Structures of Azomethine Imines of the Pyrazolidone-(3)-type, (III) The Structure of 1-[Anthryl-(9)-methylene]-pyrazolidone-(3)-betaine

C₁₈H₁₄N₂O, Pbca, a = 19.541(4) Å, b = 14.800(2) Å, c = 9.572(3) Å, Z = 8, U = 2768.3 ų, D_x = 1.32 g cm⁻³, μ(MoKα) = 0.93 cm⁻⁻¹, crystal size 0.5 × 0.2 × 0.1 mm, colourless. Final R = 0.077 for 1177 independent reflections excluded those with |F₀| < 8 σ(F₀). The intensities were measured with an automatic diffractometer. The azomethine imine unit of the molecule has a geometry in approximate agreement with a polymethinic electron structure. The conjugation of the azomethine imine unit with the anthryl unit is only small. The anthryl ring and the five membered pyrazolidone ring include a dihedral angle of 65.4°. The main intermolecular forces are C–H … N hydrogen bridges.     

Structures of azomethine imines of the pyrazolid-3-one-type (V). The structure of 1-[pyrenyl-(1)-methylene]-5,5-dimethyl-pyrazolid-3-one-betaine.

C₂₂H₁₈N₂O, P2₁, a = 7.473(2), b = 13.563(3), c = 18.264(3) Å, β = 115.49(4)°, Z = 4, U = 1670.9(6) ų, D_x = 1.295 Mg m⁻³, μ(MoKα) = 0.855 cm⁻¹, crystal size: 0.3 × 0.2 × 0.2 mm, colour: yellow. Final R = 0.086 for 1973 independent reflections excluding those with |F₀ < 3σ(F₀). The intensities were measured with an automatic diffractometer. There are two symmetrically independent molecules in the unit cell. The azomethine imine parts of the molecules are similar to those of four other relevant structures determined by X-ray analysis. A polymethinic part of a molecule is linked with an aromatic part via the bond C(4)–C(5). The mean pyrenyl plains and the mean plains of the five membered rings include dihedral angles of 29.6° for molecule A and 23.7° for molecule B.     

The molecular and crystal structure of 2-oxo-1-pyrrolidine-acetamide

C₆H₁₀N₂O₂, P1 , a = 6,607(2) Å, b = 8,538(2) Å, c = 6,392(2) Å, α = 102,43(2)°, β = 91,11(2)°, y = 79,82(2)°, V = 349,1 ų, Z = 2, D_m = 1,36 g × cm⁻³, D_x = 1,35 g × × cm⁻³, MoKα radiation, λ = 1.71069 Å, μ(MoKα) = 1.11 cm⁻¹. The structure was solved by direct methods. The parameters were refined by full matrix least squares technique to a final R = 0.088 for 834 reflections with ∥F₀∥ > 4σ(F₀). The dihedral angle between the least-squares plane through the pyrrolidine ring and that through the acetamide group is 90.4°. The N H … O hydrogen bonds connect molecules to form bands parallel to the z axis.     

Crystal and molecular structure of 2-diazo-5-phenyl-cyclohexan-1,3-dione

M_r = 214.24, monoclinic space group P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ (MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.034. M_r = 214.24, monokline Raumgruppe P 2₁, a = 10.964(2), b = 5.870(2), c = 8.574(2) Å, β = 98.09(2)°, V = 546(1) ų, Z = 2, D_x = 1.302 Mg m⁻³, F(000) = 224, λ(MoKα) = 0.71069 Å, μ = 0.8 mm⁻¹.     

Structure of monoclinic acridine orange hydrochloride monohydrate,C17H19N3 · HCl · H2O

M_r = 319.82, monoclinic P2₁/a, Z = 4, a = 14.545(5), b = 15.562(6), c = 8.538(4) Å, β = 120.66(3)°, V = 1662(1) ų, D_m = 1.27 Mgm⁻³, D_x = 1.278 Mgm⁻³, λ(MoKα) = 0.71069 Å, μ(MoKα) = 0.24 mm⁻¹, T = 297 K. Final R = 0.049 for 1485 observed reflections. All hydrogen atoms were located and refined isotropically. Bond lengths (σ = 0.004 Å) and angles (σ = 0.3°) are normal. The substance is a derivative of acridine. The structure consists of chloride anions, bisdimethylaminoacridinium cations and water molecules. In the solid state the molecules are approximately planar. Pairs of cations form dimers with parallel planes connected by an I inversion centre and plane distances of 3.474 Å. They overlap with partial areas of all three six membered rings.     

Crystal and molecular structure of 1-diazo-2,3,4,5-tetraphenylcyclopentadiene

M_r = 396.30, monoclinic space group P 2₁/c, a = 10.145(2), b = 18.523(4), c = 12.443(2) Å, β = 110.31(2)°, V = 2193(1) ų, Z = 4, D_x = 1.201 Mg m⁻³, F(000) = 832, λ(MoKα) = 0.71069 Å, μ = 0.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039.     

Crystal structure of 4,5-dihydro-6-(2-thienyl)-3(2H) pyridazinone azine, (C16H16N16S2)

M_r = 484, monoclinic, P 2₁/c, a = 5.567(1), b = 7.857(2), c = 19.194(10) Å, β = 99.97(3)°, V = 826.9 ų, Z′ = 2, D_x = 1.43 g · cm⁻³, F(000) = 372, MoKα, λ = 0.71069 Å, μ = 0.328 mm⁻¹, final R = 0.055 for 889 observed reflections, T = 293 K. The compound was prepared from a direct unusual reaction of 6-(2-thienyl)-2,3,4,5-tetrahydropyridazine-3-one with hydrazine hydrate. The structure was solved by direct methods and refined by full-matrix least squares. The molecule in the solid state consists of a dimer with its two equivalent halves related by a center of symmetry at the middle of the N N bond. Each molecular fragment is nearly planar and the N N bond between the two halves is 1.296(5) Å indicating that it is a partial double bond.     

Crystal and molecular structures of N-alkyl-N,N-dimethyl-3-(heptamethyltrisiloxan-3-yl) propylammonium bromides

C₁₆H₄₂NO₂Si₃Br: M_r = 444.76, monoclinic space group P 2₁/c, a = 23.300(8), b = 8.918(4), c = 13.403(2) Å, β = 101.69(4)°, V = 2727(1) ų, D_x = 1.08 Mgm⁻³, D_exp = 1.06 Mgm⁻³, Z = 4, F(000) = 932, λ(MoKα) = 0.71069 Å, μ = 16.3 cm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.117. C₁₅H₄₀NO₂ Si₃Br: M_r = 430.34, monoclinic space group P2₁/c, a = 23.460(4), b = 8.518(2), c = 13.403(2) Å, β = 102.03(2)°, V = 2619(1) ų, D_x = 1.09 Mgm⁻³, D_exp = 1.07 Mg⁻³, Z = 4, F (000) = 920, λ(MoKα) = 0.71069 Å, μ = 33.9 cm⁻¹. The crystal structure was determined by least-squares refinement of the structure model derived from structure determination of C₁₆H₄₂NO₂·Si₃Br to the discrepancy factor R = 0.099. C₁₆H₄₂NO₂Si₃Br: Daten siehe oben. C₁₅H₄₀NO₂Si₃Br: Daten siehe oben.     

Crystal and molecular structure of 5-diazo-2,2-dimethyl-4,6-dioxo-1,3-dioxane and 5-diazo-1,3-dimethylpyrimidin-2,4,6-trione

C₆N₂O₄H₆: M_r = 170.12, orthorhombic space group Pbca, a = 6.751(2), b = 13.669(4), c = = 16.845(4) Å, V = 1555(1) ų, D_x = 1.248 Mgm⁻³, Z = 8, F(000) = 704, λ(moKα) = 0.71069 Å, μ = 1.1 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.039. C₆N₄O₃H₆: M_r = 182.14, monoclinic space group C2/c, a = 17.726(8), b = 6.191(12), c = 16.062(6) Å, β = 117.59 (3)°, V = 1562 (1) ų, D_x = 1.549 Mgm⁻³, Z = 8, F(000) = 752, λ(MoKα) = 0.71069 Å, μ = 1.2 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.056.     

Crystal and Molecular Structure of mer-Co(4-CH3C5H4N)3(N3)3

The crystal structure of mer-Co(4-CH₃C₅H₄N)₃(N₃)₃has been determined by single crystal X-ray methods at 300 K. The compound crystallizes in the monoclinic space group C 2/c, a = 19.087(6), b = 16.769(4), c = 15.845(4) Å, β = 119.04(2)°, V = 4434(2) ų, M_r = 464.42. Z = 8, D_x = 1.391 Mgm⁻³, F(000) = 1920, λ (MoKα) = 0.71069 Å, μ = 0.802 mm⁻¹. The cobalt(III) ions are octahedrally coordinated to three azide groups and to three 4-methyl-pyridine molecules to form isolated coordination polyhedra.     

Crystal and molecular structure of 1-(p-nitrophenyl)-2-acetylamino-3-brom-propen-2-on-1, C11H9BrN2O4

M_r = 313.11, orthorhombic space group Pbca, a = 8.165(1), b = 9.491(2), c = 32.207(5) Å V = 2496(1) ų, D_X = 1.667 Mgm⁻³, Z = 8, F(000) = 1248, λ(MoKα) = 0.71069 Å, μ = 32.7 mm⁻¹. The crystal structure was determined by direct methods and refined by least-squares procedure to the discrepancy factor R = 0.065. Positions of hydrogen atoms were calculated. The structure determined by x-ray analysis confirms the chemical results.     

Crystal Structure Investigation of 2-Pheny limidazo [f]1,10-phenanthroline

The crystal structure of the title compound (PIP) has been determined by single crystal X-ray diffraction methods. C₁₉H₁₂N₄. C₂H₅OH crystallizes in the monoclinic space group P2₁/n with a = 11.4414(8), b = 12.6052(9), c = 12.4627(8) Å, β = 100.345(2)°, Z = 4, V = 1768.17 ų, D_cal = 1.286 Mg. m⁻³, μ (MoKα) = 0.80 cm^-1, F(000) = 720. The structure was solved by the direct methods and refined by full-matrix least-squares method to a final R = 0.0337 and R_w = 0.0332 for 2306 reflections with F₀ > 4σ(F₀). The phenl ring and the imidazo[f]1,10-phenanthroline moiety are coplanar in the crystal. The packing of the molecules involves hydrogen bonded association of the hydroxyl group of ethanol both with the N H of the imidazole moiety of one PIP and one nitrogen atom of the phenanthroline moiety of another PIP.     

Crystal structure determination of bis-dimethyl heptamethine cyanine chloride,C11N2H19Cl · 4 H2O

Mr = 286.59, monoclinic superposition structure C 121, Z = 4, a = 15.248(3), b = = 6.942 (3), c = 9.074(1) Å, β = 120.1(1)°, V = 827(1) ų, D_m = 1.13(1) Mg m⁻³, D_x = = 1.15 Mg m⁻³, λ(MoK_α) = 0.71069 Å, μ = 0.243 mm⁻¹, F (000) = 312, T = 296 K, final R = 0.061 for 802 reflections. All hydrogen atoms were located. The structure consists of chloride anions, bis-dimethyl heptamethine cyanine cations and water molecules. The structure of bis-dimethyl heptamethine cyanine chloride is disordered, e.g. there exist partial coincidence operations, leading to more than one stacking mode of the bis-dimethyl heptamethin cyanine chains. The crystal structure consists of rows of molecule along the a-axis. The C C bonds show the bond length compensation, typical of polymethines, towards a partial double bond (mean value 1.38 Å) between formally sp²-hybridized C atoms. The C N bond lengths to the methyl carbon atoms (mean value 1.49 Å) correspond to normal C N single bonds. The valence angles at the C atoms of the heptamethine chain clearly alternate and deviate systematically from 120°. This is also observed in other structures of a similar type. The structure determined by X-ray analysis confirms the chemical results.     

The crystal structure of dodecyltrimethylammoniumbromide

C₁₅H₃₄BrN, monoclinic, P 2₁/m, a = 21.603(9), b = 7.261(3), c = 5.636(2) Å, β = 86.85(2)°, Z = 2, V = 882.72 ų, D_x = 1.160 g/cm³, μ(MoKα) = 2.45 cm⁻¹, λ(MoKα) = 0.71069 Å. The structure of this cationic surfactant was solved with Patterson methods and refined to R = 0.091 for 2057 measured reflections. The dodecyl chains are slightly screwed around their chain axes. The hydrocarbon chains are statistically disordered. The polar regions satisfy the mirror plane which is by remaining parts only statistically fulfilled. In the process of structure refinement statistical disorder has been included by separation of some atom positions. The sublattice of the hydrocarbon chains is nearly O⟂ with a_s = 5.14, b_s = 7.26, c_s = 2.52 Å.     

Structure of the OD-disordered 2-Hydroxy-4-methoxy-2H-1,4-benzoxazin-3-one,C9H9NO4

The X-ray diagrams of the title compound show pronounced maxima on diffuse streaks parallel c* and unusual extinctions. The intensity distribution is compatible with the assumption of a disordered (OD) structure consisting of one kind of layers. The structure contains ordered domains with the crystal data: monoelinic, space group P 2₁/a, lattice parameters a = 15.910(5), b = 8.365(4), c = 15.747(5) Å, β = 120.34(6)°, V = 1809 ų, Z = 8, M_r = 195.1, D_x = 1.432 Mg m⁻³, μ(MoKα) = 0.36 mm⁻¹, final R = 0.129 for 859 observed reflections. The asymmetric unit is constituted of two crystallographically independent molecules related by a pseudo glide plane. The crystal used for X-ray analysis proved to be twinned.     

Crystal structure determination of 2-acetylamino-4-benzoyl-5,5-dimethyl-4,5-dihydro-1,3,4-thiadiazolin,C13H15N3O2S

Thiosemicarbazone is receiving increasing interest because of the biological activity of some of its derivatives. Mr = 277.35, space group P2₁2₁2₁, Z = 4, a = 9.290(3), b = = 11.512(2), c = 13.286(2) Å, V = 1421 (1) ų, D_m = 1.29(1) Mg m⁻³, D_x = 1.296 Mg m⁻³, λ(MoK_α) = 0.71062 Å, μ = 0.230 mm⁻¹, F(000) = 584, T = 296 K, final R = 0.028 for 1255 reflections. All hydrogen atoms were located. The structure determed by X-ray analysis confirms the chemical results. The structure analysis of the title compound is described and its molecular and crystal structure discussed.     

Crystal and Molecular Structure of Tosyl Pyrrolidine-2-Methanol (C12H17SO3N)

C₁₂H₁₇SO₃N, M_r = 255.33, Orthorhombic, P2₁2₁2₁, a = 11.703(1) Å, b = 14.797(3) Å, c = 14.971(2) Å, V = 2592.52 ų, Z = 8, D_m = 1.309 Mgm⁻³, D_c = 1.308 Mgm⁻³, mμ = 21.57 cm⁻¹, F(000) = 1088, T = 290 K, final R = 0.080 for 2416 unique reflections. There are two crystallographically independent molecules in the unit cell of the title compound.     

The Crystal and Molecular Structure of 2-(2′-Cyano-2′-amido-ethylenyl)-pyridine

The title compound (C₉H₇N₃O) has been determined from three dimensional X-ray diffraction data. The crystals are monoclinic, a = 4.858(3) Å, b = 15.008(7) Å, c = 11.787(2) Å, ß = 94.107(2)°, V= 857.2(4) ų, z = 4, D_calc = 1.342 g. cm⁻³, space group P2_1/c. The structure was solved by direct methods and refined by full-matrix least-squares method (γ MoK_α′, R = 0.0766).     

Crystal Structure of a Complex of Sarcosine with Barium Chloride

Single crystals of sarcosine barium chloride tetrahydrate were crystallised from a saturated aqueous solution containing stoichiometric amounts of sarcosine and barium chloride, in 2: 1 proportion. The intensity data were collected using a CAD-4 diffractometer with graphite monochromated MoKα radiation. The crystal data are as follows: a = 7.235(1) Å, b = 10.668(4) Å, c = 15.686(3) Å, V = 1210.7 ų, F.W. = 369.33, d_expt, = 2.02 g · cm⁻³, d_calc = 2.026 g · cm⁻³, Z = 4 and the space group is P2₁2₁2₁. The structure has been solved to an R value of 0.02 for all the 1239 reflections with I > 2σ(I). The sarcosine molecule exists as zwitterion in the structure. The barium ion is found to have 10-fold coordination with nine oxygens and a chlorine taking part in coordination. All the water oxygens and chlorines take part in hydrogen bonds except carboxyl oxygens.     

Structural studies of low-valent metal-fluorocarbon complexes II. Crystal and molecular structure of bis(triethylphosphine)-(hexakis(trifluoromethyl)benzene)-platinum

The crystal structure of bis(tiethylphosphine)(hexakis(trifluoromethyl)benzene) platimum, C₂₄H₃₀F₁₈P₂Pt, has been determined. The crystals are monoclinic: space groupP2₁/n,a = 9.937(6),b = 30.89(1),c= 11.398(8) Å, β = 117.15(3) ° andZ = 4. X-ray data were collected by counter methods using MoKα radiation, and least-squares refinement led toR = 0.057 for the 2154 independent reflexions for which ¦F ₀¦²> 3σ(¦F ₀¦²). The molecule has a 1,2-hapto structure, with the platinum atom bonded to only two carbon atoms of the hexakis(trifluoromethyl)benzene ring. The planarity of this ring is destroyed as a result of the coordination and there is an alternation of long and short bonds around the ring. The mean Pt—C bond length is 2.14(2) Å.