The Synthesis and Crystal Structure of New Bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol

Abstract  The title compound bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol 8 has been synthesized and established by H NMR, IR and MS spectra and X-ray diffraction crystallography. Compound 8, C₂₃H₂₉Cl₂N₃O, Mr = 424.31, crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 14.5402(6) ?, b = 12.5888(5) ?, c = 11.6510(5) ?, α = 90o, β = 100.183o(2), γ = 90o, V = 2099.05(15) ?³, D_x = 1.343 mg m⁻³ and Z = 4. The final R was 0.0514. The molecular conformation and packing is stabilized by interactions of intermolecular O1–H1···N3′. Index Abstract  The structure of bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol by the reaction of compound 4 and Grignard regent is studied.      

Crystal structure of 3,3-diphenylnaphtho [1, 2-c] furan-1 (3H)-one

The crystal structure of 3, 3-diphenylnaphtho[1, 2-c]furan-1(3H)-one 2 was determined by X-ray diffraction analysis. It possesses P2₁2₁2₁ (#19) space group symmetry, with a = 11.922(2), b = 17.142(4), c = 8.429(2) Å, and D _calc = 1.297 mg/m³ for Z = 4.     

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...     

Crystal and molecular structure of: 5-(1-oxoethyl)-1-methyl-2-(5-bromo-6-methoxy-2-naphthyl)-6-oxabicyclo[3.2.1]octan-7-one and 5-(1-oxoethyl)-1-methyl-2-(5-bromo-6-methoxy-2-naphthyl)-6-oxabicyclo[3.2.1]octane

X-ray crystallographic studies of the two title compounds have shown that the molecules crystallize in the same triclinic space group, , with very similar cell dimensions. For C₂₁H₂₁BrO₄,a=12.056(5),b=13.206(5),c=7.595(3)Å, =90.38(3), =106.07(3) and =124.42(3)° and for C₂₁H₂₃BrO₃,a=12.076(6),b=13.090(5),c=7.490(3)Å, =92.65(5), =104.90(5) and =124.55(5)°. Both compounds possess the oxabicyclo[3.2.1]octane bridged ring system and differ only at the carbon to the ring oxygen where the Csp³ in the ether is replaced by Csp²=O in the lactone. Both cyclohexane rings adopt distorted chair conformations and the lactone and ether rings approximate closely to the envelope conformation. The bromine substituent at C(4) results in distortion of the naphthalene ring. Both molecules pack with the naphthalene rings parallel to each other with interplanar spacings of 3.71 Å in the ether and 3.66Å in the lactone.     

X-ray diffraction studies of 5-functionalized substituted 1,2,3,4-tetrahydropyrimidin-2-ones(thiones): I. Molecular structures of 5-acetyl-4-ethyl-6-methyl-1,2,3,4-tetrahydropyrimidine-2-thione, 5-acetyl-6-methyl-4-(4-methylphenyl)-1,2,3,4-tetrahydropyrimidine-2-thione, and 5-acetyl-4-(4-methoxyphenyl)-6-methyl-1,2,3,4-tetrahydropyrimidin-2-one

The structures of three 5-acetyl-1,2,3,4-tetrahydropyrimidin-2-ones(thiones), namely, 5-acetyl-4-ethyl-6-methyl-1,2,3,4-tetrahydropyrimidine-2-thione, 5-acetyl-6-methyl-4-(4-methylphenyl)-1,2,3,4-tetrahy-dropyrimidine-2-thione, and 5-acetyl-4-(4-methoxyphenyl)-6-methyl-1,2,3,4-tetrahydropyrimidin-2-one, which are potential medicinals, are studied by X-ray diffraction. The conformational features of the molecules studied are analyzed. For these compounds, the dependence of the conformation of the tetrahydropyrimidine ring on the orientation of the substituent at the C(4) atom with respect to the heterocycle is found.     

Crystal structures of 3-[1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl]-1-[4-(methyl (I)/methoxy (II) phenyl)]-2-phenyl-propane-1-one

The compounds 3-(1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl)-1-[4-methyl (I)/methoxy (II)phenyl)]-2-phenyl-propane-1-one crystallize in triclinic space group P . The details are: compound I a = 11.941(6) ?, b = 12.154(7) ?, c = 13.006(7) ?, α = 63.124(8)°, β = 84.464(9)°, γ = 64.810(8)°, V = 1519.7(14) ?³, Z = 2, D _cal = 1.284 Mg m⁻³, and R = 0.0382 (wR = 0.0978); compound II a = 11.897(6) ?, b = 12.268(6) ?, c = 13.001(7) ?, α = 61.919(8)°, β = 83.480(8)°, γ = 64.676(7)°, V = 1504.0(14) ?³, Z = 2, D _cal = 1.333 Mg m⁻³, and R = 0.0422 (wR = 0.1049). The indole ring system in both the molecules I and II are not strictly planar and the dihedral angles formed by the pyrrole and benzo planes are 4.0(7)° and 3.5(8)°, respectively. The C–HO, C–Hπ and ππ types of interactions stabilize the molecules in the unit cell in addition to van der Waal's forces in I and II.     

Crystal and molecular structure of 1-(p-bromobenzoyl)-2-methyl-1,2,3,4-tetrahydroquinoline

Crystals of the title compound, C₁₇H₁₆BrNO, are monoclinic, space groupP2₁/n, unit-cell parametersa = 14.48,b = 6.20,c = 16.72 Å, and = 97.35 °. Three-dimensional data were collected with CuK radiation using an automatic diffractometer. The structure was solved by the heavy-atom method and refined by block diagonal least squares to anR index of 0.088 for 2210 reflections. The main features obtained from our studies are (i) the C=O group is orientedanti to the benzene ring, in agreement with the nmr studies; (ii) the C(2) proton is equatorial while the methyl group at C(2) is in an axial position, also in agreement with nmr data. The bromobenzoyl ring and the benzene ring are at 64 ° to each other, while the carbonyl >C=O and the bromobenzoyl groupsBr are at 42 ° to each other.     

The Synthesis and Crystal Determination of 3-Hydroxy-4-(4-methoxyphenyl)-5-(2-nitrophenyl)furan-2(5H)-one

Abstract  

The title compound, C₁₇H₁₃NO₆, was synthesized and structurally characterized by elemental analysis, MS, ¹H NMR and single crystal X-ray diffraction. It crystallizes in monoclinic system space group C 2/c with a = 27.981(6) ?, b = 12.996(3) ?, c = 8.0900(16) ?, β = 91.06(3)°, V = 2941.4(10) ?³, Z = 8, R ₁ = 0.0675, wR ₂ = 0.1626, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with p-methoxybenzene ring and forms a dihedral angle of 87.2(1)° with the nitrobenzene ring. O–H···O Intermolecular hydrogen bonds link pairs of molecules into centrosymmetric dimers, making a graph set motif of R ₂²(10). The dimers are further assembled into a chain of edge-fused R ₄⁴(34) rings running along the [001] direction. The final three-dimensional supramolecular architecture is stabilized by weak π–π interactions.     

Crystal structure of a nucleoside analog: 9-(R)-[6-(R)-hydroxymethyl-1-oxa-4-thiacyclohexan-2-yl] adenine

The title compound (C₁₀H₁₃N₅O₂S,M _r=267.3) crystallizes in the orthorhombic space groupP2₁2₁2₁ witha=7.579(8),b=7.686(2) andc=20.941(4)Å,V=1220(1)ų,D _x=1.456 gm cm^–3,Z=4,=23.6 cm^–1,F(000)=560 andT=293 K. The structure was solved by direct methods and refined to aR value of 0.068 for 776 unique observed reflections. The oxathiane ring adopts a chair conformation. In the crystal structure the molecules are held together by hydrogen bonds and C-HO close contacts.     

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...     

Crystal structure of (Z)-1-(sec-butyl)-3-(4-dimethylaminophenyl)-2-(1H-1,2,4-triazol-1-yl)propen-2-one

The crystal structure of the title compound is determined by X-ray diffraction studies. The structure is solved by the direct method. The experimental data are obtained on a DAR-UMB diffractometer by the θ-θ/2θ scan technique using MoK _α radiation. The crystal is monoclinic, a = 17.913(3) Å, b = 17.239(3) Å, c = 5.501(5) Å, γ = 74.4(3)°, space group P2₁/a, Z = 4 for C₁₇H₂₂N₄O, and ρ_calcd = 1.211 g/cm³. The molecule consists of the phenyl and triazole rings and the dimethylamino, carbonyl, and isopropyl groups attached to the rings. The dihedral angle between the rings is 67.4°. The carbonyl oxygen atom and the triazole ring are in the trans position relative to each other. The N-C-C-O torsion angle is 172.8°. The molecule is in the Z isomeric form.     

Crystal Structure of 1-(4-(5,6-Dihydropyridazin-1(4H)-yl)Phenyl)-N-Methylmethanesulfonamide

Crystallography Reports - The title compound, 1-(4-(5,6-dihydropyridazin-1(4H)-yl)phenyl)-N-methylmethanesulfonamide (C12H17N3O2S), was isolated as an impurity during the preparation of sumatriptan...     

Crystal structure of a nucleoside analog: 1-(R)-[6-(R)-hydroxymethyl-1,4-dioxan-2-yl] uracil

The title compound (C₉H₁₂N₂O₅,M _r =228.2) crystallizes in the trigonal space groupP3₁,21 witha=b=9.438(3) andc=19.775(3) Å,V=1525.5 ų,D _x =1.490 gm cm^–3,Z=6,=0.12 mm^–1,F(000)=720.0,T=293 K. The structure was solved by direct methods and refined by full-matrix least-squares calculations to anR value of 0.044 on 843 unique observed reflections. The dioxane ring adopts a chair conformation. The crystal structure is stabilized by N-HO hydrogen bonds and C-HO close contacts.     

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....     

Structure of 4,6-dimethylisothiazolo[5,4-b]pyridin-3(2H)-one and its 2-[4-(2-methylphenyl) piperazin-1-ylmethyl] derivative

The crystal and molecular structures of 4,6-dimethylisothiazolo[5,4-b]pyridin-3(2H)-one, C₈H₈N₂OS, 1, and its 2-[4-(2-methylphenyl)piperazin-1-ylmethyl] derivative, C₂₀H₂₄N₄OS, 2c, are described. These compounds crystallize in the monoclinic system in the space group P2 ₁/c. The cell constants for compound 1 are a = 5.049(1), b = 14.897(1), c = 11.330(1) Å, = 98.07(1)°, Z = 4, T = 293 K, and D _cal = 1.419 g cm^–3, and for compound 2c are a = 15.525(1), b = 12.021(1), c = 10.911(1) Å, = 106.42(1)°, Z = 4, T = 293 K, and D _cal = 1.253 g cm^–3 The structures were solved by direct methods and refined to R values of 0.0411 and 0.0380 for 1640 and 3504 reflections for 1 and 2c, respectively. The analysis of the geometry and difference electron density map reveal that the dimethylisothiazolopyridine 1 exists in the amino tautomeric form in the crystalline state. The conformation of the o-methylphenylpiperazine part of the molecule 2c strongly depends on the substituents effect in the phenyl ring and is very similar to those observed in crystals for other investigated arylopiperazine derivatives of the isothiazolopyridine.     

X-Ray Crystal Structure Analysis of Novel 6-Amino-3-Phenyl-4-(Pyridin-4-yl)-2,4-Dihydropyrano[2,3-c]pyrazole-5-Carbonitrile

Crystallography Reports - The communication deals with the eco-friendly synthesis and X-ray crystal structure of an organic carbonitrile, namely...     

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 Structure of 3-(4-Methoxy-benzylidene)-isothiochroman-4-one

Abstract  

The title compound, 3-(4-methoxy-benzylidene)-isothiochroman-4-one (C₁₇H₁₄O₂S) was prepared from the reaction of isothiochroman-4-one with benzaldehyde in the presence of small amount of HCl. The structure of the synthesised compound was determined by IR, ¹H NMR and X-ray crystallography. The structure was solved in monoclinic, space group P2₁/n with a = 3.9773 (7) Å, b = 10.918 (2) Å, c = 30.609 (6) Å, β = 90.615 (3)°, V = 1329.1 (4) Å³, Z = 4 and with R _int = 0.047. The bicyclic ring of isothiochroman-4-one moiety does not adopt a planar geometry. The molecular conformation is stable via C10–H···O1 and C16–H···S1 intramolecular hydrogen-bonding interactions. These contacts involve molecules in an extended two-dimensional sheet to the bc plane.     

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.