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)     

Crystal and Molecular Structure of an Oligomeric 1:2 Complex of Copper (II) Azide with 4-Methylpyridine

A 1:2 complex of copper (II) azide with 4-methylpyridine has been synthesized and the crystal structure has been determined by X-ray methods. The compound crystallizes in space group P2₁/a with a = 11,062(3), b = 19.310(6), c = 20.547(5) Å, β = 90.83(2)°, V = 4389(1) ų, Z = 12 and R = 0.048 for 959 observed MoKα data. The structure is built up by oligomeric edge-sharing chains of polyhedra. With the exception of a single coordinated azido group, all other azido ligands serve to bridge neighbouring copper centers [at Cu  N bond distances of 1.94(2) to 2.76(2) Å] in the μ(1,1) fashion.     

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 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.     

Crystal and molecular structure of 3‐phenyl‐4‐(p‐chlorobenzylamino)‐4,5‐dihydro‐1‐H‐1,2,4‐triazol‐5‐on

The structure of the title compound, C₁₅H₁₃N₄OCl was determined by single crystal X‐ray diffraction technique. The structure consists of a p‐chlorobenzylamino moiety and triazol and phenyl rings. The title compound crystallizes in the monoclinic space group P2₁/c with a = 14.368(3), b = 6.255(3), c = 17.631(3) Å, β = 113.24(3)°, Z = 4, V = 1455.8(8) ų and D_x = 1.372 gcm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.0477). The dihedral angle between the triazole moiety and the phenyl ring is 28.8(3)°. The molecular packing is stabilized by N‐H…N and N‐H…O types of inter molecular hydrogen bonds. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione

The crystal structure of 1‐allyl‐5‐(4‐methylbenzoyl)‐4‐(4‐methylphenyl)pyrimidine‐2(1H)‐thione (C₂₂H₂₀N₂OS) has been determined from three dimensional single crystal X‐ray diffraction data. The title compound crystallizes in the monoclinic space group P 2₁/c, with a = 10.6674(13), b = 10.1077(7), c = 17.9467(19) Å, β = 98.460(9)°, V = 1914.0(3) ų, D_calc = 1.251 g cm^–3, Z = 4. In the title compound, the allyl group shows positional disorder. Molecules are linked by C‐H···O, C‐H···N and C‐H···S intermolecular interactions forming two‐dimensional network. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structure of mer-Co(4-CH3C5H4N)3(N3)3

The crystal structure of mer-Co(4-CH₃C₅H₄N)₃(N₃)₃has been determined by single crystal X-ray methods at 300 K. The compound crystallizes in the monoclinic space group C 2/c, a = 19.087(6), b = 16.769(4), c = 15.845(4) Å, β = 119.04(2)°, V = 4434(2) ų, M_r = 464.42. Z = 8, D_x = 1.391 Mgm⁻³, F(000) = 1920, λ (MoKα) = 0.71069 Å, μ = 0.802 mm⁻¹. The cobalt(III) ions are octahedrally coordinated to three azide groups and to three 4-methyl-pyridine molecules to form isolated coordination polyhedra.     

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 structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea

The crystal structure of N‐[(1Z)‐1‐(3‐methyl‐3‐phenylcyclobutyl)‐2‐thiomorpholin‐4‐ylethylidene] thiourea (C₁₈H₂₆N₄S₂) has been determined by X‐ray crystallographic techniques. The compound crystallizes in the orthorhombic space group Pbca, with unit cell parameters: a = 15.692(3), b = 20.803(8), c = 11.979(6)Å, Z = 8, V = 3911(7)ų. The crystal structure was solved by direct methods and refined by full‐matrix least squares to a final R‐value of 0.084 for 1447 observed reflections [I > 2σ ( I ) ]. In the thiosemicarbazide moiety, the S = C bond length is 1.656(6), N‐C‐N angle is 115.6(5)°. The crystal structure is stabilized by the intermolecular N‐H...S hydrogen bonds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 2-(2′-Cyano-2′-amido-ethylenyl)-pyridine

The title compound (C₉H₇N₃O) has been determined from three dimensional X-ray diffraction data. The crystals are monoclinic, a = 4.858(3) Å, b = 15.008(7) Å, c = 11.787(2) Å, ß = 94.107(2)°, V= 857.2(4) ų, z = 4, D_calc = 1.342 g. cm⁻³, space group P2_1/c. The structure was solved by direct methods and refined by full-matrix least-squares method (γ MoK_α′, R = 0.0766).     

X-ray crystal structural analysis of dicyclohexylthiocarbamide

The title compound dicyclohexylthiocarbamide has been determined by single crystal X-ray crystal diffraction analysis. The crystals are monoclinic, space group P2(1)/c with a = 12.5908(9), b = 11.2158(9), c = 10.4255(8) Å, α = 90, β = 110.7360(10), γ = 90°, V = 1376.88(18) ų, Z = 4, F(000) = 528, D_c = 1.160 g/cm³, μ = 0.214 mm^?1, the final R = 0.0381 and wR = 0.1030. A total of 6836 reflections were collected, of which 2423 were independent (R_int = 0.0154). In the crystal packing diagram, intermolecular N?H···S hydrogen bonds stabilize the solid state of the title compound.     

Crystal structure of 4,5-dihydro-6-(2-thienyl)-3(2H) pyridazinone azine, (C16H16N16S2)

M_r = 484, monoclinic, P 2₁/c, a = 5.567(1), b = 7.857(2), c = 19.194(10) Å, β = 99.97(3)°, V = 826.9 ų, Z′ = 2, D_x = 1.43 g · cm⁻³, F(000) = 372, MoKα, λ = 0.71069 Å, μ = 0.328 mm⁻¹, final R = 0.055 for 889 observed reflections, T = 293 K. The compound was prepared from a direct unusual reaction of 6-(2-thienyl)-2,3,4,5-tetrahydropyridazine-3-one with hydrazine hydrate. The structure was solved by direct methods and refined by full-matrix least squares. The molecule in the solid state consists of a dimer with its two equivalent halves related by a center of symmetry at the middle of the N N bond. Each molecular fragment is nearly planar and the N N bond between the two halves is 1.296(5) Å indicating that it is a partial double bond.     

Crystal structure of 3‐(3‐nitrophenylhydrazonocarbonyl)‐(1H)‐1,2,4‐triazole

The title compound, C₁₀H₈N₆O₃, was synthesized by the reaction of 3‐(1H)‐1,2,4‐triazole hydrazine with 3‐nitrobenzaldehyde in ethanol. The single crystal structure has been determined by X‐ray analysis. The crystal belongs to monoclinic system, space group p2₁/c with cell constant, a = 8.0214(17) Å, b = 17.334(4) Å, c = 8.9070(18) Å, V= 1179.4(4) ų. An intramolecular N—H...O and N—H…N hydrogen bond are observed between the ‐NH group with O atom of the carbonyl group and the ‐NH group with N atom. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis,crystal structure,magnetic characterization and spectroscopic properties of a new dinuclear iron(III) complex asymmetrically bridged by a phenoxo and methoxo groups

Dinuclear iron(III) derivative of Fe₂L¹(OCH₃)Cl₂ (L¹=1,3‐bis[N‐(5‐bromo‐2‐hydroxybenzylidene)‐2‐aminoethyl]‐2‐(5‐bromo‐2‐hydroxyphenyl)imidazolidine) has been synthesized, its crystal structure determined and magnetically characterized. The title compound crystallizes in orthorhombic space group Pbcn with cell parameters a = 12.9770(10), 18.7930(10), 25.2950(10) Å, V = 6168.9(6)ų, Z = 8, D_cal = 1.951 Mg/m³. The two iron(III) ions are asymmetrically bridged by a phenoxo and methoxo groups in the compound. The iron(III) centers are separated by 3.166(3) Å. Magnetic susceptibilities of the complex were measured over the range 5 – 298 K and the observed data were successfully simulated by the equation based on the spin‐Hamiltonian operator. Magnetic susceptibility measurements indicate very weak antiferromagnetic coupling between the iron(III) ions with J = – 11.5 cm^‐1. The comparison of the magnetic and structural parameters of the investigated compound is given and the nature of the magnetic super‐exchange interaction of the title compound is compared with similar dinuclear iron(III) complexes. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure determination of 2-acetylamino-4-benzoyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazolin,C13H15N3O2S

Thiosemicarbazone is receiving increasing interest because of the biological activity of some of its derivatives. Mr = 277.35, space group P2₁2₁2₁, Z = 4, a = 9.290(3), b = = 11.512(2), c = 13.286(2) Å, V = 1421 (1) ų, D_m = 1.29(1) Mg m⁻³, D_x = 1.296 Mg m⁻³, λ(MoK_α) = 0.71062 Å, μ = 0.230 mm⁻¹, F(000) = 584, T = 296 K, final R = 0.028 for 1255 reflections. All hydrogen atoms were located. The structure determed by X-ray analysis confirms the chemical results. The structure analysis of the title compound is described and its molecular and crystal structure discussed.     

Crystal Structure of 5,6‐Dinitrobenzimidazole.monohydrate

The title compound (C₇H₆N₄O₅) crystallizes in the monoclinic space group P2₁/c with a=8.566(1) Å, b=14.493(3) Å, c=7.583(1) Å, β=87.75(1)°, V=940.7(3) ų, Z=4, D_x=1.597 g.cm^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R=0.0696). The title compound consists of an imidazole ring with the two NO₂ groups and one water molecule. The short inter‐ molecular N‐H^…N [2.03(5) Å] and O_water‐H^…O [1.98(5) Å] hydrogen bonds are highly effective in holding the molecule in a stable state as a whole.     

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.     

Crystal and molecular structure of 1-diazo-2,3,4,5-tetraphenylcyclopentadiene

M_r = 396.30, monoclinic space group P 2₁/c, a = 10.145(2), b = 18.523(4), c = 12.443(2) Å, β = 110.31(2)°, V = 2193(1) ų, Z = 4, D_x = 1.201 Mg m⁻³, F(000) = 832, λ(MoKα) = 0.71069 Å, μ = 0.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039.     

Crystal and Molecular Structure of Desmodin

The crystal structure of the title compound has been determined from X‐ray diffraction. The compound crystallizes from benzene in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a = 8.485(2), b = 9.816(2), c = 22.597(4) Å, Z = 4, V = 1881.9(7) ų. The structure was determined by direct methods and refined to a final R‐factor of 0.04. Six membered rings B and E are planar. Ring A and ring C are in slightly distorted sofa conformation. Ring D is in envelope conformation. The structure is stabilised by weak intermolecular C‐H...O hydrogen bonds.