2-Hydroxyindole Compounds. Alkylation of 3-Acetyl-1-benzyl-2-hydroxy-5-,ethoxyindole Under Basic Conditions

1992 ◽  
Vol 45 (12) ◽  
pp. 1953 ◽  
Author(s):  
HM Hugel ◽  
RJ Greenwood ◽  
MF Mackay
Keyword(s):  
Least Squares ◽  
Molecular Mechanics ◽  
Spectroscopic Data ◽  
Minimum Energy ◽  
Benzyl Bromide ◽  
Crystallographic Analysis ◽  
Energy Structure ◽  
Space Group ◽  
X Ray

Alkylation of 3-acetyl-1-benzyl-2-hydroxy-5-methoxyindole with benzyl bromide in the presence of base resulted in isolation of the C- alkylated product which has been shown by X-ray crystallographic analysis to be 3-acetyl-1,3-dibenzyl-5-methoxy-1,3-dihydro-2H-indol-2-one (5c) in accord with the spectroscopic data. Triclinic crystals of (5c) belong to the space group P1 with a 10.649(3), b 13.736(3), c 14.555(2) Ǻ, α: 86-73(2), β 85.98(2), γ 78-01(2)° and Z 4. Least-squares refinement with 1996 observed data converged at R 0.061. Molecular mechanics was used to calculate the minimum-energy structure of (5c) which is compared with the X-ray results.

The reaction of tetrasulphur dinitride with norbornadiene; the crystal and molecular structure of S4N2•C7H8, an eight-membered C2S4N2 heterocycle

1983 ◽  
Vol 61 (6) ◽  
pp. 1185-1188 ◽  
Author(s):  
Hans Koenig ◽  
Richard T. Oakley ◽  
A. Wallace Cordes ◽  
Mark C. Noble
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reaction of tetrasulphur dinitride with norbornadiene produces the 1:1 adduct S4N2•C7H8; X-ray crystallographic analysis of this compound reveals that olefin addition cleaves one of the sulphur–sulphur bonds of S4N2, yielding a novel eight-membered C2S4N2 ring. Crystals of S4N2•C7H8 are monoclinic, space group P21/c, a = 6.127(1), b = 17.369(1), c = 9.580(1) Å, β = 106.74(1)°, V = 1003.8(5) Å3Z = 4. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.039. The S—S—N—S—N—S fragment of the C2S4N2 ring is planar to within 0.15 Å. The S—C—C—S unit is folded out of this plane to produce a dihedral angle of 74.5°.

Rearrangements in the Furan Series. V. Reaction of 2,4-Di-p-methylanilino-cyclopent-2-enone With Maleic Anhydride

1991 ◽  
Vol 44 (11) ◽  
pp. 1533 ◽  
Author(s):  
BR Darcy ◽  
KG Lewis ◽  
PJ Oliver ◽  
MF Mackay
Keyword(s):  
Acetic Acid ◽  
Maleic Anhydride ◽  
Spectroscopic Data ◽  
Crystallographic Analysis ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Furan Series

A yellow product formed in the reaction of 2,4-di-p-methylanilinocyclopent-2-enone with maleic anhydride has been shown by X-ray crystallographic analysis to be (4′-p-methylanilino-1′-p-methylphenyl-2′,5′-dioxo-1′,2′,3′,5′,6′,6′a- hexahydrocyclopenta[b]pyrrol-3′-yl)acetic acid (3) in accord with the spectroscopic data. Monoclinic crystals of (3) belong to the space group P21/n with a 13.399(2), b 8.386(1), c 17.935(3)Ǻ, β 92.06(2)° and Z 4. Full-matrix refinement with 2292 observed data converged at R 0.063.

The structure of u-fac-(Diethylenetriamine)[di(3-aminopropyl)amine]cobalt(III) perchlorate, [Co(dien)(dpt)] (ClO4)3, and an energy minimization analysis of the [Co(dien)(dpt)]3+ system

1984 ◽  
Vol 37 (2) ◽  
pp. 249 ◽  
Author(s):  
TW Hambley ◽  
GH Searle
Keyword(s):  
Molecular Mechanics ◽  
Energy Minimization ◽  
Crystallographic Analysis ◽  
Geometric Isomers ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Mechanics Analysis ◽  
Chelate Rings

X-ray crystallographic analysis of u-fac-[Co(dien)(dpt)] (ClO4)3,H2O [dien = diethylenetriamine, dpt = di(3-aminopropyl)amine] confirms the assigned u-fac geometry. The two six-membered chelate rings of the coordinated dpt adopt chair and flattened-chair conformations. The crystals are triclinic, space group P1, with a 8.979(2), b 11.436(2), c 11.463(3) �, α 91.15(2), β 101 .84(2), γ 93.41(2)�. A molecular mechanics analysis of the three [Co(dien)(dpt)]3+ geometric isomers gives the u-fac as the most stable, in accord with experimental observations.

Stereochemistry of α-Amino Oximes From the Monoterpene Hydrocarbons Car-3-ene, Limonene and α-Pinene

1992 ◽  
Vol 45 (6) ◽  
pp. 1077 ◽  
Author(s):  
AV Tkachev ◽  
AV Rukavishnikov ◽  
AM Chibiryaev ◽  
AY Denisov ◽  
YV Gatilov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Molecular Mechanics ◽  
High Field ◽  
Crystallographic Analysis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Molecular Mechanics Calculations ◽  
Space Group ◽  
X Ray ◽  
Monoterpene Hydrocarbons

The conformation and configuration of the α-amino oximes derived from the terpene hydrocarbons car-3-ene, limonene and α- pinene have been determined by n.m.r. spectroscopy (high-field 1H n.m.r., 13C n.m.r., INADEQUATE technique), molecular mechanics calculations and X-ray crystallographic analysis. The crystal structure of (lS,3S,6R)-3-dimethylamino-caran-4-one (E)-oxime has been determined by X-ray diffraction; crystals are orthorhombic, space group P 212121 with a 11.421(2), b 13.223(2), c 16.992(4) �, Z 8. Refinement on 1730 observed reflections measured with Cu K α radiation converged at R 0.053.

Die Röntgenstrukturanalyse von (CO)9Co3CΟΒΒr2Ν(C5)3. X-ray Structure Analysis of (CO)9Co3COBBr2N(C2H5)3

1976 ◽  
Vol 31 (3) ◽  
pp. 342-344 ◽  
Author(s):  
Volker Bätzel
Keyword(s):  
Least Squares ◽  
Structure Analysis ◽  
Reliability Index ◽  
Three Dimensional ◽  
Diagonal Matrix ◽  
Crystal Data ◽  
Block Diagonal Matrix ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray

Using three dimensional X-ray data collected on a four circle diffractometer, the structure of (CO)9Co3COBBr2N(C2H5)3 was solved by Patterson and Fourier methods. Least squares refinement with a block-diagonal matrix leads to a reliability index of R = 10.7%. Crystal data: α = 13.277(6) Å, b = 10.17(1) Å, c = 9.22(2) Å; α = 91.12(6)°, β = 87.61(4)°, γ = 98.79(2)°; space group P1̅; Z = 2; V = 1229,7 Å3; Dx = 1.97 gcm-3.

Crystallization and preliminary X-ray crystallographic analysis of the Pseudomonas aeruginosa cyclohexadienyl dehydratase

1999 ◽  
Vol 55 (2) ◽  
pp. 539-541
Author(s):  
Palangpon Kongsaeree ◽  
Jun Liang ◽  
Roy A. Jensen ◽  
Jon Clardy
Keyword(s):  
Pseudomonas Aeruginosa ◽  
Crystal Form ◽  
High Energy ◽  
Crystallographic Analysis ◽  
Unit Cell ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The title protein has been crystallized in a new crystal form. The crystals belong to the cubic space group P4132 (or P4332) with unit-cell dimensions a = b = c = 126.1 Å at 100 K and typically diffract beyond 1.6 Å at the Cornell High Energy Synchotron Source (CHESS) A1 beamline.

The crystal structure of dibutyl-bis(pentamethylenedithiocarbamato)tin(IV)

1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Distorted Octahedron ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.

Studies on the Nature and Strength of Pt . . .H(-N) Interactions. The Crystal Structures of Chloro[N-(2-aminoethyl)-N-(2-ammonioethyl)ethane-1,2-diamine]platinum(II) Chloride and Dichloro[4,7-diaza-1-azoniacyclononane]platinum(II) Tetrachlor

2000 ◽  
Vol 53 (6) ◽  
pp. 451 ◽  
Author(s):  
Murray S. Davies ◽  
Ronald R. Fenton ◽  
Fazlul Huq ◽  
Edwina C. H. Ling ◽  
Trevor W. Hambley
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Molecular Mechanics ◽  
Metal Ion ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Protonated Amine ◽  
Protonated Amines ◽  
Close Contacts

Two complexes, namely, chloro[N-(2-aminoethyl)-N-(2-ammonioethyl)ethane-1,2-diamine]platinum(II) chloride {[PtCl(tren+H)]Cl2} and dichloro[4,7-diaza-1-azoniacyclononane]platinum(II) tetrachloroplatinate(II)–water (1/2) {[PtCl2(tacn+H)]2[PtCl4]·2H2O}, have been prepared and structurally characterized by single-crystal X-ray diffractometry as part of a study of the nature and strength of Pt···H(–N) interactions. Crystals of [PtCl(tren+H)]Cl2 are monoclinic, space group P21/c, a 8.293(2), b 14.396(6), c 11.305(3) Å, β 107.34(2)º, Z 4, and the structure has been refined to a residual of 0.042 based on 1631 reflections. Crystals of [PtCl2(tacn+H)]2[PtCl4]·2H2O are monoclinic, space group P21/a, a 12.834(4), b 8.206(4), c 13.116(8) Å, β 93.01(4)˚, Z 2, and the structure has been refined to a residual of 0.035 based on 1974 reflections. In [PtCl(tren+H)]2+, the protonated amine forms hydrogen bonds with chloride anions and no close contacts with the metal ion. In [PtCl2(tacn+H)]+, a short intramolecular contact is observed between the metal and the protonated amine and the results of molecular mechanics modelling are consistent with there being a Pt···H hydrogen bond. Molecular mechanics modelling of [PtCl(tren+H)]2+ and [PtCl2(dien+H)]+ shows that the protonated amines could readily form close contacts with the metal. It is concluded that there is evidence for the formation of Pt···H(–N) hydrogen bonds but these bonds are very weak, being similar or lower in energy than Cl···H(–NPt) hydrogen bonds.

The crystal structure of kogarkoite, Na3SO4F

1980 ◽  
Vol 43 (330) ◽  
pp. 753-759 ◽  
Author(s):  
L. Fanfani ◽  
G. Giuseppetti ◽  
C. Tadini ◽  
P. F. Zanazzi
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Least Squares Method ◽  
Thermal Parameters ◽  
Cell Content ◽  
Space Group ◽  
X Ray ◽  
Structural Relationships ◽  
Automatic Diffractometer ◽  
Monoclinic Cell

SummaryThe crystal structure of synthetic kogarkoite has been determined from X-ray data collected on an automatic diffractometer. The refinement was performed by a least-squares method employing anisotropic thermal parameters. The 3157 reflections with I > 3σ(I) converged to a conventional R value of 0.033. The cell content is 12 Na3SO4F, the space-group P21/m, a = 18.074, b = 6.958, c = 11.443 Å, β = 107.71°.Kogarkoite presents a marked trigonal subcell with c′ corresponding to [102] of the monoclinic cell. The tridimensional framework can be considered built up by nine differently stacked layers of Na atoms approximately perpendicular to the c′ axis (five sheets are present in galeite, six in sulphohalite, and seven in schairerite). The very close structural relationships between these minerals are discussed.

The chemistry of Eremophila spp. XVIII. A new class of diterpenes from Eremophila viscida

1983 ◽  
Vol 36 (5) ◽  
pp. 993 ◽  
Author(s):  
EL Ghisalberti ◽  
CH Hocart ◽  
PR Jefferies ◽  
GM Proudfoot ◽  
BW Skelton ◽  
...  
Keyword(s):  
Spectroscopic Data ◽  
Crystallographic Analysis ◽  
X Ray ◽  
New Class

Two new diterpenes have been isolated from the resin of E. viscida Endl. Evidence for their structure was obtained from spectroscopic data and from X-ray crystallographic analysis which show them to be members of a new class of diterpenes containing a C 5 extended acorane skeleton.

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