Crystal structure of 3,3-diphenylnaphtho [1, 2-c] furan-1 (3H)-one

The crystal structure of 3, 3-diphenylnaphtho[1, 2-c]furan-1(3H)-one 2 was determined by X-ray diffraction analysis. It possesses P2₁2₁2₁ (#19) space group symmetry, with a = 11.922(2), b = 17.142(4), c = 8.429(2) Å, and D _calc = 1.297 mg/m³ for Z = 4.     

An X-ray diffraction study of mesoionic 1-thia-2,3,4-triazolo-5-aminidine and some of its derivatives

X-ray diffraction data are presented for the title mesoionic compound (I), its hydrochloride salt (II) and methylated derivative (III). The crystal of (I) is orthorombic, space group P2₁2₁2₁, with cell dimensions: a = 5.857(1) Å, b = 12.494(2) Å, c = 16.328(3) Å, with four molecules per unit cell. The crystal of (II) is monoclinic, space group P2₁/n, with cell dimensions: a = 5.5720(10) Å, b = 21.5770(4) Å, c = 11.2330(2) Å, beta = 95.15(3)°, with four molecules per unit cell. The crystal of (III) is monoclinic, space group P2₁/n, with cell dimensions: a = 12.0886(5) Å, b = 7.9103(4), c = 104.29(1) Å, beta = 104.29(1)°, with four molecules per unit cell. Of particular interest is the fact that the C5–N6 bond appears to have a high double bond character in all three of the compounds studied. In addition, it is found that the exocyclic N-phenyl group changes from being in the cis conformation with respect to sulfur in compounds (I) and (III) to the trans conformation in the hydrochloric salt (II).     

Isolation and structures of eudesmanolides from Tanacetum cadmeum ssp. cadmeum

Eight sesquiterpene lactones, two coumarins, and two flavonoid derivatives were isolated from Tanacetum cadmeum (Boiss.) Heywood ssp. cadmeum. All compounds have been found previously in other plant species. The crystal structures of artesin and taurin are reported. Crystals of artesin (C₁₅H₂₂O₃) belong to the monoclinic space group P2₁: a = 8.300(1), b = 6.304(1), c = 13.118(2) Å, = 101.836(3)°, V = 671.8(2), Z = 2, R ₁ = 0.0291. Crystals of taurin belong to the monoclinic space group P2₁: a = 5.722(1), b = 8.279(2), c = 14.503(3) Å, = 90.025(1)° , V = 687.0(3), Z = 2, R ₁ = 0.0493. An investigation of the space group indicated a monoclinic system rather than orthorhombic.     

Strychnine-8-ammonio-2-naphthalenesulfonate-water (1/1/3.5): The first structure of a strychnine or brucine compound with a zwitterionic species

The crystal structure of the 1:1 adduct hydrate of strychnine with 1,7-Cleve's acid (8-amino-2-naphthalenesulfonic acid), namely strychnine-8-ammonio-2-naphthalenesulfonate-water (1/1/3.5) has been determined and provides a unique example of a neutral association involving strychnine and an achiral zwitterionic acid species, previously unobserved in the structures of either strychnine or brucine addition compounds. Crystals are orthorhombic, space group P2₁2₁2₁, with Z=4 in a cell with dimensions a=10.4484(8), b=30.850(3), c=9.4998(11) ?. Hydrogen bonding involving all available proton-donor and acceptor sites on all species gives rise to a three-dimensional framework polymer structure. The crystallographic literature for strychnine and brucine and their compounds is also reviewed.     

An investigation of the adducts of sulfur tetrafluoride (SF4) with BF3, AsF5, and SbF5

Three adducts SF₄·BF₃, SF₄·AsF₅, and SF₄·SbF₅ were studied in this work, in gas phase, DFT method was performed to study their molecular structures and thermodynamic properties. The heat of formation was studied at the high level DFT levels.

Crystal structures were predicted using the Dreiding force field and refined by DFT-GGA-RPBE method. All the obtained crystal structures belong to the P2₁/c space group. The lattice energies were predicted to be located between ?91.86 and ?693.73 kJ/mol at the GGA-RPBE level. Based on the optimized crystal structures, the band gap (ΔEg) and density of state (DOS) were predicted and the calculations indicate that they are semiconductors with the band gap between 2.22 and 2.43 ev.     

Synthesis and Novel Crystal Structure Analysis of Anthracene-Based Chalcone Derivatives

Abstract

Four novel anthracene-based chalcone derivatives, (E)-1-(anthracen-9-yl)-3-(4-nitrophenyl)prop-2-en-1-one 1, (E)-1-(anthracen-9-yl)-3-(3-chlorophenyl)prop-2-en-1-one 2, (E)-1-(anthracen-9-yl)-3-(3,4,5-trimethoxyphenyl)prop-2-en-1-one 3, and (E)-1-(anthracen-9-yl)-3-(pyridin-4-yl)prop-2-en-1-one four were synthesized and their structures were solved by single crystal X-ray diffraction methods. The anthracenyl chalcone 1 crystallizes in the centrosymmetric monoclinic P2₁/c space group. The crystal structure analysis shows that the molecules of one form two dimensional (2D) corrugated layer structure. The anthracenyl chalcone 2 crystallizes in the centrosymmetric triclinic P-1 space group and forms one dimensional (1D) tape like structure in the crystal. Compound 3 crystallizes in the centrosymmetric monoclinic P2₁/n space group. Anthracenyl chalcone 4 crystallizes in the centrosymmetric triclinic P-1 space group.     

14-Hydroxy-14-phenyldibenzo[a,j]xanthene as a lattice host: crystal and molecular structure of its (1:1) complex with diethyl ether

The title compound 14-hydroxy-14-phenyldibenzo[a,j]xanthene 1 formed a (1:1) complex with diethyl ether. 1,4-Dioxane was also enclathrated, but with a variable stoichiometric ratio. Single crystal X-ray crystallography was used to elucidate the crystal structure of the 1·diethyl ether complex. Crystals are orthorhombic with space group P2₁2₁2₁, a = 8.532(3), b = 15.040(4), c = 18.491(5) Å, V = 2373(1) ų, d _c = 1.256 g/cm³, and Z = 4. Host and guest molecules were found to associate via hydrogen bonds, with the guest molecules residing in undulating channels lined by host molecules.     

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).     

On the Symmetry of the n=1 Ruddlesden‐Popper Phase Ca2FeO3Cl

Single crystals of Ca₂FeO₃Cl have been obtained as a by product during single crystal growth experiments of calcium ferrates from a CaCl₂ flux. The reddish‐brown optically uni‐axial crystals adopt the tetragonal space group P4/nmm with a = 3.8381(4) Å and c = 13.685(2) Å and Z = 2 formula units per cell. The structure has been determined from a single crystal diffraction data set collected at room conditions and refined to final residual R(|F|) = 0.053 for 163 observed independent reflections with I > 2σ(I). Ca₂FeO₃Cl belongs to the structure family of the Ruddlesden‐Popper series with n = 1, which is also referred to as the K₂NiF₄‐type. Main building units are layers of perovskite type corner connected FeO₅Cl‐octahedra perpendicular to [001]. The two crystallographically independent calcium ions are located between the octahedral layers and are coordinated by nine ligands each: Ca1 (4×O + 5×Cl) and Ca2 (9×O). Following prior studies Ca₂FeO₃Cl crystallizes in space group P4. However, the present investigation shows clearly that this assignment is incorrect and that the compound has been described in an unnecessarily low symmetry.     

X-Ray Studies of Cyanophenyl Pyrimidines Part II The Crystal and Molecular Structure of 5-(4-Ethylcyclohexyl)-2-(4-Cyanophenyl)Pyrimidine

The crystal and molecular structure of 5-(4-ethylcyclohexyl)-2-(4-cyanophenyl)pyrimidine (ECCPP), C₁₉H₁₈N₃, has been determined at room temperature by means of direct methods. The crystals belong to the monoclinic space group P2₁/n, a = 15.959(2), b = 33.469(3), c = 6.210(3) Å β = 90.335(7)° with 8 molecules in the unit cell. Refinement converged to an R value of 0.086. One of the two independent molecules in the unit cell exhibits disorder in the cyclohexane ring. The molecules extend roughly in the [010] direction and form a rather complicated structure in which dipolar interactions play a role.     

Synthesis and crystal structure of [Y(NO3)3(OH2)3]·(Me2-16-crown-5)·H2O

The complex [Y(NO₃)₃(OH₂)₃]·(Me₂-16-crown-5)·H₂O has been prepared and its crystal and molecular structure determined using single crystal X-ray diffraction. The colorless crystals belong to the monoclinic space group P2₁/n with Z = 4. Lattice parameters are a = 10.420(1), b = 17.257(3), c = 14.646(2) Å, = 96.79(1)°, V = 2615.1(6) ų. The yttrium(III) ion is nine-coordinate, bonded to three bidentate nitrate groups and three water molecules. The average Y–O(nitrate) and Y–O(water) distances are 2.42(3) and 2.33(1) Å, respectively. The average HO–H···O hydrogen bonded separation is 2.767Å.     

Growth and Characterization of Urea-(DL) Tartaric Acid Single Crystals

A new organic UV nonlinear optical crystal urea-(DL)tartaric acid [CO(NH₂)₂₋(DL) C₄H₆O₆] (abbreviated as U(DL)T) is reported. Large single crystals have been grown from aqueous solution by the cooling method. They belong to the monoclinic space group P2₁ and the lattice parameters are: a = 7.6973 Å, b = 23.3310 Å, c = 4.8727 Å, and β = 100.82°. The structure and some of its physical properties have been determined. The crystal is transparent from 0.24 to 1.95 μm. The efficiency of powder SHG is larger by one order of magnitude than that of KDP. Thus the crystal will be a useful NLO material.     

Crystal Structure of 2-(2,2-Dibromovinyl)-1-methyl-1<Emphasis Type="Italic">H</Emphasis>-imidazole-4,5-dicarbonitrile

Abstract  

The crystal structure of 2-(2,2-dibromovinyl)-1-methyl-1H-imidazole-4,5-dicarbonitrile (C₈H₄Br₂N₄, Mr = 315.92) has been determined by single crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system with space group P2₁/c and unit cell parameters: a = 15.144(2), b = 16.382(3), c = 8.267(1) ?, β = 95.76(2)^o and Z = 8. The final reliability index is 0.0297 for 2505 observed reflections. The two molecules of 2-(2,2-dibromovinyl)-4,5-dicyano-1-methylimidazole are localized in independent part of unit cell. The crystal packing is stabilized by C–H···N hydrogen bonds and Br···N intermolecular interactions.     

Syntheses,characterization and crystal structures of two structurally similar Schiff bases isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl)methylidene]hydrazide and isonicotinic acid [1-(4-dimethylaminophenyl)methylidene]hydrazide monohydrate

The Schiff base compounds, isonicotinic acid [1-(3-methoxy-2-hydroxyphenyl) methylidene]hydrazide (C₁₄H₁₃N₃O₃, 1) and isonicotinic acid [1-(4-dimethylaminophenyl) methylidene]hydrazide monohydrate (C₁₅H₁₆N₄O·H₂O, 2) have been synthesized by the condensation of equimolar 3-methoxysalicylaldehyde or 4-dimethylaminobenzaldehyde with isonicotinic acid hydrazide in MeOH or EtOH. The compounds were characterized by elemental analysis, IR, ¹HNMR spectra, and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P-1 with unit cell dimensions a = 7.662(1) ?, b = 16.249(2) , c = 10.874(2) ?, β = 110.426(3)°, V = 1268.7(3) ′³, Z = 4, R ₁ = 0.0644, and wR ₂ = 0.1283. Compound 2 crystallizes in the orthorhombic space group P2₁2₁2₁ with unit cell dimensions a = 7.388(1) ?, b = 11.812(1) ?, c = 17.197(2) ?, V = 1500.7(2) ′³, Z = 4, R ₁ = 0.0585, and wR ₂ = 0.1143. X-ray structure determinations revealed that the molecules of both compounds display trans configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N–H···N intermolecular hydrogen bonds, forming layers parallel to the bc plane, while in the crystal structure of 2, molecules are linked through N–H···O, O–H···O, and O–H···N intermolecular hydrogen bonds, forming a network. Supplementary material CCDC-615072 and 620235 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam. ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223–336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Crystal Structure Basis for the Absence of Thermal Mesomorphism in p-Hydroxy-trans-cinnamic Acid

The molecular packing in p-hydroxy-cinnamic acid has been determined by single-crystal x-ray analysis in order to establish the role played by hydrogen bonding in inhibiting mesophase formation. The molecules exist in the crystal as centrosymmetric hydrogen-bonded dimers whose long axes are inclined at ± 84.7° to the crystal b-axis and lie almost in the (104) crystal planes. Rows of dimers lying parallel to b are linked into infinite sheets coincident with the (104) planes by head-to-tail hydrogen bonds involving the phenolic –OH groups. These sheets are interlocked by the alternating ring orientations of neighboring molecules in adjacent sheets.

Crystals belong to the monoclinic system, space group P2₁/c, with a = 8.707(3), b = 5.256(2), c = 17.207(6) Å, β = 99.67(2)°, and Z = 4. The structure was solved by direct methods, and least-squares refinement gave R = 0.057 for 800 independent reflections whose intensities were measured by counter diffractometry.     

The crystal structure of 1-phenyl-3-methyl-4(salicylaldehyde hydrazone)-propenylidene-5-pyrazolone

The crystal structure of 1-phenyl-3-methyl-4-(salicylaldehyde hydrazone)-propenylidene-5-pyrazolone (PMPP-SH) was characterized by the single-crystal X-ray diffraction method. The cell parameters of PMPP-SH in the monoclinic P2₁/c space group are a = 10.851(1) Å, b = 11.679 (1) Å, c = 14.043 (2) Å and β = 91.89 (1)^∘. Analyzing the molecular structure suggest that, in the solid state, the title compound exists mainly in enaminopyrazolone form, which is stabilized by intramolecular hydrogen bonding, rather than NH-form.     

Molecular structure of 3-mesityl-1,4-benzoquinonemonoxime

The X-ray crystal structure of 3-mesityl-1,4-benzoquinonemonoxime is described. The structure reveals that hydrogen-bonds are formed between the oxime and keto groups to form one-dimensional hydrogen bonded ribbons. The structure (C₁₅H₁₅NO₂) is orthorhombic with a = 8.9098(7), b = 10.6399(8), c = 13.7086(10) Å and space group P2₁2₁2₁.     

ThePoranthera corymbosa alkaloids,II. Molecular structure and absolute configuration of porantheridine hydrobromide

Crystals of the hydrobromide of the alkaloid designated porantheridine, C₁₅H₂₇NO, isolated from the plantPoranthera corymbosa Brogn. (family Euphorbiacaea), belong to the space groupP2₁2₁2₁, with cell dimensionsa= 10·059,b = 16·704 andc = 9·629 Å. The crystal structure was solved by the heavy-atom method and refined with 624 reflexions to a residual of 0·078. The molecule consists of three six-membered rings fused on to a common central nitrogen atom; one ring contains an oxygen atom with ann-propyl group and a methyl group substituted on the vicinal carbon atoms. The rings have thechair conformation, two being fusedtrans to each other andcis to the third. The absolute configuration was determined using the anomalous scattering power of the bromine atom.     

Synthesis and crystal structure of 7,9-dideacetyl-1-deoxybaccatinVI

7,9-dideacetyl-1-deoxybaccatinVI was synthesized from 1-deoxybaccatinVI and its crystal structure was determined by X-ray crystallographic techniques. The compound (C₃₃H₄₂O₁₁·2CH₄O) crystallizes into monoclinic space group P2₁ with unit cell parameters: a=8.654(17) ?, b=16.470(5) ?, c=12.671(3) ?, β=97.63(2)°, and Z=2. The X-ray results demonstrated that the reaction of 7,9,10-Trideacetyl-1-deoxy-baccatinVI with Ac₂O in tetrahydrofuran, using CeCl₃ as catalyst, yielded monoacetylated product 7,9-dideacetyl-1-deoxy baccatinVI. In the structure, the six-membered A ring exhibits boat conformation, the eight-membered B ring adopts boat-chair conformation, and the six-membered C ring exhibits sofa conformation.