Crystal and Molecular Structures of Modified Progestagens(III). 17α-Chloromethyl-17α-hydroxy-estr-4-en-3-one,C19H27CIO2

The crystal and molecular structure of the title compound has been determined by X-ray structure analysis. It crystallizes in the monoclinic space group P 2₁ with cell parameters a = 11.471(1), b = 17.261(3), c = 8.680(2) A, and β = 92.39(1) A. The structure was solved by MULTAN-82 and refined to R = 0.067 for all 4064 reflections. There are two molecules, A and B, in the asymmetric unit with different A ring conformations. Intermolecular hydrogen bridges link the molecules into dimers.     

Crystal and Molecular Structures of Modified Progestagens (I). 17α-Cyanomethyl-17β-hydroxy-estr-4-en-3-one,C20H27NO2

17α-Cyanomethyl-17β-hydroxy-estr-4-en-3-one is the first member in a series of progestagens investigated systematically by X-ray structure analyses. It crystallizes in the orthorhombic space group P 2₁2₁2₁ with cell parameters α = 8.887(6), b = 11.814(7), and c = 16.263(2) A. The structure was solved by MULTAN-82 and refined to R = 0.045 for 1453 observed reflections. The steroid ring A has an 1β-sofa conformation, the rings B and C adopt chair forms, ring D is intermediate between 13β,14α-half chair and 13β-envelope. All rings are trans-fused. In the present structure, O H… N hydrogen bonds link the molecules into chains parallel to α.     

Crystal structure of 17α‐acetoxyprogesterone,C23H32O4

The crystal structure of the title compound (C₂₃H₃₂O₄) has been determined by X‐ray diffraction methods. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters: a = 10.86(1), b = 11.95(2), c = 15.65(5) Å and Z = 4. The structure has been refined to an R‐value of 0.045 for 1610 observed reflections. Ring A exists in sofa conformation, Ring B adopts a distorted chair conformation while as Ring C assumes a chair conformation. The five membered ring D adopts a half‐chair conformation. The crystal structure is stabilized by intra‐ and intermolecular C‐H…O interactions. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 3-methoxy-estra-1,3,5(10)-triene-14β,17β-diol,C19H26O3

The crystal and molecular structure of 3-methoxy-estra-1,3,5(10)-triene-14β,17β-diol has been determined by single crystal X-ray analysis. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters a = 8.965(2), b = 30.520(7), and c = 6.031(2) A. The structure was solved by the POSIT system and refined by least-squares calculations to the conventional R factor of 0.075. The steroid rings A, B, and C have planar, 7α, 8β-half chair, and chair conformations, respectively. The ring D is intermediate between 13α, 14β-half chair and 13α-envelope. Rings B and C are trans-fused, and rings C and D are cis-fused. There are intra- as well as intermolecular hydrogen bonds between both hydroxyl groups of the steroid molecule.     

Crystal and molecular structure of 1,21-diacetoxy-11β,17-dihydroxy-4-methyl-19-norpregna-1,3,5(10),8(14)-tetraen-20-one,C25H30O7

The structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the monoclinic space group P 2₁ with 2 formula units C₂₅H₃₀O₇ in the unit cell. The lattice constants are a = 10.194, b = 11.790, c = 9.515 Å, and β = 100.69°. The structure was solved by direct methods using MULTAN-78 and refined by least-squares calculations to R = 0.061. The molecular configuration and conformation are discussed. The influence of the acetoxy groups and the 11-hydroxyl group on the steroid backbone is of special interest. There are two symmetry independent intermolecular but no intramolecular hydrogen bridges.     

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.     

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 structure of phenyl-β-methyl-pyridyl hydroxyimide,C13H12N2O

Phenyl-β-methyl-pyridyl hydroxyimide crystallizes in the form of prismatic crystals in the space group P 2₁ with Z = 4, a = 11.401(4) Å, b = 7.793(3) Å, c = 12.766(4) Å and β = 92.97°. The structure was solved by direct methods and was refined by block diagonal least squares calculation to a final value of 0.05. The pyridyl ring in molecule (II) is slightly distorted, all the other rings as expected are planar.     

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 1-o-nitrophenyl-3-methyl-5-tert-butylpyrazole,C14H17N3O2

Journal of Chemical Crystallography - Crystals of 1-o-nitrophenyl-3-methyl-5-tert-butylpyrazole, C14H17N3O2, are orthorhombic:a=12.0924(6),b=11.3601(7),c=10.2317(4) Å,Z=4, space groupP212221....     

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 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.     

Chemistry of organic eutectics (IV). α-Naphthol-β-naphthol eutectic system

The detailed methods of investigating the phase diagram, supercooling, crystallization velocity, microstructure, and diffusion coefficient for the α-naphthol-β-naphthol eutectic system have been discussed. The results are discussed in the light of existing theories describing morphology, nucleation, crystallization kinetics, and diffusion phenomena.     

The crystal and molecular structure of 5α,8α-epidioxyergosta-6,22-dien-3β-acetate

From the mushroom species Tricholoma populinum LANGE which shows interesting pharmaceutical effects the steroid 5α,8α-epidioxyergosta-6,22-dien-3β-ol has been isolated. The acetate of this compound crystallizes in the monoclinic space group P 2₁ with two molecules in the unit cell of dimensions a = 19.788, b = 7.241, c = 9.914 Å, β = 103,97°. The final R-value is 0.079 for 1082 reflections.     

The Crystal and Molecular Structure of 1α,2α-Methylene Gibberellin A3 Methyl Ester

The three-dimensional structure of the 1α,2α-methylene gibberellin A₃ methyl ester has been determined by single-crystal X-ray diffraction techniques. The crystals are monoclinic, space group P 2₁ with two molecules in the unit cell of dimensions a = 9.236, b = 7.109, c = 14.155 Å and β = 104.61º. The structure was refined to an R-value of 0.0983 for 1359 observed reflections.     

Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

The Crystal Structure of 3-Methoxy-estra-1,3,5(10)triene-16αBr,17αOH

The steroid 3-Methoxy-estra-1,3,5(10)triene-16αBr,17αOH crystallizes in the orthorhombic space group P 2₁2₁2₁ with lattice constants a = 30.653(5) Å, b = 9.039(2) Å, c = 6.098(1) Å. The single molecule has an intramolecular O H…︁ Br interaction. Intermolecular interactions are only of van der Waals type. Ring A is nearly planar, ring B has a nearly half chair conformation, ring C has a chair conformation and ring D an envelope conformation.