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.     

Synthesis,Crystal Structure and Characterization of (Z)-2-N′-hydroxyisonicotinamidine

The compound (Z)-2-N′-hydroxyisonicotinamidine, (2) was synthesized and characterized by ¹H NMR, FT-IR, FAB-Mass, UV-Visible Spectra, and elemental Analysis. Its molecular structure was solved by single crystal X-ray diffraction method. The title molecule, C₆H₇N₃O is crystallized in the orthorhombic crystal system with the space group Pna2₁ and with unit cell parameters a = 12.5664(8) Å, b = 8.8622(6) Å, c = 5.7953(4) Å, α = 90°, β = 90°, γ = 90°, and Z = 4. The molecular and crystal structure of the title molecule is stabilized by an intramolecular interaction of the type N—H···O, and the intermolecular interactions of types N—H···N and O—H···N.     

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.     

Synthesis,characterization, and crystal structure analysis of 2-(2-hydroxy-3-methoxyphenyl)-1-(4-chlorophenyl)-4,5-diphenyl-1h-imidazole

The substituted imidazole C₂₈H₂₁ClN₂O₂, was prepared via multicomponent reactions and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy, thermogravimetric analysis, UV-visible, proton nuclear magnetic resonance spectroscopy, and single-crystal X-ray diffraction. The molecule is crystallized in the tetragonal crystal system with the space group P4₃2₁2 and with unit cell parameters a = 12.246(4) Å, b = 12.246(4) Å, c = 31.781(2) Å, and Z = 8. The molecular and crystal structures of the title molecule are stabilized by the intramolecular interactions, O-H···N and C-H···N, and intermolecular interaction, C-H···O.     

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.     

The Crystal and Molecular Structure of 2‐[(3,4‐dimethoxybenzylidene)amino]adamantane

The crystal structure of the title compound, C₁₉H₂₅NO₂ was determined by single crystal X‐ray diffraction technique. The crystal data are Orthorombic, space group Pbca, with a = 9.2119(4), b = 9.5555(4), c = 37.6049(5) Å, Z = 8, T = 293(2) K, MoKα radiation, λ = 0.71073 Å, Mr = 299.40, R = 0.0839 for 1945 reflections with I > 2σ(I). The title compound shows intermolecular C‐H…O type interactions.     

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)     

Solvothermal syntheses and crystal structures of two 4‐heterocyclic acylpyrazolone complexes

Many explorations of transition metal (M)‐L system under solvothermal condition, have led to the syntheses of two new 4‐heterocyclic acylpyrazolone complexes [Co(L)₂(CH₃OH)₂] (HL = 1‐phenyl‐3‐methyl‐4‐(2‐furoyl)‐5‐pyrazolone) ( 1 ) and [Cr(L)₃] ( 2 ). Single‐crystal X‐ray analyses reveal that crystal structures of compound 1 and 2 are respectively orthorhombic, Pbca, a = 15.0378(6) Å, b = 9.8405(4) Å, c = 20.7321(8) Å, V = 3067.9(2) ų, Z = 8 and triclinic, P‐1, a = 10.7966(18) Å, b = 13.023(2) Å, c = 15.520(3) Å, α = 73.011(4)°, β = 84.884(4)°, γ = 70.267(4)°, V = 1964.3(6) ų, Z = 2. Complex 1 has a two‐dimensional (2D) network structure that is formed by O–H···N H‐bonding interactions. Complex 2 makes a one‐dimensional (1D) zigzag chain structure by intermolecular π···π interactions, which is further interlinked via C–H···N H‐bonding interactions to generate a 2D sheet, and then a three‐dimensional (3D) supramolecular network structure is further linked by intermolecular C–H···π interactions. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The molecular and crystal structure of p-methyl-phenyl glyoxylacid-m-trifluoro-anilide

Using X-ray crystal structure analysis of the title compound the positions of all atoms (including all A atoms) were localized in the triclinic unit cell with the parameters a = 14.68₆ Å, b = 7.70₀ Å, c = 7.89₈ Å, α = 122.5°, β = 105.4°, γ = 87.7°, space group P1. The existence of an intramolecular H N … O(1) bridge was inferred, the H-bridge acceptor of which predominantly is the π-electron density of the carbonyl group in agreement with the results of the X-ray crystal structure analysis of p-methyl-phenyl-glyoxyl-acid-p-chloroanilide (HOEHNE , SEIDEL ). Moreover, the existence of H-bridgelike interactions of the two phenyl hydrogen atoms H(6) and H(15) to the carbonyl oxygen O(2) could be proved. These interactions stabilize the conformation of the two phenyl rings in the molecule.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.     

The Molecular and Crystal Structure of p-methyl-phenyl-glyoxyacid-p-chloranilide

Using X-ray crystal structure analysis of the title compound the positions of all the atoms (including all H atoms) in the monoclinic unit cell with the parameters a = 13.90₀ Å, b = 5.13₈ Å, c = 17.95₆ Å and β = 91.05° and the space group P 2₁/n were localized. The existence of an intramolecular N—H(N)…︁ O(1)-bridge was inferred, whose H-bridge acceptor predominantly is the π-electron density of the carbonyl group. At the same time the H(N) atom participates in the intermolecular bridge N H(N)…︁ O′(1) to the symmetry-equivalent neighbouring molecule. H-bridge-like interactions of the two phenyl hydrogen atoms H(6) and H(15) to the carbonyl oxygen O(2) have also been inferred from the torsion angles.     

Crystal Structure of 5,7-Dimethoxy-8-(2-oxo-3-methylbutyl)-2 H-1-benzopyran-2-one (Isosibiricin)

The title compound, C₁₆H₁₈O₅, a simple coumarin crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 7.321(3), b = 21.111(9), c = 11.649(3) Å; β = 123.14(2)°. The structure has been solved by direct methods. The coumarin ring system is planar. The methoxy groups at C5 and C7 are almost coplanar with the coumarin mean plane. The crystal structure is stabilized by C–H… O hydrogen bonds.     

Crystal and molecular structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate

The crystal structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate is studied (T = 173 K, R1 = 0.0354 for 2713 observed reflections). This crystal is orthorhombic, a = 7.8367(8) Å, b = 9.6082(10) Å, c = 23.856(3) Å, V = 1796.3(3) ų, space group P2₁2₁2₁, and Z = 4. The molecule has a folded configuration, which is stabilized by π-π interactions between its two parts. A system of intermolecular C-H...O hydrogen bonds (H...O, 2.44–2.67 Å; CHO angles 122°–169°) and intramolecular C-H...O contacts closing five-membered cycles (H...O, 2.42–2.59 Å; CHO angles 96°–102°) are formed in the structure.     

Synthesis,characterization, single crystal X-ray diffraction and DFT studies of ethyl 5-methyl-1-phenyl-1H-pyrazole-4-carboxylate

The present study describes the synthesis, spectroscopic, and single crystal X-ray structural analysis of ethyl 5-methyl-1-phenyl-1H-pyrazole-4-carboxylate. The pyrazole ester of formula [C₁₃H₁₄N₂O₂] was prepared from the three-component one-pot condensation reaction of ethyl acetoacetate, N,N-dimethyldimethoxymethanamine, and phenyl hydrazine. The product was crystallized by using ethanol as solvent. The structure of the compound was confirmed by elemental analysis, Fourier transforms infrared (IR), thermogravimetric analysis, UV-visible (UV-Vis), ¹H NMR, and single-crystal X-ray diffraction studies. The gas-phase molecular geometry and the electronic structure-property of the molecule were calculated at the density functional theory. The frontier molecular orbitals, theoretical UV-Vis, and IR stretching vibrations were also reported. The compound crystallizes in the monoclinic system with the space group P2₁/c and Z = 4. The unit cell parameters are a = 12.141(3) Å, b = 13.934(4) Å, c = 7.2777(18) Å, and β = 97.816(14)⁰. The structure is stabilized by an intermolecular interaction of type C-H···O and the structure also involves C-H···π interactions.     

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)     

Synthesis and crystal structure of bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl)copper(II)

The title compound, bis[2-[N-(2-chlorophenyl)formimidayl]-1-naphtholato]-(6Cl) copper(II), [Cu(C₁₇H₁₁NOCl)₂] (1) was synthesized and its crystal structure was determined. The Compound 1 is monoclinic, space group P2 ₁/c with a = 9.146(3) Å, b = 18.724(3) Å, c = 16.230(2) Å, β = 96.46(1)°, V = 2761.8(11) ų, Z = 4, D _c = 1.503 g cm^?3, μ(Mo Kα) = 1.020 mm^?1, R = 0.0606 for 2361 reflections [I > 2σ(I)]. In the title compound, the Cu atom is coordinated by an N₂O₂ donor set from the imine-phenol ligand in a slightly distorted square planar coordination geometry, with the two phenolate O atoms being deprotonated. The Cu–O bond lengths are 1.878(4) and 1.889(4) Å, the Cu–N bond lengths are 1.980(5) and 1.985(5) Å. The angles O1–Cu–N1 and O2–Cu–N2 are 90.96(19) and 90.72(19)°, respectively.     

X-ray crystal structural analysis of 1,2-dihydro-3-methylpyrazole-5-one

The title compound 1,2-dihydro-3-methylpyrazole-5-one was determined by X-ray crystal structural analysis. The crystals are monoclinic, with space group P2(1)/n with a = 7.968(7), b = 6.502(6), c = 9.986(10) Å, α = 90°, β = 109.995(15)°, γ = 90°, V = 486.1(8) ų, Z = 4, F(000) = 208, D_c = 1.340 g cm^–3, μ = 0.100 mm^?1, and the final R = 0.0373 and wR = 0.0961. A total of 4776 reflections were collected, of which 1148 were independent (R_int = 0.0589). In the crystal packing diagram, intermolecular N?H···O hydrogen bonds and π?π stacking interactions stabilize the solid state of the title compound.     

Synthesis,Characterization and Crystal Structure of Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate

Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate was synthesized from ethyl 6-(4-bromophenyl)-4-(4-fluorophenyl)-2-oxocyclohex-3-ene-1-carboxylate and ammonium acetate in glacial acetic acid. The synthesized compound was characterized by elemental analysis, FT-IR, thermogravimetric analysis (TGA), differential thermal analysis (DTA), UV-Visible, and single-crystal X-ray diffraction. The title compound, ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate, C₂₁H₂OFNO₂, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 17.417(2), b = 9.7287(9), c = 21.014(2) Å, and Z = 8. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0644 for 1616 observed reflections. An intramolecular N–H…O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N–H…O hydrogen bonds, forming a two-dimensional network.     

Crystal Structure of 2-((<Emphasis Type="Italic">E</Emphasis>)-(5-Bromo-2- hydroxybenzylidene)hydrazono)-1,2-diphenylethanone

The molecular structure of the title compound, C₂₁H₁₅Br₁N₂O₂, was characterized by single crystal X-ray diffraction. The compound crystallizes in the triclinic sp. gr. \(P\bar 1\) with Z = 2. The molecule is not planar: the dihedral angle between the planes of two aromatic rings [C1/C6] and [C16/C21] is 84.9(2)°. The other dihedral angle between two aromatic rings [C9/C14] and [C16/C21] is 88.8(2)°. The title compound exists as a phenol-imine tautomer, in which a strong intramolecular O–H···N hydrogen bond is formed. This study verifies the preference of the phenol-imine tautomeric form in the solid state. A π–π stacking interactions are also observed, which may influence crystal stability: the distance between centroids is 3.702(2) Å.     

Crystal and Molecular Structure of 6‐Methyl‐2‐(trifluoromethyl)‐(6H)‐imidazo[1,2‐c]pyrimidin‐5‐one

The title compound (C8H6F3N3O) crystallizes as colorless plates, triclinic, a = 10.916(2) Å, b = 11.140(1) Å, c = 8.368(1) Å, α = 95.938(9)o, β = 105.24(1)o, γ = 64.843(9)o, V = 888.6(2) ų, Z = 4, D_calc = 1.623g/cm³, space group P . The structure was solved by direct methods and refined by the full‐matrix least‐squares method (R_w = 0.047).