute to the stability of the crystal packing.