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.     

The structure of 1-(p-fluorophenylmethyl)-2-(4-methyl-1-piperazinyl)-1H-benzimidazole hydrogen fumarate

The crystal and molecular structure of the title compound has been determined by X-ray analysis. The 1-(p-fluorophenylmethyl)-2-(4-methyl-1-piperazinyl)-1H-benzimidazole ion cocrystallizes with fumaric acid, (C₁₉H₂₂N₄F⁺·C₄H₃O ₄ ^– ), in space group P-1 with cell dimensions a = 9.938(1), b = 10.131(1), c = 12.712(1) Å, = 86.57(1), = 69.41(2), and = 67.22(2)°. The piperazine N4 atom is protonated and contacts the deprotonated O atom of the fumarate anion through a hydrogen bond. The benzimidazole ring is nearly planar and makes a dihedral angle of 111.25(12)° with the fluorophenyl ring. The piperazine ring adopts a chair conformation.     

Crystal Structure and Hirshfeld Surface Analysis of (E)-1-(4-Bromophenyl)-2-(2,2-Dichloro-1-(4-Fluorophenyl)vinyl)diazene

Crystallography Reports - The CuCl-catalyzed olefination with CCl4 in the presence of tetramethylethylenediamine in DMSO leads to the formation of...     

Crystal Structure of 4-Bromo-3,4-Dichloro-1-(1-Morpholinyl)-1-(Decylsulfanyl)-2-Nitro-Buta-1,3-Diene

Abstract  

The compound 4-bromo-3,4-dichloro-1-(1-morpholinyl)-1-(decylsulfanyl)-2-nitro-buta-1,3-diene was synthesized from the reaction of 4-bromo-1,3,4-trichloro-1-(decylsulfanyl)-2-nitro-buta-1,3-diene with morpholine and characterized by elemental analysis, IR spectrum, UV spectra, ¹H NMR,¹³C NMR and X-ray single crystal determination. In the title compound, C₁₈H₂₉BrCl₂N₂O₃S, crystallizes in the monoclinic space group P2₁/c, a = 15.8326(4) Å, b = 8.9915(10) Å, c = 16.7528(5) Å, β = 100.808(10)°, V = 2,342.6(3) Å³, Z = 4, R ₁ = 0.0590 and wR ₂ = 0.0940. The morpholine ring adopts a chair conformation. The morpholine ring and the butadiene group are inclined at an angle of 113.4 (1)°. The butadiene unit is not planar as can be expected if the two double bonds are fully conjugated.     

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 and molecular structures of 1-(2-carboxypropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (1) (C17H21NO4) and 1-(2-carbamoyl propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C17H22N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol containing 2-methylalanine fragment are described in this paper. The space groups and unit-cell parameters are: compound1 (C₁₇H₂₁NO₄): monoclinic, space groupP2₁/n,a=5.787(1),b=18.703(4),c=23.526(5)Å,=96.49(2)°; compound2 (C₁₇H₂₂N₂O₃): triclinic, space groupP¯1,a=8.321(1),b=10.121(1),c=10.368(1)Å,=109.49(1)°,=90.49(1)°, =103.48(1)°. The structures were solved by direct methods and refined with full matrix least-squares techniques toR indices of 0.055 and 0.049, respectively. The molecules of compound1 exist in the crystal as dual ions. The molecules of compound2 are compact and their external chain is twisted in a characteristic way (similar to that found in peptides).     

Silver (I) coordination by 1-(t-butyl)-2-benzoylaziridine

The reaction between AgNO₃ and 1-(t-butyl)-2-benzoylaziridine (tBBA) leads to the formation of bis-(1-(t-butyl)-2-benzoylaziridine) nitrato silver (I) which is a new metal aziridine derivative. The crystal structure was established by X-ray diffraction. [Ag(tBBA)₂(NO₃)] crystallizes in space groupC222₁ witha=11.877(6),b=13.560(4),c=16.923(4)Å andZ=4. The silver atom is six-coordinated by two N atoms of two aziridine rings (Ag-N=2.39(1)Å), two O atoms of two benzoyl groups (Ag-O=2.60(1)Å) and two O atoms of the nitrato group (Ag-O=2,60(1) Å). The coordination around the silver atom defines a very distorted octahedron with the C2 symmetry. The twofold axis passes through one O and the N nitrato atoms, and the silver atom. The nitrato group and tBBA act as bidentate ligands. These results are in contrast with our previous studies on aziridine zinc (II) complexation where the zinc atom is not coordinated by the benzoyl group.     

X-ray crystallographic analysis and NMR study of (Z)-3(2-hydroxyphenyl)-1(4-methoxyphenyl)-3-oxo-prop-1-en-1-ol

The molecular structure of the title compound has been determined by X-ray crystallography. The enol form is present in the solid state and each of the two molecules in the asymmetric unit possesses two intramolecular hydrogen bonds. The delocalization of double bonds results in an almost planar molecule. Evidence to support the enol configuration in solution is presented from an NMR investigation.     

Crystal and molecular structures of 1-(2-methyloxycarbonylo-propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol hydrochloride (1) (C18H24NO4Cl) and 1-(2-methylcarbamoylpropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C18H24N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol, are reported in this paper. The space groups and unit-cell parameters are: compound1 (C₁₈H₂₄NO₄Cl), monoclinic,P2₁,a=7.215(1),b=8.591(1),c=15.017(1)Å,=95.64(1)°; compound2 (C₁₈H₂₄N₂O₃), monoclinic,P2₁/c,a=10.218(3),b=21.616(5),c=8.124(2)Å,=101.28(2)°. The structures were solved with direct methods and refined by full-matrix least-squares techniques toR indices of 0.036 and 0.066, respectively. The molecule of compound1 has an extended external chain, and thus its structure is linear, whereas the molecule of compound2 is compact, and its external chain is twisted in a characteristic way, as is the case of peptides.     

Crystal structures of 1-(2-hydroxyphenyl)-3-phenyl-1,3-propanedione and 1-(1,3-benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione

1-(2-Hydroxyphenyl)-3-phenyl-1,3-propanedione crystallizes in the triclinic space group (a=5.4233(5),b=13.910(1),c=17.036(1) Å, =68.311(6), =80.854(7), =78.760(8)°) as two independent enolic tautomers in which the hydroxyl and phenolic protons are hydrogen bonded to the ketonic oxygen atom. The structure was refined toR=0.039 for 2085I3(I) reflections. 1-(1,3-Benzodioxol-5-yl)-3-(2,4-dimethoxyphenyl)-1,3-propanedione, which belongs to the triclinic space group (a=7.3990(7),b=8.1239(5),c=14.004(1) Å, =86.673(6). =88.574(7), =64.885(7)°) also exists in the enolic form. The structure was refined toR=0.040 for 1564I3(I) reflections.     

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.     

Crystal structure of triphenylphosphine-(1-(di(trifluoromethyl)-hydroxymethyl)-cyclopentadienyl)-(1,2-di(carboxymethyl) ethylene-1-yl) ruthenium (0)

The structure of triphenylphosphine — (1 — (di(trifluoromethyl) — hydroxymethyl) — cyclopentadienyl) — (1,2 — di(carboxymethyl)ethylene — 1 — yl) — ruthenium (0) has been studied by single-crystal X-ray diffraction techniques. This compound, [C₅ H₄(CF₃)2 COH] Ru(PPh₃)C2(CO₂Me)₂H, crystallizes in the triclinic space groupP¯1 witha =10.131,b= 15.107,c= 10.798 Å, = 102.14, = 107.04, = 89.64° andZ = 2. The structure was refined by block-diagonal least-squares methods to a finalR value of 0.042, including hydrogen atoms. The compound contains a dicarboxymethylethylene ligand coordinated to ruthenium both through a ketonic oxygen and through a metal--carbon -bond. An intramolecular hydrogen bond is observed. Details of the structure are reported, and the structures of several Ru(0) complexes are compared.     

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.     

Crystal and molecular structures of 1-(2-ethyloxycarbonylo propan-2-ylamino)-3-(1-napthyloxy) propan-2-ol-hydrochloride (1) (C19H26NO4Cl) and 1-(2-isopropyloxycarbonylo-propan-2-ylamino)-3-(1-napthyloxy) propan-2-ol hydrochloride (2) (C20H28N04Cl)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol, are shown in this paper. The space groups and unit-cell parameters are: compound1 (C₁₉H₂₆NO₄Cl): triclinic, space groupP1,a=6.420(1),b=10.161(1),c=15.823(1) Å,=82.47(1),=84.16(1), =77.55(1)°; compound 2 (C₂₀H₂₈NO₄Cl): monoclinic, space groupP2₁/c,a=6.460(1),b=33.285(2),c=10.120(1) Å,=104.83(1)°. The structures were solved by direct methods and refined with full-matrix least-squares techniques toR indices of 0.055 and 0.048, respectively. The –CH(OH)-CH₂-NH-sections of the side chains show the conformation approximate togauche.     

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.