Crystal structure of the antidepressant noxiptyline hydrochloride (5-dimethylaminoethyloximino-5H-dibenzo[a,d]-cyclohepta-1,4-diene hydrochloride)

The crystal structure of noxiptyline hydrochloride C₁₉H₂₃N ₂ ⁺ OCl^? (5-dimethylaminoethyloximino-5H-dibenzo[a,d]cyclohepta-1,4-diene hydrochloride), is monoclinic:P2₁/c, a=15.894(5),b=9.116(2),c=13.755(4) Å,β=113.00(7)°,Z=4. It has been determined by application of a multisolution direct method procedure, and refined by full-matrix least squares to a conventionalR of 0.056 for 1674 counterreflections (to 2Θ=44°, MoKα radiation). The noxiptyline molecule adopts a folded boat conformation with dihedral angle between benzo-group planes of 129.3°, and the atypical dimethylaminoethyloximino side chain adopts agauche-gauche distribution about the O-C_β and C_α-C_β bonds. The only intermolecular approach less than van der Waals distances is the hydrogen bond between the amine nitrogen atom and the chloride ion.     

Crystal Structure of 3-[1-(4-Methylphenyl)-9,10-dihydro-4-azaphenanthren-3-yl]benzo[f]coumarin

Crystallography Reports - The crystal structure of the title compound is determined by single crystal X-ray structure analysis. The structure was solved by direct method and refined to a final...     

Molecular Structure and Supramolecular Architecture of Brivanib: (R)-1-(4-(4-Fluoro-2-methyl-1H-indol-5-yloxy)-5-methylpyrrolo[2,1-f] [1,2,4]triazin-6-yloxy)propan-2-ol

Crystallography Reports - Crystal structure of brivanib ((R)-1-(4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-5-methylpyrrolo[2,1-f][1,2,4]triazin-6-yloxy)propan-2-ol) is reported for the first time....     

Inclusion Compounds of the Host 9-(4-Methylphenyl)-9<Emphasis Type="Italic">H</Emphasis>-xanthen-9-ol with a Series of Organic Guests

Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). For those guest molecules possessing electron acceptor atoms/functionalities hydrogen bonding with the host is the prominent mode of interaction and presents itself in the form of (Host)–OH···O(Guest) linkages. The cyclohexane and benzene guests however, occupy voids created by neighbouring host molecules which form hydrogen bonded dimers of the form (Host)–OH···O(Host). The structures of the inclusion compounds were investigated and their thermal stabilities determined. Selectivity experiments were also conducted. Graphical Abstract  The host 9-(4-methylphenyl)-9H-xanthen-9-ol (H) forms inclusion compounds with the guests cyclohexane (H · ?CHEX), benzene (H · ?BENZ), 1,4-dioxane (H · ?DIOX), cyclohexanone (H · CYONE), N,N-dimethylformamide (H · DMF) and N,N-dimethylacetamide (H · DMA). Crystal structures and thermal stabilities were determined. The host selectivity was also investigated.      

4-(E)-2-[3-(3-[(E)-2-(4-cyanophenyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-ylmethyl)perhydrobenzo[d]imidazol-1-yl]-1-diazenylbenzonitrile: X-ray crystal structure

4-(E)-2-[3-(3-[(E)-2-(4-Cyanophenyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-ylmethyl) perhydrobenzo[d]imidazol-1-yl]-1-diazenylbenzonitrile (1) has been synthesized by reac- tion of p-cyanobenzene diazonium chloride with a mixture of formaldehyde and trans-1,2-cyclohexanediamine. The crystal structure has been determined by single crystal X-ray diffraction analysis. The bis-triazene (1) does not adopt a folded conformation, unlike previously studied ethylenediamine analogues, and there is no indication of -stacking in the crystal packing. The dominant interaction between molecules is the van der Waal's attraction between cyclohexane rings. This result establishes the structure of the product of this diazonium coupling reaction as the 1-(1-imidazolidinylmethyl)imidazolidine derivative and not the alternate tetraazabicyclo[4.4.1]undecane derivative. Crystal data: 1 C₂₉H₃₄N₁₀, orthorhombic, space group Pbca, a = 17.946(1), b = 13.106(1), c = 24.108(1) Å, V = 5670.6(3) ų, for Z = 8.     

Synthesis and structure of 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2, 2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, a chiral ligand building block

A triphenyl analog of taddol, 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2,2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, has been synthesized and structurally characterized. This molecule could act as a chiral ligand building block in the creation of tuned taddol analogs. Structural analysis of the title compound reveals that the hydroxyl group is involved in an intramolecular hydrogen bond and does not take part in any intermolecular interaction. Crystal packing is influenced by C–H O hydrogen bonding and phenyl phenyl interactions. Crystal data: Triclinic, P1 (No. 1), a = 5.9343(4) Å, b = 8.2367(17) Å, c = 10.987(2) Å, = 88.290(6), = 75.442(4), = 80.655(6), V = 512.86(15) ų, Z = 1, D _calc = 1.258 mg/m³. Final residual values were R ₁ = 0.0407 for 3022 observed data (I > 2s(I) ) and wR ₂ = 0.0941 for all 3524 unique data.     

Crystal Structures of N-[2-(4-oxo-4H-benzo[d] [1, 3]-oxazin-2-yl)benzamide and Propionamide and Their N-Containing Analog N-[2-(4-oxo-3,4-dihydroquinazolin-2-yl)phenyl]propionamide

Crystallography Reports - Specific features of the molecular and crystal structures of two substituted benzoxazinones (I and II) and their structural analog quinazolinone (III) have been analyzed...     

Synthesis and Crystal Structure of [2-(4-chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone

[2-(4-Chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone was synthesized and characterized by spectroscopic and X-ray diffraction methods. The molecule crystallizes in the monoclinic space group P2₁/c with cell parameters a = 13.7530(19) Å, b = 10.0560(19) Å, c = 13.469(3) Å, β = 100.630(7)° and Z = 4. There is a large discrepancy between the carbonyl group bond lengths of ketone and the ester. The structure exhibits intermolecular hydrogen bonds of the type C–H···O.     

Calorimetric investigations of 2-[4-n-alkylphenyl]-5-[4-n-alkyloxyphenyl]-pyrimidines

We investigated temperatures and enthalpies of the phase transitions by means of the calorimeter DSC-2. The kinetics of polymorphic transitions in the solid state, the pretransitional behaviour in the liquid crystalline phases and the transition enthalpies, ranging from 3 J/mol up to 50 kJ/mol, in relation to the occurrence of the liquid crystalline phase types S_G, S_F, S_C, S_A, and N are points of discussion.     

1-[2-(p-Tolyl)-1-diazenyl]-3-({3-[2-(p-tolyl)-1-diazenyl] perhydrobenzo[d]imidazol-1-yl}methyl)perhydrobenzo[d]imidazole: synthesis,characterization and X-ray crystal structure

1-[2-(p-Tolyl)-1-diazenyl]-3-({3-[2-(p-tolyl)-1-diazenyl]perhydrobenzo[d]imidazol-1-yl}methyl)perhydrobenzo[d]imidazole(1) has been synthesized by reactionof a mixture of 1,2-diaminocyclohexane and formaldehyde withp-toluene diazonium chloride inaqueous solution. The product has been characterized by IR and NMRspectroscopy and elemental analysis. A crystal grown from solution ina mixed solvent system of ethyl acetate and hexanes was analyzed byX-ray crystallography. The solution of the crystal structure of(1) is important in establishing theconnectivity of this molecule and other compounds of similarstructure. The crystal structure of (1) is compared with the previously reportedstructure of the p-cyano analogue(2). Compounds (1) and (2)differ principally in the relative orientation of the heterocyclicrings; in (1), the molecule has adistinct V-shape, whereas compound (2) adopts a more extended conformation.Significant conjugation within the triazene moieties is evident inboth (1) and (2), as manifested in the N465=N andN–N bond lengths. The conjugation is greater in (2) due to the extended conjugation through tothe nitrile group. The title compound (1){C₂₉H₄₀N₈}crystallizes in the monoclinic, space group C2/c, with lattice constants: a = 30.532(6) ?,b =5.9050(12) ?, c= 15.463(3) ?, α = 90°,β = 99.94(3)°, γ = 90°,V =2746.0(10) ?³, Z = 4, D _c =1.209 mg m⁻³,F(000) = 1076, R ₁ = 0.0785,wR ₂= 0.1877.     

4-(2-Methylphenyl)-1,2,3,4,5,6,7,8-octahydroquinazoline-2,5-dione (I) and 4-(4chlorophenyl)-1,2,3,4,5,6,7,8-octahydroquinazoline-2,5-dione (II)

The crystal and molecular structures of the title compounds have been determined by x-ray structure analysis. The compounds (I) and (II) crystallize in space groups P2₁2₁2₁ and 12/a respectively. The structures were solved by direct methods and refined to R = 0.058 and R = 0.046. The saturated pyrimidine-2-one ring in both structures deviates from the planarity. There are two intermolecular hydrogen bonds in (I) and (II). The configuration at C4 in (I) is S.     

The synthesis and crystal structure of 2-[4(S)-4,5-dihydro-4-phenyl-2-oxazolinyl]-benzenamine, and 2-[4(S)-4,5-dihydro-4-benzyl-2-oxazolinyl]-benzenamine

Two oxazolines compound 1a and 1b, 2-[4(S)-4,5-dihydro-4-phenyl-2-ozazolinyl-benzenamine, and (C₁₅H₁₄N₂O), 2-[4(S)-4,5-dihydro-4-benzyl-2-ozazolinyl-benzenamine (C₁₆H₁₆N₂O) were obtained in moderate yield from the reactions of 2-aminobenzonitrile with optically active L-(+)-Phenylglycinol and L-(+)-Phenylalaninol, respectively, in chlorobenzene under dry, anaerobic conditions. ZnCl₂ was dried under vacuum and acted as a Lewis acid catalyst in this reaction. The structures of 1a and 1b were determined by X-ray diffraction and NMR. There exist intra- and intermolecular N-H…N hydrogen bonds in the crystal structure.     

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 5-carbamyl-5H-dibenzo[b,f] azepine

The structure of the title compound has been determined by direct methods from diffractometer data, and refined by full-matrix least squares. Crystals are monoclinicP2₁/n,a=7.534(1),b=11.150(2),c=13.917(3) Å,=92.94(4)°,Z=4,D _x=1.34 (3) g cm^–3,R=0.084 for 1259 observed reflections. The azepine ring has a boat conformation. The fused benzene rings are planar. Molecules are packed as hydrogen-bonded dimers through the carboxamide groups. The atomic charge distribution over the fused ring system is approximately symmetrical.     

On the stereochemistry of 7-[1(2-carbomethoxyanilino)-1-(pyridyl)-methyl]-quinolin-8-ol (CMAP-oxine)

C₂₃H₁₉N₃O₃, P1 , a = 11,683(3), b = 7.740(2), c = 14.445(3) Å, α = 131.02(8), β = 95.43(8), γ = 95.02(8)°, D_x = 1.328 Mg · m⁻³, V = 0.9614 · 10⁻²⁷ m³, Final R = 0.059 for 2905 symmetrically independent reflections (|F₀| ≧ 3σ(F₀)). The intensities were measured with an automatic diffractometer. There are two molecules in the unit cell. The substance is not tridentat in potentially coordination behaviour; coordination takes place (twodentat) on the oxine group.     

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.     

Synthesis,Crystal Structure and Biological Activity of 7-(4-Methylpiperazin-1-Yl)-5-[4-(Trifluoromethyl)Phenyl]pyrazolo[1,5-a]Pyrimidine-3-Carbonitrile

Crystallography Reports - The title compound C19H17F3N6 was synthesized and structurally characterized by infrared and mass spectroscopy, 1H NMR, elemental analyses and single crystal X-ray...