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.     

Mathematical simulation and X-ray diffraction investigation of the crystal structure of (R)-[(R)-o-(1-N,N-dimethylaminoethyl)phenyl]-2,5-dimethoxyphenyl(phenyl)methanol

The crystal structure of (R)-[(R)-o-(1-N,N-dimethylaminoethyl)phenyl]-2,5-dimethoxyphenyl(phenyl)methanol is mathematically simulated by the discrete modeling of molecular packings. A complete set of possible model variants is analyzed using the proposed algorithm with the aim of choosing the appropriate models that can serve as starting models for solving and refining the crystal structure from X-ray diffraction data. The crystals of the compound under investigation are monoclinic, a = 9.268(2) Å, b = 8.802(2) Å, c = 13.176(3) Å, β = 94.01(3)°, space group P2₁, and Z = 2. The structure is solved for a starting model calculated using the discrete modeling method and refined by the full-matrix least-squares procedure to R(F) = 0.037 and ωR(F ²) = 0.097.     

X-ray crystallography of methyl (6-amino-5-cyano-2-methyl-4-(2-nitrophenyl)-4<Emphasis Type="Italic">H</Emphasis>-pyran)-3-carboxylate

The organic carbonitrile namely methyl (6-amino-5-cyano-2-methyl-4-(2-nitrophenyl)-4H-pyran)- 3-carboxylate is synthesized via one-pot multi-component reaction at room temperature using commercially available urea as inexpensive and environmentally benign organo-catalyst and its crystal structure is determined by X-ray technique. The crystals are monoclinic, sp. gr. C2/c, a = 12.3069(8) Å, b = 9.7023(7) Å, c = 24.812(2) Å, β = 94.862(6)°, Z = 8. The dihedral angle between pyran and phenyl rings is 87.8(1)°; the pyran ring is almost planar The dihedral angle between the mean planes of phenyl ring and nitro group is 44.4(2)°. The crystal structure is stabilized by N?H···N and N?H···O hydrogen bonds. In addition, C?H···π interactions are also observed in the crystal structure.     

Solid-phase synthesis and crystal structure of 5(3-nitrophenyl)-3,7-diphenyl-4H,6H-1,2-diazepine

The title compound, 5-(3-nitrophenyl)-3,7-diphenyl-4H,6H-1,2-diazepine (C₂₃H₁₉N₃O₂), was synthesized, in 76% yield, by one-pot multicomponent solid-phase reaction of 3-nitrobenzylidene phenyl ketone, acetophenone and hydrazine, using the catalyst bismuth nitrate, co-catalyst ZnCl₂, adsorbed on neutral alumina, at 110°C. The compound was characterized by spectral methods and X-ray diffraction studies. The crystals are monoclinic, space group P2₁/c: a = 12.186(2), b = 14.769(3), c = 11.046(2) Å, β = 115.023(3)°, Z = 4; R = 0.0418 for 2576 observed reflections. The diazepine ring assumes a twist chair conformation. The dihedral angles between the mean planes through the diazepine ring and the nitrophenyl rings and two phenyl are: 89.19(5)°, 45.85(5)° and 20.80(6)°, respectively. The crystal structure is stabilized by C-H…N, C-H…O, C-H…π hydrogen bonds and π-π-stacking interactions.     

Crystal structure of zinc iodide complex with carbamide, ZnI2 · 2CO(NH2)2

The structure of ZnI₂ · 2CO(NH₂)₂ is determined by single-crystal X-ray diffraction. The crystals are monoclinic, a = 12.694(3) Å, b = 6.886(2) Å, c = 13.161(3) Å, β = 110.58(2)°, Z = 4, space group P2₁/a, and R = 0.0337 for 2481 reflections. Similar to the chloride analogue, the structure consists of discrete molecules with tetrahedrally coordinated Zn atoms. The bond lengths and angles are as follows: Zn-I, 2.5749(8) and 2.5473(8) Å; Zn-O, 1.954(3) and 1.985(4) Å; IZnI, 113.74(3)°; OZnO, 100.5(2)°; and IZnO, 108.5°–113.1(1)°. The crystal structure agrees with the IR and electronic absorption spectra of the crystals.     

X-ray mapping in heterocyclic design: 16. X-ray diffraction study of 1-(4-chlorophenacyl)-4-methyl-1,5,6,7-tetrahydro-2<Emphasis Type="Italic">H</Emphasis>-cyclopenta[<Emphasis Type="Italic">b</Emphasis>]pyridin-2-one

The structure of 1-(4-chlorophenacyl)-4-methyl-1,5,6,7-tetrahydro-2H-cyclopenta[b]pyridin-2-one is studied using single-crystal X-ray diffraction. The structure (a = 37.006(8) Å, b = 8.967(3) Å, c = 27.911(3) Å, β = 96.52(2)°, Z = 24, space group P2₁/c) is solved by direct methods and refined to R₁ = 0.0608 and wR₂ = 0.1170. Six crystallographically independent molecules differ in the dihedral angle between the phenyl and heterocycle planes. The formation of Cl?Cl aggregates is discussed.     

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.     

X-ray structure analysis of 4-cyano-4′-<Emphasis Type="Italic">n</Emphasis>-undecyloxybiphenyl

The structure of a liquid crystal of 4-cyano-4′-n-undecyloxybiphenyl (C₂₄H₃₁NO) is determined by X-ray diffraction. The compound crystallizes in the monoclinic crystal system (space group C2/c) with the unit cell parameters a = 84.108(7) Å, b = 7.159(2) Å, c = 6.922(2) Å, and β = 91.6(4)°. The structure has been solved by direct methods and refined to the residual index R₁ = 0.067. Both phenyl rings are almost planar, and the dihedral angle between these rings is 31.5(6)°.     

Crystal structure of the double magnesium zirconium orthophosphate at temperatures of 298 and 1023 K

Double magnesium zirconium orthophosphate Mg_0.5Zr₂(PO₄)₃ is synthesized by the sol-gel method. The compound prepared is characterized using electron probe microanalysis and X-ray diffraction. The crystal structure of the orthophosphate is refined by the Rietveld method in space group P2₁/n (Z = 4) at temperatures of 298 K [a = 12.4218(2) Å, b = 8.9025(2) Å, c = 8.8218(2) Å, β = 90.466(1)°] and 1023 K [a = 12.4273(5) Å, b = 8.9453(4) Å, c = 8.8405(4) Å, β = 90.320(3)°]. It is demonstrated that an increase in the temperature leads to an anisotropic expansion of the unit cell of the phosphate structure, but the structural type remains unchanged.     

Molecular and crystal structures of 2-amino-5-benzoyl-4-(2-nitrophenyl)-3-cyano-4,5-dihydrothiophene

The crystal structure of 2-amino-5-benzoyl-4-(2-nitrophenyl)-3-cyano-4,5-dihydrothiophene is determined by X-ray diffraction analysis. The unit cell parameters are as follows: a = 10.878(2) Å, b = 12.890(3) Å, c = 13.539(4) Å, α = 108.15(2)°, β = 99.26(2)°, γ = 107.13(2)°, V = 1656(2) ų, d _calcd = 1.410 g/cm³, Z = 4, and space group P1ˉ. The molecules occupy two systems of independent positions in the crystal. Similar to the compounds studied earlier in this series, the o-nitrophenyl substituent has a synperiplanar orientation relative to the hydrogen atom at the C(4) atom of the heterocycle. __________ Translated from Kristallografiya, Vol. 45, No. 2, 2000, pp. 282–285. Original Russian Text Copyright ? 2000 by Nesterov, Kuleshova, Samet, Shestopalov.     

Crystal and molecular structures of 2′-nitro-4-aminobiphenyl and 2-amino-7-nitrofluorene

2′-nitro-4-aminobiphenyl (5), C₁₂H₁₀N₂O₂, crystallizes in the monoclinic space groupP2₁/c:a = 6.043(2),b =15.795(3),c = 11.577(2) Å, β = 103.42(8) °;D _c = 1.324 g cm^?3 forZ = 4. 2-amino-7-nitrofluorene (3), C₁₃H₁₀N₂O₂, crystallizes in the monoclinic space groupP2₁ n:a = 10.765(2),b = 7.454(4),c = 12.959(2) Å, β = 95.44(1) °;D _c = 1.451 g cm^?3 forZ = 4. Three-dimensional CuKα intensity data were measured with a computer-controlled diffractometer, and the initial phases were obtained by direct methods. The two structures were refined by the full-matrix least-squares method, which gave finalR values for 5 and 3 of 0.045 and 0.043, respectively. Bond lengths in the compounds are normal, apart from slight shortening of the phenyl-phenyl C-C bond and some distortion of the phenyl rings caused by the amino and nitro groups. In 5, the two phenyl rings are twisted by 57.1 °, and the nitro group is twisted by 34.6 ° from the plane of its phenyl group. The carbon backbone of 3 is nearly planar with the two phenyl groups tilted by 4.0 ° to each other. The nitro group in 3 is twisted 5.7 ° from the plane of its phenyl group. There is amino hydrogen to nitro oxygen intermolecular hydrogen bonding in each structure.     

Crystal structure of 5-(2′-aminophenyl)-2-dimethylamino-1,3,4-thiadiazole

The crystal structure of 5-(2′-Aminophenyl)-2-dimethylamino-1,3,4-thiazole is determined by X-ray diffraction. The compound is prepared by an unusual recyclization of 3-N, N-dimethylthioureidoquinazolin-4(3H)-one. The crystal is monoclinic, space group P2₁/c, a = 7.420(2) Å, b = 10.466(5) Å, c = 14.752(9) Å, β = 109.2(4)°, ρ_calcd = 1.359 g/cm³, and Z = 4 for the C₁₀H₁₂N₄S composition. The molecule consists of the thiadiazole and phenyl rings and the dimethylamine N(CH₃)₂ and amine NH₂ groups attached to the rings. The molecule as a whole is planar. The dihedral angle between the rings is 8.9°. The N(1) and N(4) atoms in the molecule are bound through the intramolecular interaction (2.76 Å). Molecules, which are linked in pairs by antiparallel hydrogen bonds, form a framework structure.     

Copper(II) bis [2-((E)-2-(pyrid-2-yl)ethylimino)methyl)-6-bromo-4-chlorophenolate]

A new complex CuL ₂ [HL = 2-((E)-(2-(pyridin-2-yl)ethylimino)methyl)-6-bromo-4-chlorophenol] was synthesized, and its structure (C₂₈H₂₂Br₂Cl₂CuN₄O₂, Mr = 740.76) was determined by single-crystal X-ray diffraction analysis. The crystal belongs to the triclinic system, space group $P\bar 1$ , with a = 5.157(6), b = 12.090(1), c =12.310(1) Å, α = 113.962(2)°, β = 96.7910(10)°, γ = 90.0300(10)°, V = 695.4(8) ų, Z = 1, R = 0.0481. The complex molecules are linked via the weak C-H...N hydrogen bonds, leading to the formation of one dimension (1D) chains along the a axis.     

Crystal structure of the molecular complex of 3-[1-(4-nitrophenyl)-3-oxobutyl]-4-hydroxychromen-2-one with ethanol

The crystal structure of 2,3H-2-methyl-4-(4-nitrophenyl)-5-oxobenzopyrano[3,4-e]dihydropyran-2-ol is investigated using X-ray diffraction. The unit cell contains an ethanol molecule that forms hydrogen bonds with O-H and C-O groups of two molecules of the main compound and acts as a proton donor and a proton acceptor in these hydrogen bonds. Owing to these interactions, infinite chains are formed in the crystal. The crystallographic data for the structure of C₁₉H₁₅NO₆·C₂H₅OH (M = 399.39) are as follows: the crystals are triclinic, space group P1, a = 5.5340(3) Å, b = 8.0109(4) Å, c = 11.0112(5) Å, α = 88.773(2)°, β = 84.788(2)°, γ = 79.958(2)°, and Z = 1.     

Crystal structure analysis of 4-phenylquinolin-2-(1<Emphasis Type="Italic">H</Emphasis>)-one

The crystal structure of 4-phenylquinolin-2-(1H)-one (C₁₅H₁₁NO) is determined by X-ray diffraction. The compound crystallizes in the orthorhombic crystal system (space group Pbca) with the unit cell parameters a = 7.382(2) Å, b = 21.795(3) Å, c = 14.066(5) Å, and Z = 8. The structure is solved by direct methods and refined to an R-value of 0.0398 for 1360 observed reflections [F₀ > 4σ (F₀)]. The quinoline moiety and the substituted phenyl ring are nearly planar. The dihedral angle between these two moieties is 64.65(6)°. The crystal structure is stabilized by two intermolecular N-H?O and C-H?O interactions.     

Crystal and molecular structures of a samarium complex with the 3,5-Di-tert-butyl-1,2-quinone-1-(2-hydroxy-3,5-Di-tert-butylphenyl)imine ligand

X-ray structure analysis of Sm(C₂₈H₄₀NO₂)₃ is performed. The crystals are monoclinic, a = 13.490(2) Å, b = 27.955(5) Å, c = 23.000(6) Å, β = 105.30(2)°, Z = 4, space group P2₁/c, and R = 0.0332 for 9670 reflections. The coordination number of the Sm atom is nine (tricapped trigonal prism with the O atoms in the base and the N atoms at the caps). The approximate symmetry of the complex is D ₃. The mean C-O and C-N bond lengths (1.266 and 1.342 Å, respectively) correspond to the monoanion redox form of the ligands. In distinction to the earlier studied complexes ML ₂ with the same ligands, the six-membered rings in the ligands of this complex are essentially noncoplanar: the dihedral angles between them are 42.8°, 34.0°, and 41.1°.     

X-ray mapping in heterocyclic design: XI. X-ray diffraction study of 1-benzoyl-3-(pyridin-2-yl)-thiocarbamide and the product of its reaction with oxidants

The structures of 1-benzoyl-3-(pyridin-2-yl)-thiocarbamide C₁₃H₁₁N₃O₁S₁ (I) and 2-benzoylimino-1,2,4-thiadiazole[2,3-a]pyridine C₁₃H₉N₃O₁S₁ (II) are studied by X-ray diffraction. Structures I [a = 5.342(4) Å, b = 20.428(5) Å, c = 11.784(4) Å, β = 90.55(2)°, Z = 4, space group P2₁/n) and II [a = 6.258(6) Å, b = 18.068(14) Å, c = 10.185(10) tA, β = 95.45(8)°, Z = 4, space group P2₁/n) are determined by direct methods and refined to R ₁ = 0.0673 and 0.0802, respectively. In structure I, both intramolecular (involving the O atom) and intermolecular (involving the N and S atoms) hydrogen bonds are observed. The latter bonds are responsible for the formation of centrosymmetric molecular dimers. In structure II, a short intramolecular contact (2.168 Å) is observed between the S and O atoms.     

X-ray mapping in heterocyclic design: XIII. Structure of substituted tetrahydroquinolines

The structures of 4-methyl-2-chloro-5,6,7,8-tetrahydroquinoline [a = 8.138(2) Å, b = 11.127(4) Å, c = 11.234(2) Å, β = 111.30(2)°, Z = 4, space group P2₁/c, 4-methyl-2-methoxy-5,6,7,8-tetrahydroquinoline [a = 5.7651(16) Å, b = 8.530(2) Å, c = 10.455(3) Å, α = 73.76(2)°, β = 86.95(2)°, γ = 83.97(2)°, Z = 2, space group P $\bar 1$ , 4-methyl-2-(4-chlorophenacyl)-5,6,7,8-tetrahydro-1H-quinolin-2-one [a = 8.873(2) Å, b = 17.137(2) Å, c = 24.515(4) Å, Z = 8, space group Pbn2₁], and 2-(4-chlorophenyl)-5-methyl-6,7,8,9-tetrahy-drooxazolo[3.2-a]quinolin-10-ylium perchlorate [a = 8.110(6) Å, b = 17.818(7) Å, c = 17.721(5) Å, β = 100.46(4)°, Z = 4, space group P2₁/c] are studied by single-crystal X-ray diffraction. The structures are solved by direct methods and refined by the full-matrix least-squares procedures in the anisotropic approximation to R = 0.0581, 0.0667, 0.0830, and 0.0607, respectively.     

Synthesis and structural study of 1-(N,N-diethylamino)-2,2-bis(2-nitrophenylthio)ethene

The synthesis, variable temperature NMR spectra, and crystal structures of two crystalline forms, 2a and 2b, of the enamine 1-(N,N-diethylamino)-2,2-bis(2-nitrophenylthio)ethene have been obtained. Both forms crystallize in the monoclinic space group P2₁/a. The two phases have similar molecular structures but possess different intermolecular C–H······O hydrogen bonding interactions. Both forms exhibit disorder within the NEt₂ fragment at 298 K: sufficient disorder persisted with 2a (orange needles) down to 100 K to make the geometric parameters pertaining to the enamine fragment unreliable. The disorder was effectively eliminated on cooling 2b down (red colored blocks) to 150 K. Cell dimensions for the 2a-phase are at 100 K: a = 11.1030(4) Å, b = 15.1325(7) Å, c = 12.4504(7) Å, β = 114.606(3)°, while for the 2b-phase at 150 K, a = 15.5206(4) Å, b = 7.6958(2) Å, c = 15.7137(3) Å, β = 92.580(7)°. The C–N bond length in the β-form at 150 K of 1.335(3) Å indicates considerable double bond character: the rotational barrier of the C–N bond in CDCl₃ was calculated to be 52.4 kJ mol^?1.     

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.