Structures of Azomethine Imines of the Pyrazolidone-(3)-type (I). The Structure of 1-(4-Nitrobenzylidene-pyrazolidone-(3)-betaine

1-(4-Nitrobenzylidene)-pyrazolidone-(3)-betaine crystallizes in the orthorhombic space group Pbca with eight molecules per unit cell. The lattice parameters are a = 11.025 Å; b = 22.995 Å; c = 7. 677 Å. With X-ray diffraction data, collected on a automatical four circle diffractometer, the crystal structure was solved by direct methods and refined to an R-value of 0.047 for 1516 symmetrically independent reflections. The structure determination has been performed to contribute to the explanation of the photochromic behaviour of this special class of azomethine imines.     

α-substituted phosphoryl compounds (III). The crystal and molecular structure of diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide,C19H15OPS2

Diphenyl[1,3-benzodithiolyl-(2)]-phosphinoxide crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell. The lattice parameters are a = 9.600 Å, b = 11.270 Å, c = 16.484 Å; β = 99.72°. With X-ray diffraction data collected at an automatic four circle diffractometer, the crystal structure has been solved by direct methods and refined to an R-value of 0.08 for 2690 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

α-substituted Phosphoryl Compounds (I). The Crystal and Molecular Structure of Diethyl[5,6-dichloro-1,3-benzodioxol-(2)]-phosphonate,C11H13O5PCl2

Diethyl[5,6-dichloro- 1,3-benzodioxol-(2)]-phosphonate crystallizes in the triclinic space group P l̄ with two molecules per unit cell. The lattice parameters are a = 11.716 Å, b = 8.471 Å, c = 7.644 Å; α = 82.47° β = 95.81°, γ = 95.89°. With X-ray diffraction data collected on an automatic four circle diffractometer, the crystal structure was solved by direct methods and refined by least squares methods to an R value of 0.12 for 2374 measured reflections. The crystal used was im perfect. The substance is a derivative of acetales of formyl phosphoneacid esters. The aim is to find a correlation between the geometry of the structure and NMR data.     

The Crystal Structure of 3-Methoxy-estra-1,3,5(10)-triene-16α Br,17β OH

The steroid 3-Methoxy-estra-1,3,5(10)-triene-16αBr,17βOH crystallizes in the tetragonal space group P 4₁ with the lattice constants a = b = 10,358(2) Å, c = 32,591(5) Å. The crystal structure contains two symmetry independent molecules. Significant differences for the two molecules occur in all the four rings of the steroid sceleton. The molecules are linked by hydrogen bridges and Br…︁ Br contacts. The differences between the two symmetry independent molecules are interpreted as due to different intermolecular interaction.     

Studies on the Structure of alpha-Quinacridone

Alpha-quinacridone crystallizes in the triclinic space group P1 with Z = 2, a = 14.934 ± 0.064 Å, b = 3.622 ± 0.004 Å, c = 12.935 ± 0.040 Å; α = 91.39 ± 0.28°, β = 107.13 ± 0.02°, γ = 92.84 ± 0.24°. The molecules are connected by hydrogen bonds more far from linearity (≈145°) than gamma-quinacridone 162°). Together with π-π bonds, building molecular stacks along the short axis b = 3.622 Å, both types of bonds run through the whole lattice. Molecules within the hydrophobic planes exhibit orientational disorder. Transitions between gamma- and alpha-quinacridone has been discussed: all inversion centers are retained, only the vectors of bravais lattice and the angles of molecules in the stacks are changed. The calculated pattern of alpha-quinacridone is compared with the experimental one by means of overlay- and difference plots. – The transition character of the alpha-quinacridone is stressed by generation of a combined pattern of 50% alpha- and 50% gamma-quinacridone, calculating an experimental alpha-quinacridone.     

α-substitued phosphoryl compounds (IV). The crystal and molecular structure of diethyl[bis-(p-chlorophenoxy)-methan]-phosphonate,C17H19O5PCl2

Diethyl-[bis-(p-chlorophenoxy)-methan]-phosphonate crystallizes in the triclinic space group P 1 with two molecules per unit cell. The lattice parameters are a = 8.757 Å, b = 10.479 Å, c = 12.878 Å, α = 82.21°, β = 116.27°, γ = 113.80°. With X-ray diffraction data, collected on an automatic four circle diffractometer, the crystal structure was solved by direct methods and refined to an R-value of 0.049 for 3116 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl phosphonic acid esters. Correlations between the geometry of the structure and NMR-data are of interest.     

α-substituted Phosphoryl Compounds (II). The Crystal and Molecular Structure of Diphenyl-[5,6-dichloro-1, 3-benzodioxol-(2)]-phosphine-oxide,C19H13O3PCl2

The compound crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell, and with the lattice parameters a = 11.807 Å, b = 13.070 Å, c = 11.312 Å, β = 96.74°. With X-ray diffraction data collected on a four circle diffractometer, the crystal structure has been determined by direct methods and refined to an R-value of 0.061 for 2735 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

Die Molekül- und Kristallstruktur des N-Methyl-piperidinium-acet-para-brom-anilid-jodid

N-Methyl-piperidinium-acet-para-bromo-anilide-iodide crystallizes in the triclinic space group P 1 with two formula units C₁₄H₂₀N₂OBrJ and two H₂O molecules in the unit cell. The lattice constants are a = 8.950 Å, b = 14.721 Å, c = 7.440 Å, α = 80.19°, β = 112.57° and γ = 106.82°. The molecular structure of the compound was determined by the X-ray structure analysis and the interaction between the molecules in the crystal was investigated. Especially the influence of the water in the crystal on the form of the molecule was analysed.     

Die Änderung der Molekül- und Kristallstruktur des N-Methyl-piperidinum-acet-meta-chlor-anilid-jodid durch Einlagerung von Wasser

N-Methyl-piperidinium-acet-meta-chloro-anilide-iodide crystallizes from water in the space group Pna2₁ with 4 formula units C₁₄H₂₀N₂OClJ and 4 H₂O molecules in the unit cell. The lattice constants are a = 12.413 Å, b = 19.798 Å and c = 6.919 Å. The change of the molecular conformation caused by water molecules was investigated by X-ray structure analysis.     

The Molecular and Crystal Structure of 1Ref, 3trans-bis (4-chlorophenyl)-2cis-nitro-5-oxo-perhydropyrazolo [1,2-a]pyrazol

The structure of the title compound has been determined by means of an X-ray analysis. This product has been obtained by a 1,3-dipolar cycloaddition according to the concerted [π⁴S⁺π²S]-mechanism. The substance crystallizes in the monoclinic space group C 2/c with 8 molecules in the unit cell of dimensions a = 23.587; b = 11.789; c = 12.932 Å; β = 95.47°. The molecular structure determined by X-ray analysis agrees with the results of the chemical investigations. The final R-value is 0.081.     

X-Ray Diffraction Studies on Molecular Semiconductors Based on Charge-Transfer Complexes of Substituted Phenothiazines with 2,3-Dichloro-5,6-dicyano-p-benzoquinone

X-ray powder diffraction data on the molecular semiconductors based on the 1:1 charge-transfer complexes of the electron donors, viz. phenothiazine (PTZ), 2-chlorophenothiazine (CPZ), 2-acetyl phenothiazine (APZ) and 2-(trifluoromethyl)-phenothiazine (TPZ) with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) have been reported in this paper. The indexing has been done by Ito's method. All the complexes have been found to have orthorhombic crystal structures. The lattice parameters for the individual complexes are as follows: (i) PTZ-DDQ: a = 6.020 Å, b = 9.775 Å, c = 24.280 Å; (ii) CPZ-DDQ: a = 5.830 Å, b = 8.070 Å, c = 20.280 Å; (iii) APZ-DDQ: a = 5.055 Å, b = 7.955 Å, c = 19.520 Å; (iv) TPZ-DDQ: a = 5.130 Å, b = 8.195 Å, c = 19.850 Å.     

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.     

Crystal and Molecular Structure of 1-Cyano, 4(Trans-1′, N-Pentyl-Cyclohexyl-4′-Carboxy)-Benzene,ECH-5

The crystals of ECH-5 belong to the triclinic system, the space group is P1 with two molecules in the unit cell. The lattice dimensions are a = 9.153(2), b = 16.848(3), c = 5.770(4) Å, α = 97.26(5), β = 93.68(4), γ = 93.07(2)°. The structure was solved by direct methods and was refined using block diagonal least squares method to a final value of R₀ = 0.083 for 1787 observed reflections. The cyclohexane ring is chair. Torsion angles calculations showed that the middle part of the molecule is bent. The molecules are packed in head to tail manner, and they are arranged nearly parallel to each other.     

Crystal and Molekular Structure of Piperidinium-acet-p-Cl-anilide-chloride

Piperidinium-acet-p-Cl-anilide-chloride crystallizes in the triclinic space group P 1 with 2 formula units C₁₃H₁₈ON₂Cl₂ in the unit cell. The lattice constants are a = 10.471 Å, b = 12.545 Å, c = 6.149 Å, α = 72.14°, β = 105.70° and γ = 105.21°. Bond lengths, bond angles and the conformational flexibility were determined by X-ray structure analysis. The crystal structure contains dimeres consisting of drug molecules connected by hydrogen bonds.     

Crystal and Molecular Structure of Piperidinium-acet-m-Cl-anilide-chloride

Piperidinium-acet-m-Cl-anilide-chloride crystallizes in the orthorhombic space group Pca2₁ with 4 formula units C₁₃H₁₈ON₂Cl₂ in the unit cell. The lattice parameters are a = 10.348 Å, b = 12.280 Å and c = 11.335 Å. The crystal structure was determined by the heavy atom method and refined by least-squares procedures to the conventional R = 0.045. Bond lengths, bond angles and the conformation of the drug molecule were determined. Cl⁻ ions are linked to the molecules by hydrogen bonds forming chains together with iones and molecules related by the a-glide plane.     

Thermal dehydration of the double salts K2Be(XO4)2·2H2O (X = S,Se)

The thermal dehydration of the title compounds was studied by TG, DTA and DSC methods and the enthalpies of dehydration were calculated (87.6 kJ mol^–1 and 167.5 kJ mol^–1 for the sulfate and selenate compound, respectively). The larger value of ΔH_deh of K₂Be(SeO₄)₂·2H₂O is due to the stronger hydrogen bonds formed in the selenate as compared to those formed in the respective sulfate owing to the stronger proton acceptor capabilities of the SeO₄^2– ions. The enthalpies of formation (ΔH_f⁰) of the dihydrates are also calculated from the DSC measurements (– 4467.4 kJ mol^–1 and – 3447.1 kJ mol^–1 for the sulfate and selenate compound, respectively). The anhydrous double salt, K₂Be(SO₄)₂, forms tetragonal crystals with lattice parameters: a = 7.232(2) Å; c = 14.168(2) Å; V = 741.0 ų, while the anhydrous salt, K₂Be(SeO₄)₂, forms monoclinic crystals with lattice parameters: a = 9.217(3) Å; b = 10.645(3) Å; c = 8.989(2) Å; β = 108.52(4)°; V = 836.2 ų. Vibrational spectra (infrared and Raman) of both the dihydrates and the anhydrous compounds are also presented and discussed. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structure of 6α-Methyl-3,20-Dioxo-5β-Pregnan-17α-yl Acetate

The title compound 6α-methyl-3.20-dioxo-5β-pregnan-17α-yl acetate crystallizes in the monoclinic space group P 2₁ with two molecules in the unit cell and the lattice parameters a = 10.889, b = 11.056, c = 9.8029 Å, β = 101.51° The crystal structure is isostructural with medroxyprogesterone acetate and refined by full matrix least squares calculations up to the discrepancy factor R = 0.051.     

Crystal and Molecular Structure of the Smectogen 1-[4-n-heptylbenzoyl]-2-[cyanoacetyl]-hydrazine

The compound 1-[4-n-heptylbenzoyl]-2-[cyanoacetyl]-hydrazine crystallizes in the triclinic space group Pl̄ with two molecules in the unit cell and the lattice parameters a = 4.702, b = 8.640, c = 20.906 Å, a = 97.50, β = 92.79, γ = 100.19°. The structure was solved by direct methods and refined by full-matrix least squares calculations to the final residual value R = 0.039.     

The Crystal and Molecular Structure of the Smectogenic Compound 5-Hexyl-2-(4-bromophenyl)-1,3-dioxane

The title compound with the formula C₆H₁₃ C₄O₂H₆ C₆H ₄Br (HBPD) crystallizes in the monoclinic space group C 2/c with lattice parameters a = 28.48 Å, b = 5.71 Å, c = 20.19 Å, β = 97.4° and molecules per unit cell. The structure has been solved by the heavy atom method and refined to a final R value of 0.094. – The HBPD molecules adopt a fully stretched form, both the alkyl and phenyl substituent are in equatorial position with respect to the chair-shaped dioxane ring. The orientation of the phenyl group is an intermediate between the perpendicular and parallel conformation. The molecules show a nearly perfect parallel arrangement in the crystal lattice.     

Crystal and molecular structure of 17α,21-dihydroxy-1,4-pregnadiene-3,20-dione

The title compound 17α,21-dihydroxy-1,4-pregnadiene-3,20-dione crystallizes in the orthorhombic space group P 2₁2₁2₁ with four molecules in the unit cell and the lattice parameters a = 7.727, b = 10.095, c = 22.876 Å. The crystal structure was determined by direct methods and refined by full matrix least squares calculations up to the discrepancy factor R = 0.048.