Crystallographic and Computational Analysis of the Supramolecular Structure of 2,5-Dimethylpyrazolo[1,5-a]pyrimidin-7(4H)-one

Abstract  

The structure of 5-dimethylpyrazolo[1,5-a]pyrimidin-7(4H)-one 1 has been determined by X-ray crystallography. The compound 1 crystallizes in the space group P−1 with two molecules in the asymmetric unit solvated with one molecule of the acetic acid The unit cell parameters are a = 8.796(1) ?, b = 10.531(1) ?, c = 10.680(1) ?, α = 96.901(2)o, β = 98.135(2)o, γ = 107.248(2)o. In the crystal molecules A and B are linked into R ₂²(9) hydrogen bonded rings and these rings form chains parallel to [101] Overall, the supramolecular structure 1 consists of two hydrogen bonded and two π–π stacking dimers. An energetic interplay between these dimers has been studied using B3LYP DFT calculations. In addition π–π interactions are analyzed using the Bader’s atoms in molecules’ (AIM) theory.     

N-[[5-[[(1,4-二氢-2-甲基-4-氧-6-喹唑啉基)甲基]甲氨基]-2-噻吩基]羰基]-L-谷氨酸的一水合甲醇溶剂合物的合成、晶体结构及Hirshfeld表面分析

合成制备了N-[[5-[[(1,4-二氢-2-甲基-4-氧-6-喹唑啉基)甲基]甲氨基]-2-噻吩基]羰基]-L-谷氨酸的一水合甲醇溶剂合物(C21H22N4O6S·CH3OH·H2O(化合物1)的晶体,通过单晶X射线衍射,红外,热重分析表征.分析其含有一个结晶水和一分子甲醇溶剂,晶胞参数为a=7.9730(16)nm,b=13.558(3)nm,c=11.412(2)nm,α=90°,β=91.12(3)°,γ=90°.采用Hirshfeld表面分析方法对分子间作用力分析.Hirshfeld表明作用分析得到的二维指纹图显示,其中O…H,N…H,C…H,S…H的作用力要强与C…O,C…N作用力,其中H…H作用力明显.     

Crystal Structure of 7-Phenyl-5,6-Dihydro-14-Aza-[1]benzopyrano[3,4-b]phenanthren-8H-One

Crystallography Reports - The crystal structure of the title compound is determined by single crystal X-ray structure analysis. The crystals are monoclinic, space group P21/c, a = 13.607(3) Å,...     

Synthesis and structure ofexo-11-cyano-endo-11-(trimethylsilyloxy)pentacyclo[5.4.0.02,6.03,10.05,9]undecan-8-one

The crystal structure of an asymmetric pentacyclo[5.4.0.0^2,6.0^3,10.0^5,9]undecan-8,11-dione derivative is reported, in which Me₃SiCN has been added across one of the keto groups. The cage structure demonstrates the expected effects of this addition.     

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 synthesis and structure of 1,2,3,4-tetrahydro-2,4,4-trimethyl-8-nitroimidazo[1,5-d] [1,2,4]triazin-1-one,C8H11N5O3: A heterocycle with a rare ring system

The title compound (IV) was isolated as a by-product during the course of purification of 4-nitroimidazol-5-(N-methyl)hydrazide (II) by silica gel flash chromatography, employing chloroform-acetone (4:1) as the eluting solvent. The crystals are monoclinic, space groupP2₁/c,a=7.425(1),b=13.615(2),c=10.359(2) Å,=97.66(1)°,d _caled=1.44 g cm^–3, (MoK)=1.06 mm^–1,T=298 K. The number of unique reflections=2401, reflections withI3 (I)=1773;R=0.051,R _w =0.061. The bond distances inIV are: N-N, 1.419(3); N-C(=0), 1.359(3); N(H)-C(CH₃), 1.457(3); N(C)-C(CH₃), 1.501(3); N=C, 1.316(3); C=C, 1.368(3), N-C(=N), 1.353(3); N-C(=C), 1.367(2) Å.     

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.     

3-Methyl-3a,4-Dihydro-3H-Thiochromeno[4,3-c]isoxazol

Abstract  The crystal structure of the title compound, C₁₁H₁₁NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)^°, V = 979.5(3) ?³ and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation. The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions. Graphical Abstract  The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation. The methyl group is in an equatorial position.      

The crystal and molecular structure of 6,8,15,16b,16c,17-hexahydro-16b,16c-diphenyl-7H,16H-6a,7a,15a,16a-tetraazanaphtho[5,6]azulano[2,1,8-ij]naptho[f]azulene-7,16-dione

The crystal and molecular structure of a clip containing molecule is described. The structure was solved by vector search methods and refined by least squares methods toR _l=0.0768 [I>2(I)]. Crystal data: C₄₀H₃₀N₄O₂·HCCl₃, triclinic, space group ,a=9.302(2),b=12.981(2),c=15.765(2)Å, =65.91(2)°, =76.40(2)°, =80.15(1)°,V=1682.9(4)ų, Z=2.     

Photochemical reaction products. CI:8b-methoxy-1,3-diphenyl-2a,8b-dihydrocyclobuta[a]naphthalene. CII:8b-methoxy-2,3-diphenyl-2a,8b-dihydrocyclobuta[a]naphthalene

The title compound CI, C₂₅H₂₀O₁, crystallizes in the monoclinic space groupCc with cell parametersa = 1.0186(2),b = 1.6327(6),c = 1.1000(4) nm, = 99.43(2) °,Z = 4, andV = 1.8047 nm³; title compound CII, C₂₅H₂₀O₁, crystallizes in the tetragonal space groupP4₂/n with cell parametersa =b = 2.4218(7),c = 0.6352(2) nm,Z = 8, and V = 3.7255 nm³. Both structures were refined by full-matrix least squares using diffractometer data to reliability indices (R) of 0.048 and 0.053, respectively. In each structure one single carbon-carbon bond, C2a-C8b, was significantly elongated (4.5 pm), otherwise the geometry observed was not unusual.     

Interhalogen 1,2,3-Triazolium Ionic Liquid: Synthesis,Crystal Structure,Hirshfeld Surface Analysis and Photophysical Properties

Journal of Chemical Crystallography - A new interhalogen ionic liquid [C17H25N3Br]+[IBr2]? (IL-1) was synthesized from its triazolium iodide precursor [C17H26N3+I?] in THF under cold...     

X-ray crystallographic determination of the structure and conformation of 1,4,4-trimethyltricyclo[5.4.0.03,5]-undec-7-en-9-one and 1,4,4,8-tetramethyltricyclo[5.4.0.03,5]-undec-T-en-9-one

The crystal structure and conformation of 1,4,4-trimethyltricyclo[5.4.0.0^3,5]undec-7-en-9-one (I) and 1,4,4,8-tetramethyltricyclo[5.4.0.0^3,5]undec-7-en-9-one (II) have been determined by X-ray diffraction. In both cases the crystals are orthorhombic, P2₁2₁2₁,a=6.194 (2) (I); 7.499 (2) (II),b=7.486 (3) (I); 12.855 (3) (II),c=26.283 (7) (I); 13.928 (4) (II) Å,Z=4. The structure was solved by direct methods, and refined to anR value of 0.048 for 1534 (I) and 0.054 for 1357 (II) withI>3.0 (I). In both compounds substituted by carbonyl group ring has the distorted³E sofa conformation whereas the second one possesses the slightly deformed^7.10B boat conformation.The nomenclature of IUPAC for the name of compounds in the title is applied. However, for simplicity the numbering of the atoms in the paper follow Fig. 1a and 1b.     

Crystal Structure of 3,4-Dihydro-2-methoxy-2-methyl-4-phenyl-2H,5H-pyrano[3,2-c]chromen-2-one

Crystallography Reports - A new polymorph of 3,4-dihydro-2-methoxy-2-methyl-4-phenyl-2H,5H-pyrano[3,2-c]chromen-2-one (pyranocoumarin) was studied by X-ray diffraction. The crystallographic...     

3-(benzo[d]thiazol-2-YL)phenol and 4-(benzo[d]thiazol-2-YL)phenol: Crystal Structure Determination,DFT Calculations and Visualizing Intermolecular Interactions Using Hirshfeld Surface Analysis

This article describes the synthesis and X-ray crystal structure analysis of 3-(benzo[d]thiazol-2-yl) phenol (I) and 4-(benzo[d]thiazol-2-yl)phenol (II), crystallized in centrosymmetric triclinic and orthorhombic space groups respectively. The packing in the unit cell of these two positional isomers are different resulting difference in various types of intermolecular interactions (C-H…S, O-H…O_w and O-H…N) connect the molecules into 2D frameworks. Due to presence of lattice water in compound (I), H-bonding interactions are strong and melting point of (I) is comparatively higher than (II). The DFT optimized molecular geometries in (I) and (II) agree closely with those obtained from crystallographic studies.     

Crystal and molecular structure of 2-bromo-5,6-dihydro-6-methyl-4H,8H-pyrido [3,2,1-de]phenanthridin-8-one

Crystals of the title compound, C₁₇H₁₄BrNO, are monoclinic, with space groupP2₁/a,a = 14.314(5),b = 15.009(11),c = 6.596(3) Å, and = 102.39(3) °. Diffraction data were collected with CuK radiation to a Bragg angle of 77 °. The structure was solved by the heavy-atom method and refined to anR index of 0.059 for 2129 reflections. In agreement with NMR results, the C=O group is orientedanti to the benzene ring, and the methyl group at C(6) is axial. Unlike 1-(p-bromobenzoyl)-2-methyl-1,2,3,4-tetrahydroquinoline, the heterocyclic ring assumes a well defined half-chair conformation. Except for C(5) and the methyl group at C(6), the whole molecule is very nearly planar.     

Synthesis and Crystal Structure Studies of Novel Bioactive Heterocycle: 7-Chloro-5-Cyclopropyl-9-Methyl-10-(2-Piperidin-1-yl-Ethyl)-5,10-Dihydro-4,5,6,10-Tetraaza-Dibenzo[a,d] Cyclohepten-11-One

Abstract  The compound, 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one, C₂₂H₂₆N₅ClO, crystallizes in the triclinic space group Pī with cell parameters a = 8.918(7) ?, b = 9.297(7) ?, c = 14.184(8) ?, V = 1095.98(1) ?³ and Z = 2. The final residual factor R ₁ = 0.0451. The structure exhibits intermolecular hydrogen bonds. The 2-piperidin-1-yl-ethyl ring adopts a chair conformation. The starting material used to synthesize the title compound is the intermediate compound of well known anti-HIV drug Nevirapine hence the title compound is having biological importance and hence this crystal structure will helps to structural characterization of the molecule and also for the molecular modeling it will helps for biological study. Graphical Abstract  The title compound 7-chloro-5-cyclopropyl-9-methyl-10-(2-piperidin-1-yl-ethyl)-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one was synthesized by condensation of 7-chloro-5-cyclopropyl-9-methyl-5,10-dihydro-4,5,6,10-tetraaza-dibenzo[a, d] cyclohepten-11-one with 1-(2-chloro-ethyl)-piperidine hydrochloride in presence of anhydrous powdered potassium carbonate as base using N,N-dimethyl formamide as solvent and its crystal structure determined. The title compound derived from bioactive molecule and it is also having biological importance hence this crystal structure will helps for the structural characterization and the biological study of the novel molecule.      

Crystallographic and conformational analysis of 2-methyl-3-(2-nitro-phenyl)-4-phenyl-[1,2,4]oxadiazolidin-5-one

Molecular and crystal structure of 2-methyl-3-(2-nitro-phenyl)-4-phenyl-[1,2,4]oxadiazolidin-5-one, C₁₅H₁₃N₃O₄, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 10.0313(8) Å, b = 9.0372(5) Å, c = 15.5964(14) Å, β = 96.926(7)^∘, Z = 4, D_x = 1.42 g/cm³, μ (Mo-K_α) = 0.105 mm⁻¹, and space group is P 2₁/c. The structure was solved by direct methods and refined to a final R = 0.036 for 1894 reflections with I > 4σ (I). The crystal structure is stabilized by C–H⋅sO type inter-molecular, C–H⋅sN and C–H⋅sO type intra-molecular, π–π stacking and edge to face (C–H⋅s π-ring) interactions. To enlighten conformational flexibility of the title molecule, selected two torsion angles are varied from −180^∘ to +180^∘ in every 10^∘ separetely and then molecular energy profile is calculated and construed.     

Crystal and molecular structure of dihydro-8b,8c-diphenyl-1H,3H,4H,5H,7H,8H,-2,6-dioxa-3a,4a,7a,8a-tetraazacyclopenta[def]fluorene-4,8-dithione

The title compound C₂₀H₁₈N₄O₂S₂ crystallizes in the monoclinic space group P2₁/n witha=8.4930(1) Å,b=11.4880(1) Å,c=20.0709(2) Å, =94.933(1)°,V=1951.01(3) ų,Z=4. The crystal structure has been solved by vector search methods and refined by fullmatrix least-squares toR=0.04 for 2888 reflections and 116 restraints. The title compound has a suitable geometry for synthesizing receptor molecules with a cleft for selective complexation.     

Synthesis,Crystal Structure and Hirshfeld Surface Analysis of Ethyl 4-(4-(2-Bromoethyl)-1H-1,2,3-triazol-1-yl)benzoate

Crystallography Reports - The title compound, C13H14BrN3O2, was synthesized by click chemistry (CuAAC) using 4-bromobut-1-yne and ethyl 4-azidobenzoate. Its molecular structure was determined by 1H...