Crystal and Molecular Structures of Modified Progestagens (IV). 17α-Azidomethyl-17β-hydroxy-estra-4,9-dien-3-one,C19H25N3O2

The crystal and molecular structure of 17α-azidomethyl-17β-hydroxy-estra-4,9-dien-3-one has been determined by X-ray structure analysis. It crystallizes in the orthorhombie space group P 2₁2₁2₁ with cell parameters a = 9.118(1), b = 9.252(1), and c = 20.444(2) Å. The structure was solved by MULTAN-82 and refined to R = 0.042 for 1408 observed reflections. Steroid ring and 17β-side chain conformations are discussed in the paper. Intermolecular hydrogen bridges between hydroxyl groups and carbonyl oxygen atoms link molecules forming chains in c-direction.     

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 (20R)-19-nor-5β,14β-pregnane-3β,14,20-triol 3,20-diacetate

The title compound (20R)-19-nor-5β,14β-pregnane-3β,14,20-triol 3,20-diacetate crystallizes in the monoclinic space group P2₁ with 4 formula units C₂₄H₃₈O₅ in the unit cell. The lattice parameters are a = 14.324, b = 12.569, c = 12.685 Å, β = 90.21°. The crystal structure was determined by direct methods and refined by the least-squares procedure to the discrepancy factor R = 0.042. Bond length, bond angles, ring conformations, as well as the absolute configuration at C20 were determined. In the crystal the molecules are linked to infinite chains by two hydrogen bonds.     

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 structure of (21R)-3β-acetoxy-14,21-epoxy-5β,14β-card-20(22)-enolide

The title compound (21R)-3β-acetoxy-14,21-epoxy-5β,14β-card-20(22)-enolide crystallizes in the monoclinic space group P2₁ with 2 formular units C₂₅H₃₄O₅ in the unit cell. The lattice parameters are a = 13.471, b = 7.959, c = 10.514 Å and β = 102.73°. The crystal structure was determined by direct methods and refined by least-squares procedures to the discrepancy factor R = 0.045. Bond length, bond angles, ring conformations and the configuration at C(21) were determined. Intermolecular interactions are only of van der Waals type.     

The Molecular and Crystal Structure of 3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin

3β-O-(2′,3′ -O-isoropylidene-α-L-rhamnopyranosyl) — digitoxigenin crystallizes in the monoclinic space group P 2₁ with two molecules C₃₂H₄₈O₈ per unit cell and the lattice constants a = 7.865, b = 6.470, c = 29.803 Å, β = 93.95°. The structure was solved by direct methods of phases determination and subsequently refined by least squares technique to the final R-value 0.06. The position of the lactone ring is disordered in the crystal.     

Crystallographic Investigations of 3β‐acetoxy‐5α‐cholestan‐6‐one‐semicarbazone ‐ A Steroid

The crystal structure of 3b‐acetoxy‐5a‐cholestan‐6‐one‐semicarbazone (C₃₀H₅₁O₃N₃) has been determined by X‐ray diffraction methods. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters a = 11.641(1), b = 16.552(1) c = 31.181(4) Å and Z = 8. The structure has been refined to an R‐value of 0.050 for 4407 observed reflections. Two molecules in the asymmetric unit have been observed. In both the crystallographically independent molecules, all the three six‐membered rings (A, B and C ) of steroid nucleus exist in chair conformation, while the five‐ membered ring D exists in 13β distorted‐envelope in molecule‐I and 13β, 14α half‐chair conformation in molecule‐II. Three intermolecular N‐H … O hydrogen bonds have been observed.     

Crystal and molecular structure of bis[2-ethylamino-4-n-propylamino-6-methoxy-1,3,5-triazine] copper(II) dichloride. 2-Ethylamino-4-n-propylamino-6-methoxy-1,3,5-triazine

The title compound crystallizes in the triclinic space group P1 with 2 formula units C₂₇H₅₁Cl₂CuN₁₅O₃ in the unit cell. The lattice constants are a = 11.298(2), b = 16.024(4), c = 11.977(3) Å, α = 111.64(2), β = 102.59(2), and γ = 94.46(2)°. The crystal structure was determined by the conventional R = 0.147. The complex formation and the conformations of the three independent triazine molecules are discussed.     

Crystal and Molecular Structure of 1-Ethyl-3-[tris(trimethylsiloxanyl)silyl]pyrrolinium Hydrochloride

The crystal and molecular structure of 1-Ethyl-3[tris(trimethylsiloxyl)silyl]pyrrolinium hydro-chloride (C₁₅H₃₈N⁺O₃Si₄ · C¹⁻) has been determined by direct methods. The title compound crystallizes in the monoclinic space group C2/c with a = 20.640(3), b = 19.494(2), c = 27.34(3) Å, β = 90.60(4)°, V = 11000(13) ų, Z = 16, D_x = 1.034 Mg m⁻³. There are two molecules with different conformations in the crystal. The pyrroline rings are non-planar.-The Si O Si angles range from 149(1)° to 163(1)°. Two of the SiMe₃ groups are disordered. All molecules are connected by C¹⁻ – N⁺ contacts and C¹⁻ - HN⁺ hydrogen bonds to form double chains.     

Crystal and molecular structure of (E)-21-Methoxycarbonyl-19-nor-pregna-4,8(14),20-trien-3-one

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the orthorhombic space group P 2₁2₁2₁ with cell parameters a = 12.662 Å, b = 17.995 Å, c = 8.433 Å. The structure was solved by direct methods using MULTAN-78 and refined by least-squares calculations to the conventional R = 0.061. The ring conformations of the steroid skeleton and the 17β-side chain conformation are discussed in detail.     

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.     

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.     

Structure,absolute configuration,and conformation of a fused complex cyclic carbohydrate from a cameroon plant extract (CAMT2)

The crystal and molecular structure of the natural product C₂₉H₃₈O₉, an extract from a Cameroonian plant, has been determined by direct methods. Crystals are orthorhombic, P2₁2₁2₁,a=24.571(4),b=16.398(3),c=13.778(4) Å,Z-8,D _c=1.270 mg/m³. The final R-factor for 2892 reflections withI>2(I) is 0.0531. The two molecules forming the asymmetric unit have very similar molecular geometry. each molecule comprising a nucleus of six fused rings B to G: where B=pyranyl, C=pyranyl, D=furanyl, E=cyclohexene, F=pyranyl, G=cyclohexyl. Ring B also has a furanyl side-group (ring A). The ring conformations in both molecules are: A (1/2-chair/envelope); B(envelope); C(envelope); D(1/2-chair); E(1/2-chair); F(envelope); G(chair). In the cyclohexene ring E the substitution pattern is 2-hydroxy 3-methyl 5-dimethyl. The two molecules in the asymmetric unit are linked by two OH...O hydrogen bonds to form the crystal structure.     

Crystallographic Analysis of Acetyl β ‐boswellic acid

The crystal structure of the title compound (3 α ‐acetoxy‐urs‐12‐en‐24‐oic acid, C₃₂H₅₀O₄) has been determined by X‐ray crystallographic techniques. The compound crystallizes into orthorhombic space group P2₁2₁2₁ with unit cell parameters : a = 12.773(2), b=16.381(4), c=27.929(7)Å. The structure has been solved by direct methods and refined to R = 0.054 for 4930 observed reflections. The structure contains two crystallographically independent molecules in the asymmetric unit which are almost identical in geometry. Rings A, B, D and E have chair conformations while ring C assumes a sofa conformation in both the molecules. The molecules in the structure are linked together by intra‐ and intermolecular O‐H…= and C‐H…O hydrogen bonds.     

Synthesis and characterization of single crystals of the layered copper hydroxide acetate Cu2(OH)3(CH3COO)·H2O

Single‐crystals of the layered copper hydroxide acetate Cu₂(OH)₃(CH₃COO)·H₂O were synthesized by heating copper acetate solution at 60 °C. The standard synthesis of the title compound based on slow titration of copper acetate solution with NaOH yielded materials with worse morphology and an additional phase present. The obtained products were characterized with powder X‐ray diffraction, high temperature powder X‐ray diffraction, scanning electron microscopy and infrared spectroscopy. The crystal structure was determined from single‐crystal X‐ray diffraction data, collected both at 120 K and at 293 K. The title compound crystallizes in the monoclinic botallackite‐type layered structure, space group P 2₁, with the lattice parameters a = 5.5776(3) Å, b = 6.0733(2) Å, c = 18.5134(8) Å, β = 91.802(4)° and a = 5.5875(4)Å, b = 6.0987(4) Å, c = 18.6801(10)Å, β = 91.934(5)° for 120 K and for 293 K, respectively. Acetate groups and water molecules are interlayered between corrugated sheets of edge‐sharing CuO6 octahedra exhibiting strong distortion resulted from the Jahn‐Teller effect. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 1-vinyl-3-methyl-imidazolium iodide,C6H9N2I

The title compound crystallizes with two independent molecules in the unit cell. The two molecules arecis-trans isomers. Crystal data: orthorhombic, P2₁2₁2₁,a=7.0417(6),b=9.5341(9),c=25.411(2) Å,Z=8. The crystal structure has been solved by automated Patterson methods and refined toR=0.024 for 1843 observed reflections.     

Crystal and molecular structure of chlorotris(triphenylarsine)Cu(1),C54H45As3CuCl

The title compound crystallizes in the monoclinic space groupP2₁/n, witha=28.494(2),b=10.148(5),c=32.172(2) Å,=94.57(1)°, andZ=8 (with two independent molecules in the asymmetric unit). The structure was solved by direct methods and refined by block-diagonal least-squares methods toR=0.057 for 12286 observed reflections. The dimensions and conformations of the two independent molecules are closely similar. The coordination around the copper and arsenic atoms is approximately tetrahedral, although distortion is considerable. Some important mean bond distances and angles with their rms standard deviations are: Cu-Cl=2.270(4), Cu-As=2.419(4), As-C=1.953(2) Å, Cl-Cu-As=105.4(1.2), and As-Cu-As=113.3(8)°.     

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 piperidinium-acet-p-Cl-anilide-bromide

The crystal structure of piperidinium-acet-p-Cl-anilide-bromide is monoclinic, space group P 2₁/n with 8 formula units C₁₃H₁₈N₂OBrCl in the unit cell. The lattice constants are a = 7.337(2), b = 17.865(4), c = 22.822(5) Å, and β = 94.66(1)°. The title compound is not isomorphous to the corresponding chloride. Br ions are linked to the molecules by hydrogen bonds forming chains in the crystal structure.     

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.