Crystal and molecular structure of 5,6-diphenyl-2-(α-formyl-benzyliden)-2H-thiopyranes

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the monoclinic space group P2₁/n with cell parameters a = 6.101(3) Å, b = 14.365(6) Å, c = 21.888(7) Å, β = 90.20(4)°, Z = 4. The structure was solved by direct methods and refined by least-squares calculations to an R value of 0.074. The molecule exists in solid state in the Z configuration. The very short intramolecular O S distance of 2.654(8) Å can be explained with polar interactions between the O and S atoms.     

Synthesis,characterization, and antibacterial activity of 6-Chloro-8-methyl-2-oxo-2H-chromene-3-carboxylic acid ethyl ester

The title compound was synthesized by reacting 2-hydroxy-4-methoxy-benzaldehyde with diethyl malonate in the presence of piperidine catalyst and ethanol as solvent. The chemical structure of the title compound was elucidated by elemental analysis, ¹H-NMR, and IR. The crystal structure was determined by X-ray diffraction data. It crystallizes in monoclinic crystal system, P2₁/c space group with unit cell parameters, a = 12.840(2) Å, b = 24.790(4) Å, c = 7.8544(13) Å, β = 98.035(5)°, V = 2475.5(7) ų, and Z = 8. The molecular and crystal structure of the title compound is stabilized by inter- and intramolecular interactions of the type C—H···O. The newly synthesized compound was screened for its antibacterial activity against two gram-positive and two gram-negative bacteria.     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Crystal Structure of NdCaGaO4

The crystal structure of the NdCaGaO₄ compound was investigated by means of X-ray structure analysis (powder diffractometer HZG-4, CuK_α): structure type LaCuO₄, space group Cmca, a = 5.3700(2) Å, b = 12.1058(3) Å, c = 5.3937(2) Å, Z = 4, R_I = 0.126. The shortest interatomic distances are: Nd(Ca)—O — 2.240(14) Å; Ga—O — 1.913(2) Å, O—O — 2.6852(2) Å, Nd(Ca)—Nd(Ca) — 3.442(3) Å, Nd(Ca)—Ga — 3.154(4) Å, Ga—Ga — 3.8056(2) Å. Atoms have the following coordination numbers: Nd(Ca) — 8; Ga — 6; O1 — 14(6); O2 — 9(5).     

Crystal Structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)2

The crystal structure of 6,6′-dimethoxy-2,2′-diphenyl-19-crown-5 Hg(SCN)₂ has been determined from three-dimensional X-ray diffraction data. The compound crystallizes in the triclinic space group P1 (no 2) with unit cell parameters α = 9.712(6) Å, β = 11.137(7) Å, c = 14.768(12) Å, α = 86.04(5), β = 80.36(4), γ = 65.70(4), Z = 2, V= 1435(2) ų. The structure was determined by direct methods which on refinement yielded a final value of R(F) index as 0.068.     

Growth and crystal structure of the layered compound TlGaSe2

The semiconducting compound TlGaSe₂ was grown by solid state reaction technique. The crystal structure of this material was confirmed by single‐crystal X‐ray diffraction. TlGaSe₂ crystallizes in the monoclinic system with space group C2/c (No. 15), Z = 16 and unit cell parameters a = 10.779(2) Å, b = 10.776(1) Å, c = 15.663(5) Å, β = 99.993(6)°. The structural refinement converged to R(F) = 0.0719, R(F²) = 0.0652 and S = 1.17. The structure consists of a three‐dimensional arrangement of distorted TlSe₈ and GaSe₄ polyhedrons. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The crystal and molecular structure of 2,6,11-tribromo-14-oxabicyclo[8.3.1]tetradec-6(E)-ene – A transannular O-heterocyclization product of a thirteen membered triene

The crystal structure of the title compound has been determined from single-crystal X-ray diffractometer data collected with a CAD-4 diffractometer. C₁₃H₁₉OBr₃ crystallizes in space group Pbca with a = 24.005(6) Å, b = 12.038(4) Å, c = 10.397(2) Å and Z = 8. Leastsquares refinement gave an R value of R = 0.057 for 1072 observed reflections I > 3σ(I). The investigated product is a bicyclic tetrahydropyran compound with a vinylic bromine atom.     

The crystal structure of zinc azide · 2-methylpyridine at 98 K

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods at 98 K. Zinc azide · 2-methyl pyridine crystallizes in the space group P1 with a = 6.028(2) Å, b = 7.610(3) Å, c = 10.052(4) Å, α = 92.81(3)°, β = 101.08(2)·, γ = 94.64(3)° and Z = 2. Least-squares refinement gave an R value of R_w = 0.039 for 2096 observed reflections. Each zinc atom is surrounded by four nitrogen atoms of different azide groups and one nitrogen atom of the pyridine adduct in a distorted trigonal bipyramidal fashion. The ZnN₅-polyhedra share common edges to form chains along the crystallographic a-axis.     

Crystal structure of a furo-[3,2-g]-[1]-benzopyran-7-one derivative

The crystal structure of 9–(1,1-dimethyl–2-propenyl)-4-hydroxy-7H-Furo-[3,2-g]-benzopyran-7-one has been determined from X-ray diffraction data. The compound crystallizes in the monoclinic space group C2/c with unit cell parameters a = 8.976(3) Å, b = 16.621(2) Å, c = 17.818(2) Å, β = 95.79(2) Å. The gross structure was determined by direct methods and refined to a final value of R = 0.053. The three ring framework of the molecule is nearly planar. The side chain attached at the atomic position C(9) possesses significant foldings and has been found inclined to the ring system of the molecule.     

The Crystal and Molecular Structure of the Complex Diaquatetrakis(imidazole)copper(II) Terephthalate Crystal Structure Containing Cu(II) Him and TA

The title compound has been synthesized and its crystals structure determined at room temperature. MW = 536.01, monoclinic, space group C2/c, Z = 4, a = 22.193(5) Å, b = 8.038(2) Å, c = 15.699(4) Å, β = 119.64(2)°. The crystal structure consists of repeated [Cu(Him)₄(H₂O)₂] (Him = imidazole) cations and non-coordinated terephthalato dianions. The copper(II) ion displays an elongated octahedral coordination being linked to the four nitrogen atoms of the four imidazole ligands and to the two oxygen atoms of the two water molecules. The terephthalato dianions are hydrogen bonded to the four water molecules and four imidazole groups.     

Synthesis Characterization and Crystal Structure of 2-(3,4,5-trimethoxyphenyl)-1-(4-fluorophenyl)-4,5-diphenyl-1H-imidazole

The title compound, C₃₀H₂₅FN₂O₃, was prepared from the four-component one-pot condensation reaction and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-Visible, and single-crystal X-ray diffraction. The compound crystallizes in the triclinic crystal system with the space group Pī, with unit cell parameters a = 10.286(2) Å, b = 11.795(2) Å, c = 21.331(4) Å, α = 100.270(3)°, β = 90.093(3)°, γ = 90.062(3)°, and Z = 4. The crystal and molecular structure of the title molecule is stabilized by intra-molecular interactions of types C–H···N and C–H···O.     

The Crystal and Molecular Structure of 4-Hydroxy-4′-nitro- biphenyl and its Potassium Salt

The crystal and molecular structures of the title compounds have been solved by single crystal X-ray analysis. 4-Hydroxy-4′-nitro-biphenyl (NBO) crystallizes in the centrosymmetric, monoclinic space group P2₁/n with a = 6.036(4) Å, b = 12.392(3) Å, c = 13.346(8) Å, β = 96.46(3)° and 4 molecules in the unit cell. Its potassium salt (NBOK) similarly belongs to P2₁/a with a = 11.277(2) Å, b = 7.3606(6) Å, c = 14.383(3) Å, β = 107.804(7)° and also 4 molecules in the unit cell. The structure of NBO was refined by full matrix least-squares calculation to R = 0.043 for 1105 observed reflections, the structure of NBOK to R = 0.041 for 2288 observed reflections, respectively. NBO and NBOK crystallize in layer-like structures. The biphenyl molecules of NBO are arranged as corrugated ribbons in layers. The ionic and polar moiety of NBOK (potassium, oxygen, and crystal water) are separated by biphenyl units to form layers. The almost planar biphenyl units of NBOK are arranged in pairs and exhibit a short molecular distance of 3.08 Å within one pair.     

Crystal and molecular structure of 2,6‐bis(4‐chlorophenyl)‐3‐phenylpiperidin‐4‐one

The crystal structure of the title compound is described. The chemical formula of the compound is C₂₃H₁₉Cl₂NO. The compound is found to crystallize in monoclinic system with space group P2₁/c, Z = 4. The unit cell dimensions are a = 15.137(3) Å, b = 8.9171(18) Å, c = 14.779(3) Å, β = 91.461(4)° and V = 1994.2(7) ų, D_calc = 1.320 gcm^‐3. The final R factor is 4.4%. The central piperidone ring of the molecule adopts a slightly distorted chair conformation, the mean torsion angle being 52.3°; the phenyl rings are planar. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Tautomeric properties and crystal structure of N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline

The title compound has been synthesised by the reaction of 2-hydroxy-1-naphthaldehyde with 2,5-dichloroaniline. The compound was characterized by elemental analysis, IR and UV-Visible techniques. The UV-Visible spectra of the Schiff base with OH group in ortho position to the imino group was studied in polar and nonpolar solvents in acidic and basic media. The structure of compound has been examined cyrstallographically. It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 6.059(1), b = 12.105(2) c = 20.006(2) Å, V = 1467.4(3) ų, D_x = 1.431 g.cm^-3 and Z = 4. The crystal structure was solved by direct methods and refined by full-matrix least squares. Molecule of the title compound N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline is nearly planar. The molecule contains a strong intramolecular N…H-O hydrogen bond between the imine and hydroxyl group [O1 and N1 = 2.540(4) Å]. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of N-(Diethylaminothiocarbonyl)-N′-phenyl-benzamidine

The crystal structure of the title compound has been determined by X-ray diffractometer data collected on a CAD-4 diffractometer. C₁₈H₂₁N₃S crystallizes monoclinic, space group P 2₁/n with a = 8.939(1) Å, b = 18.992(3) Å, c = 10.416(2) Å, β = 97.29(2) Å and Z = 4. Least-squares refinement gave a value of R = 0.107 for 2647 observed reflections. The molecule has a configuration which can be described best by Z, E′ and exists in the tautomeric enamine form. The molecules form infinite chains connected by intermolecular N—H … S interactions, with H … S distances of 2.46 Å.     

Crystal structure of a dehydroabietate derivative

The crystal structure of methyl-16, nor-5-hydroxy-6,7,15-trioxo dehydroabietate has been determined from three-dimensional X-ray diffraction data. The compound crystallizes in the orthorhombic space group P2₁2₁2 with unit cell parameters a = 19.226(3) Å, b = 11.075(3) Å, c = 8.375(2) Å, Z = 4, V = 1783.3(7) ų, d₀ = 1.36 gcm⁻³. The gross structure was determined by direct methods which on refinement yielded a final value of R index as 0.038. Ring A is a chair, ring B an envelope whereas the ring C adopts a strictly planar conformation. The rings A and B are trans fused. The ester group at C4 is cis fused to methyl carbon C15 whereas another methyl carbon C18 and oxo O(15) of the isopropyl group at C13 are rotated to positions 0.107(3) Å and 0.179(2) Å out of the plane of ring C.     

Crystal Growth from Silica Gels and Single Crystal Structure of Bariumchromate

Rhombic single crystals of bariumchromate were grown in silica gels up to 1.5 mm in size. The influence of the initial pH-value of the gel and the kind and concentration of reactants are studied. The crystal structure has been determined. The compound crystallizes in space group Pnma, with cell dimensions a = 9.113(4) Å, b = 5.528(3) Å, c = 7.336(4) Å and Z = 4. The structure was refined to R = 0.062 on the basis of 364 reflections. Every barium atome, centered in a distorted archimedian antiprism, is coordinated to 8 oxygen atoms each belonging to a chromate tetrahedron. Interatomic distances and bond angles were calculated.     

Die Molekül- und Kristallstruktur des N-Methyl-piperidinium-acet-para-brom-anilid-jodid

N-Methyl-piperidinium-acet-para-bromo-anilide-iodide crystallizes in the triclinic space group P 1 with two formula units C₁₄H₂₀N₂OBrJ and two H₂O molecules in the unit cell. The lattice constants are a = 8.950 Å, b = 14.721 Å, c = 7.440 Å, α = 80.19°, β = 112.57° and γ = 106.82°. The molecular structure of the compound was determined by the X-ray structure analysis and the interaction between the molecules in the crystal was investigated. Especially the influence of the water in the crystal on the form of the molecule was analysed.     

Hirshfeld Surface Analysis and Crystal Structure of [2-Bromo-4-(4-Fluoro-Benzoyl)-Phenoxy]-Acetic Acid Ethyl Ester

The title compound C₁₇H₁₄BrFO₄ was synthesized using 3-Bromo-4-hydroxy-phenyl-(4-fluoro-phenyl)-methanone, ethyl chloroacetate, and anhydrous potassium carbonate. Its structure was established using elemental analysis, NMR, and single crystal X-ray diffraction techniques. The compound crystallizes in orthorhombic crystal system and space group Pbca. The cell parameters are a = 10.1444(13) Å, b = 8.2781(10) Å, c = 38.423(5) Å, Z = 8, V = 3226.6(7) ų. The dihedral angle between two least squares planes of two phenyl rings bridged by keto carbonyl group is ?28.2(5)°. The molecule exhibits intermolecular interactions of the type C?H…F and C?H…O. The intercontacts in the crystal structure are studied using Hirshfeld surface analysis.