Crystal and molecular structure of 5-carbamyl-5H-dibenzo[b,f] azepine

The structure of the title compound has been determined by direct methods from diffractometer data, and refined by full-matrix least squares. Crystals are monoclinicP2₁/n,a=7.534(1),b=11.150(2),c=13.917(3) Å,=92.94(4)°,Z=4,D _x=1.34 (3) g cm^–3,R=0.084 for 1259 observed reflections. The azepine ring has a boat conformation. The fused benzene rings are planar. Molecules are packed as hydrogen-bonded dimers through the carboxamide groups. The atomic charge distribution over the fused ring system is approximately symmetrical.     

Crystal and molecular structure of 1,2-difluoroethane and 1,2-diiodoethane

A single crystal of phase 1 of 1,2-difluoroethane was grown from the melt directly on an X-ray diffractometer close to the melting point of 169 K. It crystallizes in the monoclinic space group C2/c with lattice parameters a = 7.775(4), b = 4.4973(7), c = 9.024(3) Å, = 101.73(1)°, V = 308.9(2) ų, d _calc = 1.420 g cm^–3 for Z = 4. A second phase of 1,2-difluoroethane was obtained under similar conditions which crystallizes in the orthorhombic space group P2₁2₁2₁ with the unit cell parameters a = 8.0467(16), b = 4.5086(9), c = 8.279(2) Å,V = 300.36(11) ų, d _calc = 1.461 g cm^–3 for Z = 4. In both phases the 1,2-difluoroethane molecules adopt the gauche conformation with F–C–C–F torsion angles close to 68°. Crystals of 1,2-diiodoethane C₂H₄I₂ were grown from pentane at –30°C. A platelet single crystal of the size 0.35 × 0.25 × 0.03 mm was measured with Mo K-radiation at 153 K. 1,2-Diiodoethane crystallizes in the monoclinic space group P2₁/n with a unit cell of a = 4.6051(7), b = 12.939(2), c = 4.7318(7) Å, = 104.636(3)°, V = 272.79(7) ų, Z = 2, d _calc = 3.431 g cm^–3, (MoK) = 11.353 mm^–1. In the molecule the two neighboring iodine atoms are positioned anti. The shortest intermolecular contacts occur via iodine–iodine interactions resulting in layers of molecules in the crystal.     

Crystal and molecular structure of dimethylpyrazolo [1,2-a]pyrazolo[1,2-b]benzotriazole-3,4-dicarboxylate,C15H13N3O4

Crystals of dimethyl pyrazolo [1,2-a]pyrazolo[1,2-b]benzotriazole-3,4-di-carboxylate, C₁₅H₁₃N₃O₄, are triclinic:a=9.268(10),b=19.367(50),c=8.821(9) Å,=96.76(18),=115.39(10),=80.17(22)°,Z=4, space group P¯1 with two independent molecules in the asymmetric unit. The crystal and molecular structures have been determined from X-ray diffractometer data by direct methods, and refined by least-squares methods toR=0.047 for 2653 observed reflections. In a least-squares fitting procedure the two independent molecules show an almost perfect resemblance, except for the orientations of the 3-carbomethoxy groups. Their chiral structure is described asS. There is an appreciable puckering of the condensed five-membered rings. Bond distances and angles are found to be not comparable with those in the literature, and are discussed. The carbomethoxy groups of the same molecule show a different slant, owing to overcrowding. Close molecular packing is afforded by layers of molecules approximately parallel to the (001) plane.     

Crystal and molecular structure of [Cu(pyrimidine)4]2BF4

The crystal structure of [Cu(pyrimidine)₄]2BF₄ was determined using single crystal X-ray diffraction. The compound crystallizes in the monoclinic space groupP2₁/n, with lattice parametersa=9.9736(8),b=13.872(1),c=16.568(1) Å. β=98.002(1), andZ=8, yielding a calculated density of 1.857 g/cm³. The Jahn-Teller distorted copper coordination sphere is composed of the four pyrimidine ligands in the equatorial positions (ave. Cu?N=2.02 Å) and the longer axial bonds from the copper to one fluorine (ave Cu?F=2.39 Å) on each of the BF ₄ ^? anions. The crystal structure features layers of molecules having interleaved pyrimidine rings: the layers are connected through intermolecular H … F hydrogen bonds.     

Crystal and molecular structure of triphenyl[2-(p-tolylthio)ethyl]tin

The crystal and molecular structure of Ph₃SnCH₂CH₂SC₆H₄Me-p has been determined by X-ray crystallography. In each of the two independent molecules in the asymmetric unit the tin atom has an irregular tetrahedral geometry, with C–Sn–C valency angles ranging from 104.1(5) to 114.7(5)° in molecule (1) and from 104.6 to 112.7(6)° in molecule (2). The bond lengths, C_alkyl–Sn are 2.18(1) and 2.17(2)Å (in molecules (1) and (2), respectively) while the C_aryl–Sn bond lengths range from 2.11(1) to 2.13(1)Å in molecule (1) and from 2.09(1) to 2.14(1)Å in molecule (2). The Sn–C–C–S torsion angle, 172(1)° is the same for both molecules. NMR spectral data are presented; the¹H NMR spectrum in solution of the central-CH₂–CH₂-unit suggests that each of the protons on each of the CH₂ groups is magnetically distinct and that rotations about the C–C bond are slow on the NMR time scale. Comparisons with similar molecules are made and conformations discussed in terms of steric effects.     

Crystal and molecular structure of 6-exo-methyl-6-endo-nitro-2-exo-phenylbicyclo[2.2.1]heptan-2-endo-ol

The molecular and crystal structure of the title compound2, prepared in racemic form by addition of phenylmagnesium bromide to 6-exo-methyl-6-endo-nitrobicyclo[2.2.1]heptan-2-one (1) in the presence of cerium(III) chloride, were determined by single-crystal X-ray diffraction. The crystal selected for analysis was found to belong to the chiral orthorhombic space group P2₁2₁2₁, witha=6.685(3),b=10.0788(5),c=18.581(1) Å. In the crystal, molecules of2 are associated by intermolecular hydrogen bonds between hydroxy and nitro groups (OH...O₂N=0.82 Å).Nitrobicyclo[2. 2. 1]heptanes. Part 10. Part 9: Michael, Maqutu and Denner (1991).     

Crystal and molecular structure ofp-aminobenzene sulfonacetamide sodium [sulfacetamide sodium] monohydrate

The crystal and molecular structure ofp-aminobenzene sulfonacetamide sodium, C₈H₉N₂NaO₃S·H₂O, an important substituted sulfa drug, has been determined from diffractometric data using MoK radiation. The crystals are monoclinic, witha=6.614(2),b=23.788(6),c=7.012(2) Å,=103.13(2)°, and space groupP2₁/c. The structure was solved by the heavyatom method, and refined by full-matrix least squares to a finalR value of 0.040 with 1435 unique reflections. In packing, the molecules form dimers through pairs of N-HN and N-HO hydrogen bonds. The molecules are further stabilized by O-HO and O-HN hydrogen bonds.     

Crystal and molecular structure of 1-chlorobenz[a]phenazine-7N-oxide

Crystals of 1-chlorobenz[a]phenazine-7N-oxide, C₁₆H₉N₂OCl, are orthorhombic,a =15·04,b = 3·91,c = 20·50 Å,Z = 4, space groupPna2₁. The crystal structure has been determined from two- and three-dimensional X-ray photographic data and refined by Fourier and least-squares methods toR = 0·095 for 715 observed reflexions. The molecule is slightly non-planar. Bond lengths and angles compare well with those of other molecules. Close molecular packing is given by layers of molecules parallel to (001) plane.We are grateful to Professor V. Riganti for assistance with the data collection.     

The structure of 2-phenylperhydro-1,2-oxazolo[3,2-c] [1,4]oxazine

The title compound crystallizes in the monoclinic space group P2₁/n, witha=9.590(6),b=11.574(2),c=9.609(2) Å, =105.72(3)^o andZ=4. The structure was solved by direct methods and refined by full matrix least squares methods toR=0.039 for 1899 observed reflections. The stereochemistry of this 6/5 ring system is found to becis-fused with C(3)–C(4) bond in the axial and N(9)–O(1) bond in equatorial disposition. The six-membered ring in the molecule is in the chair and the five-membered isoxazolidine ring adopts an envelope conformation.     

Crystal and molecular structure of [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II)

The silver(II) complex of the chlorin-like derivativev [5,10,15,20-tetrakisphenyl-2-ethoxy-3-oxa-chlorinato]Ag(II) (1Ag), formally formed by substitution of one pyrrolic subunit in silvermeso-tetraphenylporphyrin by one ethoxy-substituted hydrooxazole moiety, crystallizes in the tetragonal space groupI4/m witha = 13.4811(10) Å,c = 9.7361(13) Å, andZ = 2. The molecule, which is asymmetric, accommodates the high-symmetry space group by rotational disorder with the silver atom located on the four-fold axis.     

Synthesis of 1,2-dimethoxy-1,2-di(pyridin-2-yl)-1,2-ethanediol: Crystal and molecular structure determination

The compound, 2-hydroxy-[1,2-di(pyridin-2-yl)]ethane-1-one, 1, was isolated from the reaction of 2-pyridinecarboxaldehyde and 2-pyridinemethanol at 140°C without catalyst or solvent and characterized by¹H-NMR and IR spectral data. The compound 1 was treated with ethyl acetate to produce the 1,2-di(pyridin-2-yl)ethane-1,2-dione, 2. When 2 was dissolved in an excess of CH₃OH, crystals of 1,2-dimethoxy-1,2-di(pyridin-2-yl)-1,2-ethanediol, 3, were obtained. The molecular and crystal structure of 3 was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system belonging to the P2₁/n space group with a = 6.867(2) ?, b=9.546(4) ?, c=10.522(5) ?, α=90°, β=98.48(4)°, γ=90°. The asymmetric unit comprises two molecules of 3. Although the di-hemiketal was obtained in crystal form, it was found to be unstable, because its IR spectrum changed after a short time, indicating that it had been converted back to the original diketone, 2. The IR showed signals at 1713, and 1690 due to νC =O assigned to di-ketone group.     

Crystal and molecular structure of 1,4-dichloro-7-methylpyrrolo[3,2-d]pyridazine

Crystals of 1,4-dichloro-7-methylpyrrolo[3,2-d]pyridazine,·C₇H₃N₃Cl₂, are monoclinic:a = 18.7465(9),b = 9.3031(3),c = 9.5363(3) Å, = 104.755(3) °,Z = 8,P2₁/n,D _x = 1.667 g cm^–3, (MoK) = 7.4 cm^–1. The structure was solved by Fourier techniques and refined toR = 0.042 for the observed reflections, and 0.060 for all data measured. The two independent molecules in the asymmetric unit have similar geometry. The packing in the crystal is due to van der Waals' forces and two hydrogen interactions of type N-H N.     

Crystal and molecular structure of 3-methoxy-10-methyl-11-phenyl-11-hydroxy-10,11-dihydrodibenzo [b,f] thiepine

Journal of Chemical Crystallography - The structure of the title compound (C22 H20O2S) is orthorhombic with space groupPca21,a=15.467(8),b=9.410(6),c=25.092(7) Å andZ=8. It has been solved by...     

Crystal and molecular structure of 6-t-butyl-1,2-naphthoquinone-1-oxime

The structure of 6-t-butyl-1,2-naphthoquinone-1-oxime was determined by direct methods by the use of MoK diffractometer data and was refined toR = 0.12. The crystals are monoclinic:a = 8.32(1),b = 6.70(1),c = 11.14(1) Å, = 101(1) °,Z = 2,P2₁/m. The molecule is crystallographically flat and lies in a mirror plane. Pronounced diffuse scattering on [010] oscillation photographs is caused by disorder in the orientation of thet-butyl group. The compound occurs in the oxime form, and not as a 1,2-nitroso naphthol.     

Crystal and molecular structure of a new biguanide metal complex, [Cu(AMNH)2]Cl2

The crystal structure of C₆H₁₆N₈O₂·CuCl₂, a biguanide metal complex, has been determined by X-ray diffraction data using MoK radiation. The compound crystallizes in the monoclinic space groupP2₁/a, witha=11.074(4),b=12.061(4),c=5.312(3)Å and=102.8(1)°.The structure was solved by direct methods and refined by full-matrix least-squares to a finalR value 0.037 with 1245 unique reflections. The complex molecule is centrosymmetric, with the Cu atom (0.5,0.5,0.5) on a crystallographic center of symmetry. The complex molecule is rhombic planar with a trans configuration.     

Blue electroluminescent materials based on indeno[1,2-a]arene derivatives for Organic Light-Emitting Diodes

Abstract

In this study, as a continuous effort for searching efficient blue-emitting materials, we designed and synthesized materials based on indeno[1,2-a]arene. OLED devices using these materials were fabricated in the following sequence; ITO (180?nm)/N,N'-diphenyl-N,N'-(2-napthyl)-(1,1'-phenyl)-4,4'-diamine (NPB) (50?nm)/emitting materials (30?nm)/4,7-diphenyl-1,10-phenanthroline (Bphen) (30?nm)/Liq/Al (2/100?nm). Particularly, a device using 7,7-dimethyl-7H-indeno[1,2-a]pyrene as emitter showed maximum values of luminous efficiency, power efficiency, and external quantum efficiency of 1.10?cd/A, 0.49?lm/W, 1.47% at 20?mA/cm², respectively with CIE (x,y) coordinates of (0.15, 0.08) at 6.0V.     

Crystal and molecular structure of 3,3-diphenyl-3-phosphoniabicyclo[3.2.1]octane bromide monohydrate

The title compound crystallizes in the monoclinic space groupP2₁/n, witha=13.316(2),b=18.513(3),c=14.621(4) Å,=90.73(2)°,Z=8, and two independent molecules in the asymmetric unit. The structure was solved by heavy-atom methods and refined to a finalR value of 0.036. The phosphoranium ring adopts a chair conformation, which is substantially flattened at the phosphorus end. The ring conformation and torsion angles are compared with those of similar compounds.