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...     

Single Crystal X-ray Study of 6-Phenyl-4-(p-tolyl)pyridin-2(1H)-one

Crystallography Reports - The title compound 6-phenyl-4-(p-tolyl)pyridin-2(1H)-one was synthesized via one-pot, three component reaction of (E)-1-phenyl-3-(p-tolyl)-2-propen-1-one, ethyl...     

Synthesis and crystal structure elucidation of 1-(4-fluorobenzyl)-2-(4-cyanophenyl)-1H- benzimidazole-5-carbonitrile

The synthesis and spectral identification of 1-(4-fluorobenzyl)-2-(4-cyanophenyl)-1H-benzimidazole-5-carbonitrile (1) have been reported. IR, ¹H NMR, and EI mass spectral analysis were used for its spectral identification. The structure of 1 was confirmed by X-ray crystallographic studies. Intramolecular hydrogen bond occurs between the imidazole nitrogen and one of hydrogen of the florobenzene. The crystal packing is governed by C–HN intermolecular hydrogen bonds. The molecular structure observed in crystal and the optimised geometries at the HF level by doing semi-empirical and ab initio calculations were compared.     

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.     

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...     

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.     

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.     

Methyl 4-((E)-2-{3-[(3-{ (E)-2-[4-(methoxycarbonyl)phenyl]- 1-diazenyl}-5,5-dimethylhexahydro-1-pyrimidinyl)methyl]-5,5-dimethylhexahydro-1-pyrimidinyl-1-diazenyl) benzoate. X-ray crystal structure

Methyl 4-((E)-2-{3-[(3-{(E)-2-[4-(methoxycarbonyl)phenyl]-1-diazenyl}-5, 5-dimethyl hexahydro-1-pyrimidinyl)methyl]-5, 5- dimethylhexahydro-1- pyrimidinyl}-1- diazenyl) benzoate (1) has been synthesized by reaction of a mixture of formaldehyde and 2,2-dimethyl-1,3-propanediamine with p-methoxycarbonylbenzenediazonium chloride. The crystal structure of 1 has been determined by single crystal X-ray diffraction analysis. The crystals of 1 displayed problems of disorder; the asymmetric unit is built up by two independent molecules, which display disorder within a methoxycarbonyl group. The two independent molecules in the asymmetric unit are very similar, differing only slightly about the mutual orientation of the aryltriazenyl groups. With respect to the N–C–N bridge between the hexahydropyrimidinyl rings, the two equivalent fragments containing the triazene moieties are in a cis orientation. The N–N single bonds, in the range 1.319(4)–1.348(4) Å, and the N=N double bonds, in the range 1.255(5)–1.275(4) Å, indicate significant conjugations within the triazene moieties. All the hexahydropyrimidine six-membered rings adopt a chair conformation as shown by their puckering parameters. The crystal packing is determined only by simple van der Waals interactions. The crystal structure of 1 is compared with the previously reported structure of the unbranched hexahydropyrimidine analogue 2. Crystal data: 1 C29H40N8O4, triclinic, space group P-1, a = 13.9652(2), b = 14.2908(3), c = 16.6129(4) Å, = 97.279(1), = 90.872(1), = 107.385(1), V = 3133.6(1) ų, for Z = 4.     

The Synthesis and Physical Properties of Some 1-n-Alkyl-4-(4-substituted phenyl) bicyclo(2.2.2)octanes

The preparation and mesomorphic properties of a number of 1-n-alkyl-4-(4-n-alkyl- and 4-n-alkoxy-phenyl)bicyclo(2.2.2)octanes and 1-n-alkyl-4-(4′-n-alkylbiphenyl-4-yl)bicyclo(2.2.2)octanes are described. The clearing temperatures reported emphasise the high thermal stability conferred upon liquid crystal phases by the presence of the bicyclo-octane ring in a mesogen. Some physical data relating to the use of such materials in mixtures for electro-optical displays have been obtained.     

Molecular and crystal structures of 1-methyl-2-Oxo-3-acetoxy-4-hydroxy-4-(Phenyl)piperidine, 1-ethyl-2-oxo-3,4-dihydroxy-4-(Pyridyl)piperidine, and 1-benzyl-2-oxo-3,4-dihydroxy-4-(Pyridyl)piperidine and the role of hydrogen bonds in molecular packing in crystals

The molecular and crystal structures of 1-methyl-2-oxo-3-acetoxy-4-hydroxy-4-(phenyl)hydropyridine, 1-ethyl-2-oxo-3,4-dihydroxy-4-(pyridyl)piperidine, and 1-benzyl-2-oxo-3,4-dihydroxy-4-(pyridyl)piperidine are determined by X-ray diffraction analysis. These three hydroxy derivatives of hydropyridine are the convenient model compounds in studies of the influence of intramolecular and intermolecular hydrogen bonds on the conformation and packing of molecules in crystals. The molecules of hydroxy derivatives possess a considerable conformational flexibility and can form an extended network of intramolecular and intermolecular hydrogen bonds. It is shown that these compounds more often than others form noncentrosymmetric and polysystem crystals. The role of the molecular association and the type of hydrogen-bonded associates (syntons) in crystal packing are discussed.     

Synthesis and crystal structures of 5-amino-1-(2-hydroxyethyl)imidazole-4-carboxamide and 5-amino-1-(2-chloroethyl)-4-cyanoimidazole

Both 5-amino-1-(2-hydroxyethyl)imidazole-4-carboxamide (AHIC) and 5-amino-1-(2-chloroethyl)-4-cyanoimidazole (ACCI) have been synthesized and crystallized in the monoclinic space group P2₁/c, Z = 4, with a = 8.420(2), b = 9.759(2), c = 10.583(2) Å, = 111.80(2)° for AHIC and a = 6.139(1), b = 8.522(2), c = 15.156(3) Å, = 96.71(2)° for ACCI. Differences in the molecular geometries of the two compounds are attributed to the differences in the substituents at the 1- and 4-positions of the imidazole ring. The molecular conformation of AHIC is stabilized by intramolecular hydrogen bonding between the 5-amino and the vicinal carboxamide moiety, resulting in an extended planar structural pattern. The presence of the cyano group in the 4-position of ACCI prevents the formation of such an intramolecular hydrogen bond. Both the crystal structures are stabilized by networks of intermolecular hydrogen bonds.     

Synthesis and crystal structure of 1-(4-bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane

1-(4-Bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane, C₁₃H₁₅BrO₃, has been synthesized from 4-bromophenylacetic acid chloride via the oxetan ester (3-methyl-3-oxetanyl)methyl-2-(4-bromophenyl)acetate. The crystal structure of the title compound has been determined at low temperature (120 K), by X-ray diffraction methods. This compound crystallizes in the monoclinic space group P2₁/n (No. 14), Z = 4, with lattice parametersa = 6.019(5), b = 20.990(5), c = 9.915(2) Å, and = 101.29(1)°.     

The utility of 4-aminobenzoic acid in promotion of hydrogen bonding in crystallization processes: the structures of the cocrystals with halo and nitro subsituted aromatic compounds, and the crystal structures of the adducts with 4-nitroaniline (1:1), 4-(4-nitrobenzyl)pyridine (1:2), and (4-nitrophenyl)acetic acid (1:1)

A number of molecular adducts of 4-aminobenzoic acid (4-ABA) have been prepared and characterized using infrared spectroscopy and in three cases by X-ray diffration methods. These three compounds are with 4-nitroaniline [(4-ABA) (C₆H₆N₂O₂)], 4-(4-nitrobenzyl) pyridine, [(4-ABA)₂(C₁₂H₁₀N₂O₂)₄], and (4-nitrophenyl)acetic acid, [(4-ABA) (C₈H₇NO₄)]. Other compounds described are with 4-chlorobenzoic acid, [(4-ABA) (C₇H₅ClO₂)], 4-bromobenzoic acid, [(4-ABA) (C₇H₅BrO₂)], 4-cyanobenzoic acid, [(4-ABA) (C₇H₆N₂)], 2-nitrobenzoic acid, [(4-ABA) (C₇H₅NO₄)], and 3-nitrobenzoic acid, [(4-ABA) (C₇H₅NO₄)]. All compounds have 1:1 stoichiometry except that with 4-(4-nitrobenzyl)pyridine (1:2) which is unique in being retro-stoichiometric. A review of the systematics of the 4-aminobenzoic acid adducts is also made, particularly with respect to the infrared characterization of the cocrystalline materials and prediction of their NLO potential.     

Mn(II) and Zn(II) Complexes Constructed by Bis(4-(1H-Imidazol-1-yl)phenyl)methanone and Salicylate: Syntheses and Crystal Structures

Crystallography Reports - Two complexes with V-shaped ligands, [(L1)2Mn(H2O)4](HSA)2] (1), {[(L1)2Zn(H2O)2](HSA)2}n (2) (L1 = bis(4-(1H-imidazol-1-yl)phenyl)methanone, H2SA = salicylic acid), have...     

Crystal Structure of 1-(4-Pyridylmethyl)-2,4,6-Triphenyl Pyridinium Perchlorate

1-(4-pyridylmethyl)-2,4,6-triphenyl pyridinium perchlorate crystallizes in space groups P1 with 3 molecules per asymmetric unit. The cell parameters obtained are: a = 12.142(3), b = 16.972(4), c = 20.229(7) Å, α = 83.66(4), β = 74.83(3), and γ = 69.47(2)°. The crystal structure was determined using the direct methods technique. Anisotropic refinement was undertaken using block diagonal least squares. In the final cycle of the refinement the reliability factor was found to be R₀ = 0.084 for 3982 reflections with I ≧ 3σ (I). All rings are planar within experimental errors. Rings B, C, D, and E are twisted with respect to the central plane.     

Synthesis and some Physical Properties of 1-Cyclohexyl-2-(4”-Halobiphenyl-4'-yl)Ethanes

A series of 1-(trans-4'-n-alkylcyclohexyl)-2-(4”-halobiphenyl-4'-yl)ethanes, which show nematic phases, was prepared. Their transition temperatures, enthalpies and entropies were measured. Their bulk viscosities, birefringences and dielectric constants were determined by extrapolation. 1-(trans-4'-n-propylcyclohexyl)-2-(4”-fluorobiphenyl-4'-yl)ethane has a high clearing of 125° C, a low viscosity of 25 c.p. at 20 °C, a relatively high birefringence of 0.166 at 25 °C, and a positive dielectric anisotropy of 4.9. The transition temperatures, the N-I transition entropies, the bulk viscosities and the birefringences for the 1-(trans-4'-n-alkylcyclohexyl)-2-(4”-fluorobiphenyl-4'-yl)ethanes exhibited odd-even effects in relation to the number of carbon atoms in the alkyl chain. The bulk viscosity as a function of the third power of the van der Waals radius of the halogeno group, the birefringence as a function of the van der Waals radius of the halogeno group, and the dielectric constants as a function of the dipole moment of the halogeno group are discussed for the 1-(trans-4'-n-propylcyclohexyl)-2-(4”-halobiphenyl-4'-yl)ethanes.     

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.      

Synthesis, spectroscopy, magnetism, and X-ray structures of hexakis(1-(2-chloroethyl)-tetrazole-N4)copper(II) salts

The compounds hexakis(1-(2-chloroethyl)-tetrazole-N4)copper(II) tetrafluoroborate mono(1-(2-chloroethyl)-tetrazole) (1) and hexakis(1-(2-chloroethyl)-tetrazole-N4) copper(II) perchlorate mono(1-(2-chloroethyl)-tetrazole) (2) were obtained from the crystallization of 1-(2-chloroethyl)-tetrazole (teec) with the respective copper salt. The X-ray structures are reported. Both compounds crystallize in the monoclinic space group C2/c for 1: a = 25.754(3) Å, b = 18.162(3) Å, c = 10.298(2) Å = 104.294(7)° and Z = 4 and for 2: a = 25.745(3) Å, b = 18.197(3) Å, c = 10.29355(3) Å = 104.512(10)° and Z = 4. The Cu^II ions are octahedrally surrounded by six teec ligands. One free teec ligand is present in the structures. The Cu–N distances in the centrosymmetrical units are 2.01, 2.04, and 2.39 Å in both compounds, consistent with a Jahn–Teller elongated octahedron. The ligand field spectra of both compounds show a signal in the visible range at about 15.200 cm^–1 and by an EPR spectrum the following values are found: g _| = 2.29 and g = 2.03. The compounds are both paramagnetic and the T value of 0.37 cm^–1 K mol^–1, which is associated with S = 1/2, is what would be expected for a mononuclear Cu^II complex.     

Crystal structures of three 1-arylpropane-1,2-diol 2-aryl ether derivatives and the acetate of 2,6-dimethoxy-4-(1-(E)-propenyl)phenol

The crystal structures ofthreo-2-[2,6-dimethoxy-4-(1-(Z)-propenyl)phenoxy]-1-(4-hydroxy-3,5-dimethoxyphenyl)-1-propanol (7b),threo-2-(2,6-dimethoxy-4-propylphenoxy)-1-(3,4-5-trimethoxyphenyl)-1-propanol (7c), the diacetate oferythro-2-[2,6-dimethoxy-4-(1-(Z)-propenyl)phenoxy]-1-(4-hydroxy-3,5-dimethoxyphenyl)-1-propanol (8d) and the acetate of 2,6-dimethoxy-4-(1-(E)-propenyl)phenol (9) have been determined by single-crystal X-ray diffraction methods;7b,7c, and8d are structurally closely related to a class of optically-active neolignans of 1-arylpropane-1,2-diol 2-aryl ether type occurring in plant extracts. The reflection intensities were recorded at room temperature for7b and8d, at -140°C for7c and at -120°C for9. Compound7b crystallized as needles in the orthorhombic space groupPna2₁ witha=27.055(3),b=11.850(8),c=6.717(4)Å andZ=4.R became 0.041 for 1792 observed [I>3(I)] reflections used in the refinement of the structure. Compound7c crystallized as prisms in the monoclinic space groupP2₁/a witha=12.565(4),b=13.96(1),c=12.846(7)Å,=93.86(3)° andZ=4. The refinement gaveR=0.051 for 2101 observed [I>3(I)], unique reflections. Compound8d crystallized as prisms in the monoclinic space groupP2₁/n witha=13.182(4),b=8.518(5),c=23.322(5)Å,=106.12(2)° andZ=4. The finalR-valuebecame 0.042 for 2131 observed [I>3(I)], unique reflections. Compound9 crystallized as prisms in the orthorhombic space groupPca2₁ witha=18.216(4),b=9.483(3),c=7.416(2)Å andZ=4. TheR-value became 0.038 for 1502 observed [I>3(I)], unique reflections. The crystals of7b are stabilized by moderately strong hydrogen bonds. All the 1-arylpropane-1,2-diol 2-aryl ethers examined adopted conformations in which the aromatic groups tend to be as remote as possible. Observed double bond lengths in the propenyl groups of the compounds examined (1.30 Å) deviate significantly from the expected value (1.34 Å). The cause of this discrepancy is discussed.     

Synthesis of a Cobalt Coordination Polymer Based on 4-(1H-Imidazol-1-yl)phenyl)methanone and Fumaric Acid

Crystallography Reports - A cobalt coordination polymer with V-shaped ligands, {[Co0.5(L1) ⋅ (C4H2O4)0.5] ⋅ 0.25H2O}n, (L1 = 4-(1H-imidazol-1-yl)phenyl)methanone, C4H2O4 =...