Showing papers in "Acta Crystallographica Section E-structure Reports Online in 2011"
TL;DR: Good-quality single crystals of the title compound, indigo B, have been prepared with high selectivity by a sublimation process and more realistic geometrical parameters and modern standards of precision are reported.
Abstract: Good-quality single crystals of the title compound, indigo B [systematic name: 2-(3-oxoindolin-2-ylidene)indolin-3-one], C16H10N2O2, have been prepared with high selectivity by a sublimation process. The previous structure of indigo B [Susse & Wolf (1980). Naturwissenschaften, 67, 453], which showed that the complete molecule is generated by crystallographic inversion symmetry has been confirmed, but the present study reports more realistic geometrical parameters and modern standards of precision (e.g. σ for C—C bonds = 0.002–0.003 A). Each molecule features two intramolecular N—H⋯O hydrogen bonds. In the crystal, molecules are linked by strong face-to-face π–π stacking interactions involving both the six- and five-membered rings [centroid–centroid separations = 3.6290 (14) and 3.6506 (14) A] and intermolecular N—H⋯O hydrogen bonds.
44 citations
TL;DR: The crystal structure of the low-temperature form of synthetic naumannite [disilver(I) selenide], Ag2Se, has been reinvestigated based on single-crystal data and in comparison with previous powder diffraction studies, anisotropic displacement parameters are additionally reported.
Abstract: The crystal structure of the low-temperature form of synthetic naumannite [disilver(I) selenide], Ag2Se, has been reinvestigated based on single-crystal data. In comparison with previous powder diffraction studies, anisotropic displacement parameters are additionally reported. The structure is composed of Se layers and two crystallographically independent Ag atoms. One Ag atom lies close to the Se layer and is surrounded by four Se atoms in a distorted tetrahedral coordination, while the second Ag atom lies between the Se layers and exhibits a [3 + 1] coordination defined by three close Se atoms, forming a trigonal plane, and one remote Se atom.
24 citations
TL;DR: In the title molecule, C16H12F2N2O, the pyrazole ring adopts a slight envelope conformation with the methylene C atom deviating by 0.114 (3) Å from the mean plane of the other four atoms.
Abstract: In the title molecule, C16H12F2N2O, the pyrazole ring adopts a slight envelope conformation with the methylene C atom deviating by 0.114 (3) A from the mean plane of the other four atoms [maximum deviation = 0.021 (3) A]. The dihedral angles between the four essentially planar atoms of the pyrazole ring and the fluoro-substituted benzene rings are 2.6 (2) and 82.2 (2)°. The dihedral angle between the two benzene rings is 83.7 (2)°. The crystal packing is stabilized by weak intermolecular C—H⋯O hydrogen bonds.
20 citations
TL;DR: The title compound, AgMg3(PO4)(HPO4)2, which has been synthesized by the hydrothermal method, has an alluaudite-like structure which is formed by edge-sharing MgO6 octahedra resulting in chains linked together by phosphate groups and hydrogen bonds.
Abstract: The title compound, AgMg3(PO4)(HPO4)2, which has been synthesized by the hydrothermal method, has an alluaudite-like structure which is formed by edge-sharing MgO6 octahedra (one of which has symmetry 2), resulting in chains linked together by phosphate groups and hydrogen bonds. The three-dimensional framework leads to two different channels along the c axis, one of which is occupied by Ag+ ions with a square-planar coordination. The Ag+ ions are disordered over two sites in a 0.89 (3):0.11 (3) ratio. The OH groups, which point into the other type of channel, are involved in strong O—H⋯O hydrogen bonds. The title compound is isotypic with the compounds AM3H2(XO4)(HXO4)2 (A = Na or Ag, M = Mn, Co or Ni, and X = P or As) of the alluaudite structure type.
19 citations
TL;DR: In the title compound, C21H16F2N2, the seven-membered 1,4-diazepine ring of the benzodiazepineRing system adopts a distorted-boat conformation.
Abstract: In the title compound, C21H16F2N2, the seven-membered 1,4-diazepine ring of the benzodiazepine ring system adopts a distorted-boat conformation. The benzene ring of this system makes dihedral angles of 18.6 (2) and 78.8 (2)° with those of two fluorophenyl substituents. In the crystal, inversion dimers linked by two weak C—H⋯F hydrogen bonds generate R22(20) ring motifs. There are also weak N—H⋯π and C—H⋯π interactions.
19 citations
TL;DR: In the crystal structure of the title compound, C7H6BFO2, a broad-spectrum antifungal drug, the planar molecules form centrosymmetric R 2 2(8) dimers via strong O—H⋯O hydrogen bonds, which build up the three-dimensional structure.
Abstract: In the crystal structure of the title compound, C7H6BFO2, a broad-spectrum antifungal drug (AN2690), the planar [maximum deviation 0.035 (1) A] molecules form centrosymmetric R22(8) dimers via strong O—H⋯O hydrogen bonds. The dimers are arranged into layers by weak intermolecular C—H⋯O and C—H⋯F hydrogen bonds. The symmetry of this two-dimensional supramolecular assembly can be described by the layer group p\overline{1} and topologically classified as a simple uninodal four-connected two-dimensional network of a (4.4.4.4.6.6) topology. Further weak C—H⋯O interactions build up the three-dimensional structure.
19 citations
TL;DR: The benzohydrazide derivative C15H14N2O4 as discussed by the authors, which is a benzene derivative, exists in a trans conformation with respect to the C=N double bond and is twisted, the dihedral angle between the two benzene rings being 24.17°.
Abstract: The molecule of the title benzohydrazide derivative, C15H14N2O4, exists in a trans conformation with respect to the C=N double bond and is twisted, the dihedral angle between the two benzene rings being 24.17 (6)°. The methoxy group is almost co-planar with respect to the attached benzene ring [Cm—O—C—C (m = methyl) = −1.45 (17)°]. In the crystal, the molecules are linked by N—H⋯O and O—H⋯O hydrogen bonds into sheets parallel to the bc plane. These sheets are further connected into a three-dimensional network by weak C—H⋯O and C—H⋯π interactions.
18 citations
TL;DR: In the title compound, C30H46O3, an isolation product of Pistacia integerima Stewart, the five-membered ring is nearly in the envelope form and an S(6) ring motif is formed due to intramolecular C—H⋯O hydrogen bonding.
Abstract: In the title compound, C30H46O3, an isolation product of Pistacia integerima Stewart, the five-membered ring is nearly in the envelope form. A 6-carboxyhept-5-en-2-yl group is attached to the five-membered ring. An S(6) ring motif is formed due to intramolecular C—H⋯O hydrogen bonding. In the crystal, intermolecular O—H⋯O hydrogen bonds form carboxylate dimers with R22(8) ring motifs.
17 citations
TL;DR: In the asymmetric unit of the title compound, C18H20N2O5, there are two crystallographic independent molecules, both molecules are twisted; the dihedral angle between the two benzene rings is 7.2 (5)° in one molecule, whereas it is 85.9”(4)°in the other.
Abstract: The title benzohydrazide derivative, C17H18N2O5, exists in a trans conformation with respect to the C=N double bond. The dihedral angle between the benzene rings is 19.41 (5)°. The two methoxy groups at the meta positions of the trimethoxybenzene group are almost coplanar with the ring [C—O—C—C = 1.62 (16) and 178.33 (10)°], whereas the third methoxy group, at the para position, is (+)-synclinal with the ring. In the crystal, molecules are linked by N—H⋯O and bifurcated O—H⋯(N,O) hydrogen bonds, as well as weak C—H⋯O interactions, into sheets lying parallel to the ac plane. A C—H⋯π interaction also occurs.
16 citations
TL;DR: The trinuclear title compound, [Co3(CH3COO)4(C20H22N2O6)2]·2CH2Cl2, contains mixed-valence cobalt ions in the following order CoIII–CoII–CoIII where all the three cobalt ion are hexacoordinated.
Abstract: The trinuclear title compound, [Co3(CH3COO)4(C20H22N2O6)2]·2CH2Cl2, contains mixed-valence cobalt ions in the following order CoIII–CoII–CoIII where all the three cobalt ions are hexacoordinated. The central cobalt ion is situated on an inversion centre and is in an all-oxygen environment, coordinated by four phenolate O atoms and two O atoms from bridging acetate groups, while the terminal cobalt ion is hexacoordinated by two phenolate O atoms, two acetate O atoms and two imine N atoms. This complex contains a high-spin central CoII and two terminal low-spin CoIII i.e. CoIII(S = 0)–CoII(S = 3/2)-CoIII(S = 0). There are weak intermolecular C—H⋯O interactions involving the methoxy groups, as well as intermolecular C—H⋯O interactions involving the acetate anions. In addition, the dichoromethane solvate molecules are held in place by weak C—H⋯Cl interactions.
16 citations
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TL;DR: Single crystals of Cu2ZnSiS4, dicopper(I) zinc silicon tetrasulfide, have been prepared via high-temperature solid-state synthesis and were found to have the wurtz-stannite structure type, like that of Li2CdGeS4.
Abstract: Single crystals of Cu(2)ZnSiS(4), dicopper(I) zinc silicon tetrasulfide, have been prepared via high-temperature solid-state synthesis. Cu(2)ZnSiS(4) was found to have the wurtz-stannite structure type, like that of Li(2)CdGeS(4), Li(2)CdSnS(4), and Cu(2)CdSiS(4). Each sulfur anion is tetra-hedrally coordinated by two Cu cations, one Si cation, and one Zn cation, forming a three-dimensional honeycomb structure. When viewed along the c axis, the atoms are aligned in rows in which each cation alternates with the sulfur anions.
TL;DR: The dihydropyridine ring in the title compound, C25H31NO4, adopts an envelope conformation with the methine C atom representing the flap, and the cyclohexenone rings also adopt envelope conformations with the C atoms bearing the methyl C atoms representing the flaps.
Abstract: The dihydro-pyridine ring in the title compound, C(25)H(31)NO(4), adopts an envelope conformation with the methine C atom representing the flap. The cyclo-hexenone rings also adopt envelope conformations with the C atoms bearing the methyl C atoms representing the flaps. The phenolic hy-droxy group forms an intra-molecular hydrogen bond to one of the two keto O atoms. The hy-droxy group of the N-bonded alkyl chain forms an inter-molecular hydrogen bond to the other keto O atom of an adjacent mol-ecule. The latter hydrogen bond leads to the formation of a helical chain running along the b axis.
TL;DR: In the title compound, C22H17ClN4O2S2, both benzoyl groups are trans to the thiono group across their C—N bonds.
Abstract: In the title compound, C22H17ClN4O2S2, both benzoyl groups are trans to the thiono group across their C—N bonds. The two methylene carbamothioyl formamide fragments of the benzoylthiourea side arms make a dihedral angle of 87.00 (10)°. The molecule is stabilized by intramolecular N—H⋯O, N—H⋯S and C—H⋯·S hydrogen bonds. In the crystal, molecules are linked by N—H⋯O and N—H⋯S intermolecular hydrogen bonds into zigzag chains along the a axis.
TL;DR: In the title compound, C7H6O5, the three hydroxy groups on the ring are oriented in the same direction and there are two intramolecular O—H⋯O hydrogen bonds in the ring.
Abstract: In the title compound, C7H6O5, the three hydroxy groups on the ring are oriented in the same direction. There are two intramolecular O—H⋯O hydrogen bonds in the ring. In the crystal, there are several intermolecular O—H⋯O hydrogen bonds and a short contact of 2.7150 (18) A between the O atoms of the para-OH groups of adjacent molecules.
TL;DR: In the title compound, C29H24N4O2S, intramolecular O—H⋯N hydrogen bonding influences the molecular conformation; the naphthol system and triazole ring form a dihedral angle of 3.88 (7)°.
Abstract: In the title compound, C29H24N4O2S, intramolecular O—H⋯N hydrogen bonding influences the molecular conformation; the naphthol system and triazole ring form a dihedral angle of 3.88 (7)°. In the crystal, π–π interactions between the five- and six-membered rings of neighbouring molecules [centroid–centroid distances = 3.541 (3) and 3.711 (3) Å] consolidate the crystal packing.
TL;DR: In the title compound, C10H12N2OS, the amide NCO group is twisted relative to the thioureido SCN2 group, forming a dihedral angle of 55.3 (2)°, which leads to the formation of centrosymmetric R 2 2(8) dimers.
Abstract: In the title compound, C10H12N2OS, the amide NCO group is twisted relative to the thioureido SCN2 group, forming a dihedral angle of 55.3 (2)°. The crystal packing shows intermolecular N—H⋯S and weak C—H⋯O interactions, the former giving rise to the formation of centrosymmetric R22(8) dimers.
TL;DR: The title compound, C7H6O5·H2O, is a new polymorph of the structures reported by Jiang et al. (2000) and Okabe (2001) and the hydrogen-bonding pattern differs from those reported for the previous polymorphs.
Abstract: The title compound, C7H6O5·H2O, is a new polymorph of the structures reported by Jiang et al. (2000) [Acta Cryst. C56, 594–595] and Okabe et al. (2001) [Acta Cryst. E57, o764–o766]. The gallic acid molecule is essentially planar (r.m.s. deviation = 0.550 A). An intramolecular O—H⋯O hydrogen bond occurs in the gallic acid molecule, which is linked to the water molecule by a further O—H⋯O hydrogen bond. In the crystal, the components are linked by O—H⋯O hydrogen bonds. The hydrogen-bonding pattern differs from those reported for the previous polymorphs.
TL;DR: A monoclinic polymorph of theophylline has been obtained from a chloroform/methanol mixture by evaporation under ambient conditions and features intermolecular N—H⋯O hydrogen bonds, resulting in the formation of dimers between two crystallographically different molecules.
Abstract: A monoclinic polymorph of theophylline, C7H8N4O2, has been obtained from a chloroform/methanol mixture by evaporation under ambient conditions. The new polymorph crystallizes with two molecules in the asymmetric unit. The structure features intermolecular N—H⋯O hydrogen bonds, resulting in the formation of dimers between two crystallographically different molecules; each molecule acts as both donor and acceptor.
TL;DR: In the title compound, C18H13Cl2NO, the naphthalene ring system and the benzene ring form dihedral angles of 74.73”(13) and 62.53 (16)°, respectively, with the acetamide grouping.
Abstract: In the title compound, C18H13Cl2NO, the naphthalene ring system and the benzene ring form dihedral angles of 74.73 (13) and 62.53 (16)°, respectively, with the acetamide grouping [maximum deviation = 0.005 (3) A]. The naphthalene ring system forms a dihedral angle of 75.14 (13)° with the benzene ring. In the crystal, molecules are linked by N—H⋯O hydrogen bonds, forming C(4) chains propagating in [010]. The O atom also accepts two C—H⋯O interactions.
TL;DR: In the title compound, C16H12BrNO3, the butyrolactone core adopts the furan-2(5H)-one structure and forms dihedral angles of 44.80 (17)° with the bromobenzene and phenol rings, respectively.
Abstract: In the title compound, C16H12BrNO3, the butyrolactone core adopts the furan-2(5H)-one structure and forms dihedral angles of 44.80 (17) and 65.73 (18)° with the bromobenzene and phenol rings, respectively. In the crystal, N—H⋯O and O—H⋯O hydrogen bonds link the molecules, generating R43(26) loops The edge-fused rings extend to form a chain running along the b-axis direction and C—H⋯π contacts help to consolidate the packing.
TL;DR: The centrosymmetric mononuclear NiII compound [Ni(C8H5O3]2(C10H14N2O)2(H2O2)2] has a centroid-centroid centroid distance of 3668 2π(2)
Abstract: In the title centrosymmetric mononuclear NiII compound, [Ni(C8H5O3)2(C10H14N2O)2(H2O)2], the central NiII atom is coordinated by two O atoms from two 4-formylbenzoate (FOB) ligands, two O atoms from two water molecules and two N atoms from two diethylnicotinamide (DENA) ligands The coordination geometry is slightly distorted octahedral, with four O atoms in the equatorial plane and two N atoms in axial positions Intramolecular O—H⋯O hydrogen bonds are observed In the crystal structure, molecules are linked into chains along the a axis by intermolecular O—H⋯O hydrogen bonds The structure is further stabilized by π–π interactions between the pyridine rings of DENA units, with a centroid–centroid distance of 3668 (2) A
TL;DR: The molecular structure of the title compound, C17H20N4O5, contains a central fused-ring system, comprised of six- and five- Membered rings, linked by C2 chains to two 2-oxo-1,3-oxazolidine five-membered rings.
Abstract: The molecular structure of the title compound, C17H20N4O5, contains a central fused-ring system, comprised of six- and five-membered rings. This unit is linked by C2 chains to two 2-oxo-1,3-oxazolidine five-membered rings. The central fused-ring system is essentially planar, with a maximum deviation of 0.008 (1) A from the mean plane. Both oxazolidine five-membered rings are also nearly planar, with maximum deviations of 0.090 (1) and 0.141 (1) A.
TL;DR: In this paper, the asymmetric title compound, [Cs2(C7H5N2O4)2(H2O)2]n, was extended to a three-dimensional polymeric structure, which is stabilized by both intra-and inter-molecular amine N-H⋯O and water O-H 2 O hydrogen bonds to carboxylate O-atom acceptors, as well as inter-ring π-π inter-actions.
Abstract: In the structure of title compound, [Cs2(C7H5N2O4)2(H2O)2]n, the asymmetric unit contains two independent Cs atoms comprising different coordination polyhedra. One is nine-coordinate, the other seven-coordinate, both having irregular configurations. The CsO9 coordination polyhedron comprises O-atom donors from three bridging water molecules, one of which is doubly bridging, three from carboxylate groups, and three from nitro groups, of which two are bidentate chelate bridging. The CsO6N coordination polyhedron comprises the two bridging water molecules, one amine N-atom donor, one carboxylate O-atom donor and four O-atom donors from nitro groups (two from the chelate bridges). The extension of the dimeric unit gives a three-dimensional polymeric structure, which is stabilized by both intra- and intermolecular amine N—H⋯O and water O—H⋯O hydrogen bonds to carboxylate O-atom acceptors, as well as inter-ring π–π interactions [minimum ring centroid–centroid separation = 3.4172 (15) A].
TL;DR: The title compound, C56H83N9O11S·2C4H10O·H2O, is a butanol–water solvate of the cyclolinopeptide cyclo(Metsulfone1-Leu2–Ile3–Pro4–Pro5-Phe6–Phe7–Val8-Ile9) (henceforth referred to as CLP-K) which was isolated from flax oil.
Abstract: The title compound, C56H83N9O11S·2C4H10O·H2O, is a butanol–water solvate of the cyclolinopeptide cyclo(Metsulfone1-Leu2–Ile3–Pro4–Pro5–Phe6–Phe7–Val8–Ile9) (henceforth referred to as CLP-K) which was isolated from flax oil. All the amino acid residues are in an l configuration based on the CORN rule. The cyclic nonapeptide exhibits eight trans peptide bonds and one cis peptide bond observed between the two proline residues. The conformation is stabilized by an α- and a β-turn, each containing an N—H⋯O hydrogen bond between the carbonyl group O atom of the first residue and the amide group H atom of the fourth (α-turn) and the third residue (β-turn), repectively. In the crystal, the components of the structure are linked by intermolecular N—H⋯O and O—H⋯O hydrogen bonds into a two-dimensional network parallel to (001). The –C(H2)OH group of one of the butanol solvent molecules is disordered over two sets of sites with refined occupancies of 0.863 (4) and 0.137 (4).
TL;DR: The title compound, Ag2Ni3(HPO4)(PO4)2, has been synthesized by the hydrothermal method and its structure is formed by two types of chains running along the b axis, formed by a linear and continuous succession of NiO6 octahedra linked to PO4 tetrahedra by a common vertex.
Abstract: The title compound, Ag2Ni3(HPO4)(PO4)2, has been synthesized by the hydrothermal method. Its structure is formed by two types of chains running along the b axis. The first chain results from a linear and continuous succession of NiO6 octahedra linked to PO4 tetrahedra by a common vertex. The second chain is built up from two adjacent edge-sharing octahedra (dimers) whose ends are linked to two PO4 tetrahedra by a common edge. Those two types of chains are linked together by the phosphate groups to form polyhedral sheets parallel to the (001) plane. The three-dimensional framework delimits two types of hexagonal tunnels parallel to the a-axis direction, at (x, 1/2, 0) and (x, 0, 1/2), where the Ag atoms are located. Each silver cation is surrounded by eight O atoms. The same Ag+ coordination is found in other phosphates with the alluaudite structure, for example, AgMn3(PO4)(HPO4)2. Moreover, O—H⋯O hydrogen bonds link three PO4 tetrahedra so as to build a three-dimensional network.
TL;DR: In the title compound, C18H13ClFNO, the dihedral angle between the mean planes of the chloro- and fluoro-substituted benzene ring and the naphthalene ring system is 60.5 (8)°.
Abstract: In the title compound, C18H13ClFNO, the dihedral angle between the mean planes of the chloro- and fluoro-substituted benzene ring and the naphthalene ring system is 60.5 (8)°. In the crystal, molecules are linked by N—H⋯O hydrogen bonds, forming a zigzag chain along [101].
TL;DR: A new crystalline form of 2,6-dimethoxybenzoic acid, C9H10O4, crystallizing in a tetragonal unit cell has been identified during screening for co-crystals, and the asymmetric unit comprises a non-planar independent molecule with a synplanar conformation of the carboxy group.
Abstract: A new crystalline form of 2,6-dimethoxybenzoic acid, C9H10O4, crystallizing in a tetragonal unit cell has been identified during screening for co-crystals. The asymmetric unit comprises a non-planar independent molecule with a synplanar conformation of the carboxy group. The sterically bulky o-methoxy substituents force the carboxy group to be twisted away from the plane of the benzene ring by 65.72 (15)°. The carboxy group is disordered over two sites about the C—C bond [as indicated by the almost equal C—O distances of 1.254 (3) and 1.250 (3) A], the occupancies of the disordered carboxym H atoms being 0.53 (5) and 0.47 (5). In the known orthorhombic form reported by Swaminathan et al. [Acta Cryst. (1976), B32, 1897–1900], due to the antiplanar conformation adopted by the OH group, the molecular components are associated in the crystal in chains stabilized by linear O—H⋯O hydrogen bonds. However, in the new tetragonal polymorph, molecules form dimeric units via pairs of O—H⋯O hydrogen bonds between the carboxy groups.
TL;DR: In the title compound, C15H19ClN2OS, the dihedral angle between the amide and thiourea fragments is 58.07 (17)°, and in the crystal, N—H⋯S hydrogen bond links the molecules into chains running parallel to the a-axis direction.
Abstract: In the title compound, C15H19ClN2OS, the dihedral angle between the amide and thiourea fragments is 58.07 (17)°. The cyclohexane group adopts a chair conformation and is twisted relative to the thiourea fragment, forming a dihedral angle of 87.32 (18)°. In the crystal, N—H⋯S hydrogen bond links the molecules into chains running parallel to the a-axis direction.
TL;DR: The 2-bromobenzoyl group in the title compound, C22H19BrN2OS, adopts an E conformation with respect to the thiono S atom across the N—C bond, forming a one-dimensional chain along the b axis.
Abstract: The 2-bromo-benzoyl group in the title compound, C(22)H(19)BrN(2)OS, adopts an E conformation with respect to the thiono S atom across the N-C bond. In the crystal structure, the mol-ecule is stablized by N-H⋯O inter-molecular hydrogen bonds, forming a one-dimensional chain along the b axis.
TL;DR: In the non-centrosymmetric structure of the title compound, (C5H7N2), an extensive three-dimensional network of hydrogen bonds involving all the water molecules, the 4-aminopyridinium cation and some of the oxalate O atoms contributes to the stabilization of the structure.
Abstract: In the non-centrosymmetric structure of the title compound, (C5H7N2)[Cr(C2O4)2(H2O)2]·H2O, the CrIII ion has a slightly distorted octahedral coordination environment defined by two chelating oxalato ligands in equatorial positions and two water molecules in axial positions. An extensive three-dimensional network of hydrogen bonds involving all the water molecules, the 4-aminopyridinium cation and some of the oxalate O atoms contributes to the stabilization of the structure. π–π interactions between adjacent pyridine rings provide additional stability of the crystal packing, with a closest distance between pyridine mean planes of 3.613 (1) A.