Structure of 11α-hydroxy-progesterone,C21H30O3

The structure of the title compound, C₂₁H₃₀O₃, was determined by X-rays.M _r =330.5, orthorhombic,P2₁2₁2₁,a=8.4451(9),b=10.7074(8),c=20.1525(40) Å,V=1822(8) ų,Z=4,D _x =1.205 mg m^–3. CuK radiation (1.54184 Å),(CuK)=5.85 cm^–1,F(000)=720. FinalR=0.054R _w =0.049 for 1774 unique reflections. The structure was solved usingMultan. TheA ring adopts an intermediate sofa-half-chair conformation and is bent toward the face of the steroid skeleton. RingsB andC have typical chair conformations, and theD ring has a slightly distorted half-chair conformation. The progesterone side chain has a typical conformation, and the C16-C17-C20-O20 torsion angle is –17.9°. An intermolecular hydrogen bond is formed between the hydroxyl group and the progesterone side chain.     

Structure of 9α, 11β-dichloro-4-pregnene-3,20-dione,C21H28O2Cl2

The crystal and molecular structure of 9, 11-dichloro-4-pregnene-3,20-dione, C₂₁H₂₈O₂C1₂, has been determined:M _r =383.4,P3₁,a=7.358(2),c=30.137(20) Å,V _c =1413(2)ų,Z=3,D _x =1.35 g cm^–3, (MoK)=0.71073Å,=3.6 cm^–1,F(000)=612,T80K,R=0.060,R _w =0.052 for 2376 unique observed reflections. The steroid skeleton exhibits a flattening of theA ring relative to the rest of the molecule caused by halogen substituents. The title compound has a very high relative binding affinity for the rabbit uterine progesterone receptor. The high binding affinity may result from the flattening of theA ring relative to the rest of the steroid skeleton.     

Synthesis and Crystal Structure of a Bulky β-Diketiminato Ytterbium(II) Iodide Complex

Abstract  

The reaction of YbI₂ with [K(THF)₃(^ButNacnac)] (^ButNacnac = [(DipNCBu^t)₂CH]⁻; Dip = C₆H₃Pr₂ⁱ-2,6) has afforded the dimeric complex, [{Yb(η⁵-^ButNacnac)(THF)(μ-I)}₂] 1. The cell parameters of compound 1 are: P-1, a = 10.498(2), b = 13.146(3), c = 16.293(3); α = 88.06(3), β = 79.43(3), γ = 71.10(3). The compound represents a rare example of a structurally characterized complex exhibiting an η⁵-interaction between a β-diketiminate ligand and an ytterbium(II) center.     

Growth from Solutions,Structure, and Spectral–Luminescent Properties of Crystalline Films of Di-n-hexyl-para-quaterphenyl

Crystallography Reports - The results of studying the growth and structure of crystalline films of para-quaterphenyl derivative with terminal n-hexyl...     

Synthesis,Crystal Structure,Antioxidant, and α-Glucosidase Inhibitory Activities of Methoxy-substituted Benzohydrazide Derivatives

Eight methoxy substituted at the benzylidene moiety benzohydrazide derivatives [R = 2-OCH₃ (1), 3-OCH₃ (2), 4-OCH₃ (3), 2,3-(OCH₃)₂ (4), 3,4-(OCH₃)₂ (5), 2,4,5-(OCH₃)₃ (6), 2,4,6-(OCH₃)₃ (7), and 3,4,5-(OCH₃)₃ (8)] were synthesized and characterized by ¹H NMR, FT-IR and UV-Vis spectroscopy. The crystal structure of 4 was determined by single crystal X-ray diffraction (sp. gr. Pbca, Z = 8). The molecule is slightly twisted with the dihedral angle between the two phenyl rings being 9.33(14)°. The methoxy group at the ortho position is twisted [C–O–C–C angle is–109.2(3)°] whereas the other at meta position is co-planar with the attached benzene ring. In the crystal packing, the molecules are linked into two-dimensional network parallel to the (001) plane by O–H···O, O–H···N, and N–H···O hydrogen bonds. Compounds 1–8 were evaluated for an antioxidant and α-glucosidase inhibitory activities and the results suggested that the ?OCH₃ substituent was ineffective for bioactivity enhancement.     

Synthesis,structure, spectroscopic investigations,and computational studies of optically pure β-ketoamide

Chemical preparation, X-ray single crystal diffraction, IR and NMR spectroscopic investigations of a novel nonlinear optical organic compound (C₁₇H₂₂NO₂Cl) are described. The compound crystallizes in the orthorhombic system with the non-centrosymmetric sp. gr. P2₁2₁2₁. In the crystal structure, molecules are interconnected by N–H…O hydrogen bonds forming infinite chains along a axis. The Hirshfeld surface and associated fingerprint plots of the compound are presented to explore the nature of intermolecular interactions and their relative contributions in building the solid-state architecture. The molecular HOMO–LUMO compositions and their respective energy gaps are also drawn to explain the activity of the compound. The first hyperpolarizability β_tot of the title compound is determined using DFT calculations. The optical properties are also investigated by UV–Vis absorption spectrum.     

Structure of the dipeptide L-lysine-L-leucine·Acetate, 0.5 acetic acid hemihydrate

2(C₁₂H₂₆O₃N₃·C₂H₃O₂)·C₂H₄O₂·H₂O,M _r =350.44, triclinic, P1,a=5.576,b=12.574(3),c=14.946(2) Å, =107.80(2), =96.34(2), =89.89(2)°.B=991.04(6) ų,Z=2,D _x =1.201 g/cm³, (KCu)=1.5418, Å, =7.4 cm^–1, room temperature.R=0.074 for 2645 observed reflections. In the unit cell there are two peptide molecules, three acetic acid molecules, two of them likely to be present as acetate anions, and one water molecule. Each peptide exists in zwitterionic form with the carboxylic group deprotonated, and with positive charges both in the amino terminal and -amino groups of lysine. The two peptide molecules have almost identical conformations. The dipeptide backbone is folded.     

Structure of 6β-acetoxyprogesterone,C23H32O4

The X-ray crystal structure of 6-acetoxyprogesterone, C₂₃H₃₂O₄, has been determined. This compound crystallizes in space groupP2₁2₁2₁ witha=13.195(3),b=15.035(4),c=10.705(3) Å,V=2139.8(9) ų,M _r=372.5,Z=4,D _x=1.156g cm^–3; MoK radiation (=0.7107 Å),=0.72 cm^–1,F(000)=808;R=0.069, andR _w=0.052 for 1292 reflections. RingA adopts a normal 1,2-half-chair conformation. The side chain is typical for a 20-ketosteroid conformation.     

Structure of 21-fluoro-4,9(11)-pregnadiene-3,20-dion-17α-yl acetate,C23H29O4F

The crystal and molecular structure of 21-fluoro-4,9(ll)-pregnadiene-3,20-dion-17a-yl acetate has been determined by X-ray diffraction methods;P2₁2₁2₁,a=15.827(4),b=16.912(4),c=7.513(2) Å,Z=4;R=0.062, (R _w =0.065) for 2028 unique observed reflections. The progesterone side chain has an unusual conformation; the C16-C17-C20-O20 torsion angle is 173.1(4)°. Molecular mechanics calculations suggest that this conformation may be cuased by 17-acetoxy substituent and the additional double bond between C9 and C11.Research supported in part by RP.II. 10 grant from the Polish Ministry of National Education (to Z. G., P. G., and Z. W.) and by PHS Grant DK26546 (to WLD).     

Structure of tetrazole steroid analogues,IV: Structure of 7a-aza-B-homocholest-5-eno [7a, 7-d]tetrazol-3β-yl-acetate (HS503)

The crystal and molecular structure of the steroidal tetrazole 7a-aza-B-homocholest-5-eno[7a,7-d]tetrazol-3-yl acetate (C₂₉H₄₆N₄O₂) has been determined by vector verification, and refined to a finalR of 0.087 for 3454 observed reflections. The compound crystallizes in space groupP2₁ with cell dimensionsa=7.352(3),b=25.950(8),c=15.408(6) Å,=91.22(3)°;Z=4,D _x=1.33 g cm^–3, (CuK)=4.87 cm^–1. The two independent molecules exhibit similar overall topography, ringsA, B, C, andD adopting chair, butterfly (Husainet al., 1981), sofa, and distorted envelope conformations respectively in both molecules.Steroids and Related Studies, Part 74.     

Crystal Structure of 9α,11-Epoxy-7α-(methoxycarbonyl)-3-oxo-17α-pregn-4-ene-21,17-carbolactone

Abstract  The title compound (common name eplerenone), C₂₄H₃₀O₆, is an aldosterone receptor antagonist. From the isopropyl acetate solution the compound crystallizes in monoclinic space group P 21 with a = 8.811(1) ?, b = 11.250(1) ?, c = 11.079(1) ?, β = 93.822(12)°, Z = 2. The molecule contains three six membered rings, two five membered rings and one three membered ring. Both five membered rings display envelope conformation, whereas three six membered rings show different conformation: chair, half-chair and envelope. In the crystal the eplerenone molecules link to one another via intermolecular weak C–H···O hydrogen bonding to form the smaller cavity of 12.0(1) ?³ between eplerenone molecules, no solvent molecule filled in this cavity. Index Abstract  In the title molecule three six-membered rings show different conformation. Weak C–H···O hydrogen bonding links adjacent molecules to form the small cavity 12.0(1) ?³, no solvent molecule filled in the cavity.      

Crystal Structure of 2-Cyclohexylethyl α-d-Mannopyranoside

Abstract  

The crystal structure of 2-cyclohexylethyl α-d-mannopyranoside (C₁₄H₂₆O₆, Mr = 290.35) has been determined by single crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system with space group C2 and unit cell parameters: a = 14.2420(2), b = 6.0320(1), c = 17.8065(3) ?, β = 102.131(2)° and Z = 4. The final reliability index is 0.0256 for 2,654 observed reflections. The one molecule of 2-cyclohexylethyl α-d-mannopyranoside is localized in independent part of unit cell. The molecules of 2-cyclohexylethyl α-d-mannopyranoside are linked through O–H···O hydrogen bond into bilayer.     

Preparation,structural, and spectroscopic study of tetrakis(4-methylpyridinium) β-octamolybdate

The title compound, (C₆H₈N)₄[Mo₈O₂₆], has been prepared and its crystal structure determined by X-ray crystallography. The compound is triclinic,P¯1,Z=1 witha=10.167(1),b=10.745(1),c=10.027(8) Å,=85.05(1),=106.73(3), =107.75(1)°,V=999.1(7) ų,F(000)=748,D _x=2.59 andD _o=2.61(1) Mg/m³. The [Mo₈O₂₆]^4– anion shows slight differences in several bond lengths and angles when compared with other related octamolybdates. The planar cations are connected to the polyanions through bifurcated hydrogen bonds. The MoO₆ octahedra are distorted and the distortion has been evaluated using three different equations. The spectroscopic study shows that the cations are protonated and the polyanion presents the well-known infrared spectrum for octamolybdates.     

Synthesis and Structure of a Chromium(III) Complex Supported by a β-diketiminate and an Enediolate Ligand

Abstract  

The complex (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(9,10-dihydro-9,10-(ethenediolato)anthracene)(tetrahydrofuran)chromium(III) (1) has been synthesized and structurally characterized. Complex 1 crystallizes in the spacegroup Cc with the crystal cell parameters a = 22.285 (3) ?, b = 9.3317 (13) ?, c = 40.782 (6) ?, β = 99.338 (3)°, V = 8369 (2) ?³, and Z = 8. Two symmetry unique complex molecules were located in the asymmetric unit making Z′ = 2. The chromium atoms display square pyramidal coordination with THF located in the axial position. The previously neutral α-diketone moiety has been reduced by two electrons to an enediolate group with a corresponding increase of oxidation state of the chromium center.     

Synthesis and Structure of Chromium(II) Complexes Supported by Both a β-Diketiminate and an Amidinate Ligand

Abstract  

The complexes (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ₂-diisopropylacetamidinato) chromium(II) (1) and (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ₂-dicyclohexylacetamidinato) chromium(II) (2) have been synthesized and structurally characterized. Complex 1 crystallizes in space group Pbcn with crystal cell parameters a = 10.7183(13) ?, b = 16.4093(19) ?, c = 20.687(2) ?, V = 3,638.3(7) ?³ and Z = 4. Complex 2 crystallizes in triclinic space group P-1 with crystal cell parameters a = 10.750(3) ?, b = 12.174(3) ?, c = 16.308(4) ?, α = 75.903(4)°, β = 82.137(4)°, γ = 85.511(4), V = 2,048.4(8) ?³ and Z = 2. The complexes adopt a spiro distorted square planar geometry and have similar structural parameters.     

Raman study of β-irradiated glasses

The ageing processes of nuclear glasses under irradiation have been simulated on three simple glass compositions (4-, 5- and 6-oxide glasses) by external β-irradiation. The structure of these glasses has been studied by Raman spectroscopy, and all three exhibit similar evolution under irradiation. The main findings are: (i) an increase of the network polymerization relative to the non-irradiated samples, (ii) an increase in concentration of molecular O₂ and (iii) a decrease of the average Si–O–Si bond angle. These data confirm the structural effects of the migration of sodium ions under external irradiation.     

Study on the Local Structure Phase Transition, Spectral Fine Structure and EPR Spectra of RbCdF3∶Ni2+ Crystals

本文采用半自洽场(semi-SCF) 3d轨道模型和μ-K-α模型,利用完全对角化方法,建立了Oh、D4h对称晶体场局部结构参数与光谱精细结构、EPR谱之间的定量关系,统一解释了RbCdF3∶ Ni2晶体的光谱精细结构和EPR谱.所得理论结果与实验值符合很好.     

X-Ray Crystal Structure of Betulin–DMSO Solvate

Abstract  

Betulin is a lupane triterpenoid [lup-20(29)-ene-3β,28-diol, C₃₀H₅₀O₂] showing high biological activity. This activity is supposed to be strongly affected by the molecular structure of its polymorphic forms. Different solvate polymorphic forms of betulin have aroused increasing interest as the possible anticancer agents of natural origin. X-ray diffraction was used to investigate crystal structure of (1:1) betulin–DMSO solvate. Title compound crystallizes in the orthorhombic P2₁2₁2₁ space group. Unit cell parameters are as follows: a = 7.0006(2) ?, b = 12.1623(3) ?, c = 33.6991(8) ?, Z = 4. Crystal packing and selected geometric parameters are described. It has been found that the hydrogen bonding and the dipole–dipole interaction between DMSO molecules play the major role in the formation of the crystal structure.     

Structure of amorphous GeSe thin films

Amorphous films of GeSe_0.7 and GeSe_2.4 have been examined by energy-filtered scanning electron diffraction and by electron microscopy. Radial distribution analysis of the GeSe_0.7 intensity curves indicates that the local atomic order of these films differs considerably from the distorted rocksalt structure of bulk crystalline GeSe. Radial distribution studies also indicate a change in the structure of GeSe_0.7 and GeSe_2.4 films supported on copper mesh as they are heated with an electron beam. Gross structural features are not observable in the electron micrographs of the amorphous films. This does not eliminate, however, the possibility of the presence of glassy phase separation on a fine scale in the heat-treated films.