Crystal and molecular structure studies of 2-(3-chlorophenyl),3,5-diphenylisoxazolidine

The structure of the title compound, 2-(3-chlorophenyl),3,5-diphenylisoxazolidine (C₂₁H₁₈ NOCl) (1) has been investigated by X-ray crystallography. Compound (1) crystallizes in orthorhombic space group P2₁2₁2₁ with cell parameters a=10.288(17) Å, b=37.98(3) Å, c=8.809(9) Å, Z=8. Compound (1) has both intra- and intermolecular hydrogen bonds.     

Crystal and molecular structure of (E)-2-t-butyl-3(3′-t-butyldimethylsiloxy)propyl-2-cyanocyclobutanone

The title compound crystallizes in the monoclinic space group P2₁/a, witha+12.906(9).b+11.604(2).c+14.631(9) Å, β=108.70(3)° andZ+4. The structure was solved by direct methods from diffractometer data and refined to a finalR value of 0.057 for 2020 independent reflections. The structure analysis confirms the cis disposition of the bulky substituents and indicates a puckered four-membered ring with a dihedral angle of 18.5° as expected for a non-centrosymmetrically substituted cyclobutanone.     

Crystal and molecular structure of di(1-pyrazolyl)methane,CH2(C3N2H3)2

The title compound consists of two planar pyrazolyl fragments oriented at 73.0° to each other and linked to a common carbon atom. All hydrogen atoms were located unambiguously and their positions were refined.     

Crystal and molecular structure of (2R,3R)-2-exo-((1R)-1-hydroxy-2-methyl-propyl)-3-exo-hydroxymethyl-bicyclo[2.2.1]-hept-5-ene,C12H20O2

The stereogeometry of the title compound which was prepared by a stereoselective addition reaction, has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, P2₁,a=10.495(16),b=8.392(16),c=13.209(20) Å, =93.80(8),Z=4. The crystal structure has been solved by vector search methods and refined toR=0.05 for 782 observed reflections.     

Crystal structure of bis(2-butyl-4-chloro-imidazole)5-iminoethane

The title compound (C₁₈H₂₆N₆Cl₂) crystallizes in monoclinic space group P2₁/c with a = 14.867(4) Å}, b = 7.758(2) Å}, c = 9.671(3) Å}, = 108.78(1), V = 1056.0(5) Å}³, Z = 2, D_cal = 1.250 Mg/m³ at T = 293 K. The structure was solved by direct methods and refined by full-matrix least-squares procedures to final R = 0.0650 and wR = 0.1719 using 2493 reflections. The imidazole ring is planar and the n-butyl chain adopts an extended conformation. The molecules in the crystal are stabilized by N–H s N type of intermolecular hydrogen bondings in addition to van der Waals forces.     

Spectroscopic studies, antimicrobial activities, and crystal structure of N-[2-hydroxy-1-naphthylidene]3, 5-bis(trifluoromethyl)aniline

A new Schiff base compound has been synthesized by the reaction of 2-hydroxy-1-naphthaldehyde with 3,5-bis(trifluoromethyl)aniline.The title compound was characterized by elemental analysis, IR,¹H NMR,¹³C NMR, and UV–Visible techniques.Its UV–Vis spectra was examined in polar and nonpolar solvents and in acidic and basic media. The crystal structure of the compound showed the OH group to be ortho to the imine group. It crystallizes in the monoclinic space group P2₁ with a = 11.328(2), b = 6.125(1), c = 11.937(2) ?, V = 825.1(2) ?³, D _x = 1.543 g cm⁻³and Z = 2. An intramolecular O1- H⋯N1 [2.558(7) ?] hydrogen bond stabilizes the molecule. The compound has also been characterized by its antimicrobial activities. The ligand has been screened in vitro against the organisms Escherichia coli ATCC 11230, Staphylococcus aureus ATCC 6538, Klebsiella pneumoniae UC57, Micrococcus luteus La 2971, Proteus vulgaris ATCC 8427, Pseudomonas aeruginosa ATCC 27853, Mycobacterium smegmatis CCM 2067, Bacillus cereus ATCC 7064, and Listeria monocytogenes ATCC 15313, the yeast cultures Candida albicans ATCC 10231, Kluyveromyces fragilis NRRL 2415, Rhodotorula rubra DSM 70403, Debaryomyces hansenii DSM 70238, and Hanseniaspora guilliermondii DSM 3432.     

Crystal structure of pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate, (NH3(CH2)2NH3)5(Sb2Cl11)2·4H2O

The pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate salt is monoclinic with the following unit cell dimensions:a=16.271(5) Å,b=13.004(4) Å,c=13.932(4) Å, β=111.72(2)°, space groupP2₁/c withZ=2. The structure was solved by Patterson methods and refined to a finalR value of 0.023 for 4435 reflections withF ₀>4σ(F ₀). The structure shows a layer arrangement perpendicular to thea axis: planes of the [Sb₂Cl₁₁]⁵⁻ bioctahedra alternate with planes of [NH₃(CH₂)₂NH₃]²⁺ dications. The [Sb₂Cl₁₁]⁵⁻ bioctahedra are connected through O−H...Cl hydrogen bonds, such that infinite chains of composition [Sb₂Cl₁₁(H₂O]_n ⁵ⁿ⁻ are formed in the structure, parallel to the twofold axis. These chains are themselves interconnected by means of N−H...Cl and O−H...Cl bonds originating from the [NH₃(CH₂)₂NH₃]²⁺ entities and the water molecules, respectively, and form a threedimensional network.     

Crystal and molecular structure of the bidentate ligand 2,2-di(1-pyrazolyl)propane,CH3C(C3N2H3)2CH3

The title compound lies on a site of C₂ symmetry, with the two planar pyrazolyl moieties oriented at 86.1° to one another. The hydrogen atoms were located and refined.     

Crystal and molecular structure of the ethanol adduct of tris(oxinato)indium(III)

The ethanol adduct of tris(oxinato)indium(III), prepared in aqueous ethanol, crystallizes in the monoclinic space groupP2₁/n (Nr.14) witha=11.343(2),b=13.477(3),c=16.845(2)Å, -94.71(1)°,V=2566.4(8)ų andZ=4. The structure was solved by direct methods and refined by full-matrix least-squares methods toR=0.032 for 3374 observed reflections withI>2 (I). Three bidentate oxinato ligands (or 8-quinolinolato) coordinate to indium atom leading to an approximately octahedral coordination of the metal(III) ion. One ethanol molecule per mole of metal complex is occluded in the crystal lattice and forms a hydrogen bond with the O(3) oxygen atom of one oxinato ligand [O(3) ... O(4) =2.715(3) Å]. The two other oxinato ligands of the same unit are not involved in hydrogen bonding.     

Crystal and molecular structure of the symmetrical bidentate ligand 3,3-di(1-pyrazolyl)pentane, CH3CH2C(C3H3N2)2CH2CH3

The title compound crystallizes in the centrosymmetric space group C2/c with a = 14.4005(23), b = 7.0494(12), c = 11.2462(20) Å, = 101.572(13)° and Z = 4; the molecule lies on a crystallographic C ₂ axis. Hydrogen atoms were both located and refined.     

Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).     

Crystal structure and phase transition in the compound [C6H5CH2NH(CH3)2]TlCl4

The N‐N dimethyl benzylammonium tetrachlorothallate (III) [C₆H₅CH₂NH(CH₃)₂]TlCl₄ crystallizes in the monoclinic system P2₁/n at room temperature with the following unit cell dimensions: a = 7.725(3) Å, b = 14.080(5) Å, c = 13.697(4) Å, β = 91.2(2)° with Z = 4. The structure shows a layer arrangement perpendicular to the b axis: planes of [TlCl₄]^‐ tetrahedra alternate with planes of [C₆H₅CH₂NH(CH₃)₂]⁺ cations. The cohesion of the atomic arrangement is ensured by hydrogen bonds N‐H…Cl. Differential scanning calorimetric and optical birefringence measurements reveals a phase transition at T = 339K. Raman spectroscopic study and dielectric measurements were performed to discuss the mechanism of the phase transition. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

Crystal and molecular structure of iso-grayanotoxin II

The crystal and molecular structure of a grayanotoxin derivative, iso-grayanotoxin II, is presented. The crystal is orthorhombic, space group . The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered rings with various conformations.     

Crystal and molecular structure of tris(2-aminocyclopentene-1-dithiocarboxylato)-cobalt (III) monoacetone

The title compound crystallizes in the monoclinic space groupP2₁/c withZ=4 and cell dimensionsa=7.724(1),b=19.274(5),c=18.638(4) Å, and =105.68(2) °. Refinement with 1126 terms, measured with MoK radiation on a diffractometer, has yielded a conventionalR factor of 0.059. The non-hydrogen atoms in the complex molecule were refined with anisotropic temperature factors whereas those in the acetone molecule were refined isotropically. The nitrogen atoms in the complex are not coordinated; the coordination sphere involves Co—S₆ bonding of approximateD ₃ symmetry, the average Co—S bond length being 2.275 Å. The geometry of the coordination sphere with respect to a definedC ₃ reference axis is similar to that found in several tris(N,N-disubstituted-dithiocarbamato)cobalt(III) complexes. The acetone molecule is hydrogen bonded to one of the amino groups, the O N distance being 2.99 Å.     

Crystal structure and phase transition of single crystalline CsNH2SO3

Differential scanning calorimetry (DSC) and X‐ray diffraction measurements have been performed on cesium sulfamate CsNH₂SO₃ single crystal. Two distinct endothermic peaks in the DSC curves are observed at 330 and 436 K. It is pointed out that the peak at 330 K is attributed to the structural phase transition, and the other peak at 436 K is associated with the thermal decomposition of the crystal. The structures in room‐ and high‐temperasture phases are determined, and the space group of the sample crystal is found to change from monoclinic P 2₁/c to orthorhombic Pnma. The structure of the room‐temperature phase consists of two different types of N‐H···O hydrogen bond, but in the high‐temperature phase there is no specific hydrogen bond between the NSO₃ pseudo‐tetrahera. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 3β-hydroxy-5β-estr-8(14)-en-17-one

The title compound crystallizes in the orthorhombic space group P2₁2₁2₁ with 4 formula units C₁₈H₂₆O₂ in the unit cell. The lattice constants are a = 10.356(2) Å, b = 19.743(3) Å, and c = 7.487(1) Å. The structure was solved by direct methods of phases determination and refined by least-squares calculations to the conventional R = 0.054. The configuration and conformation of the molecule were determined and compared with those of Δ-8,14-anhydrodigitoxigenin.     

Crystal and molecular structure of 6,7-benzo-3,4 (1,4-dimethoxy-2,3-naphtho)-1,5-dioxosuberane

The crystal and molecular structure of the title compound (2) C₂₁H₁₆O₄ has been determined by an X-ray analysis, by direct methods from diffractometer data and refined by full-matrix least squares. The compound (2) crystallizes in the space group P2₁/a, with cell parameters:a=36.432(5),b=5.512(3),c=8.269(5) Å, =108.0(3)°,z=4,D _c =1.397 g/cm^–3,R=7.8 for 1136 observed reflections. The conformation of the tetracyclic ring system shows a folding of two planar parts of the carbon skeleton about an axis passing thorough C8 and C16 of the seven membered ring C.     

Synthesis and crystal structure of 5-amino-4-cyano-1-[(5-methyl-1-t-butyl-4-pyrazolyl)carbonyl]-3-methylthio-1H-pyrazole

The title compound, 5-amino-4-cyano-1-[(5-methyl-1-t-butyl-4-pyrazolyl)carbonyl]-3-methylthio-1H-pyrazole 5, was synthesized by the treatment of 4 (5-methyl-1-t-butylpyrazole-4-carbohydrazide) with 2-cyano-3, 3-dimethylthio-acrylonitrile, and its crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic, space group P2₁/c with unit cell parameters a = 13.566(4) Å, b = 10.833(3) Å, c = 11.202(3) Å, α = 90°, β = 98.073(5)°, γ = 90°, V = 1629.9(8) ų, Z = 4, D _c = 1.298, M _r = 318.40, μ = 0.210 mm⁻¹, F(000) = 672, R ₁ = 0.0488 and wR ₂ = 0.1250.     

Crystal structure of [Cu2(II)(dmpa)2(p-Cl-C6H5COO)2] (Hdmpa = N,N-dimethyl-3-amino-1-propanol)

The copper complex, [Cu₂(II)(dmpa)₂(p-Cl-C₆H₅COO)₂], has been prepared and its structure determined using X-ray crystallography. The dimer is a di-₂-alkoxo complex which is a five-coordinate copper dimer with unsupported alkoxo bridges. The complex crystallizes in the triclinic space group P-1 with a = 11.384(2), b = 14.636(5), c = 9.609(2) Å, = 100.07(2), = 104.33(3), = 72.79(2)°, V = 1471.8(7) ų, and Z = 2. The structure is comprised of discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the dmpa^– ligands. The Cu-O and Cu-N distances are in good agreement with those found for other copper(II) aminoalcoholato complexes. The Cu···Cu distance is 2.9765(6) Å. In the crystal, every two dimeric coordination molecules are combined together by the recognition through intermolecular hydrogen-bonding interactions between the apical water molecule and the non-coordinated O atom from the p-chlorobenzoato ligand, forminga tetramer.