Synthesis and Crystal Structure of Pergolide Sulfoxide

1998 ◽  
Vol 63 (6) ◽  
pp. 803-812 ◽  
Author(s):  
Jan Čejka ◽  
Zdeněk Horák ◽  
Svetlana Pakhomova ◽  
Bohumil Kratochvíl ◽  
Petr Sedmera ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Peroxide ◽  
Ergot Alkaloids ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Pergolide sulfoxide (1), a metabolite of pergolide (2), has been prepared by oxidation of 2 with hydrogen peroxide. Its structure was determined by X-ray diffraction and compared with the structures of related ergot alkaloids. Two molecules of pergolide (S)- and (R)-sulfoxide crystallize with one molecule of water in the orthorhombic space group P212121 with a = 12.216(3) Å, b = 13.733(2) Å, c = 22.186(6) Å, Z = 4, V = 3 722(2) Å3.

Darstellung und Kristallstruktur von Bis(triphenylphosphin)-decahydro-hypho-hexaboran [(PPh3)2B6H10]·CH2Cl2 / Synthesis and Crystal Structure of Bis(triphenylphosphine)-decahydro-hypho-hexaborane[( PPh3)2B6H10]CH2Cl2

1998 ◽  
Vol 53 (11) ◽  
pp. 1326-1328 ◽  
Author(s):  
T. Schaper ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

By reaction of [B6H6]2- with (PPh3)3AgCl in dichloromethane the belt-shaped hypho-hexaborane adduct [(PPh3)2B6H10] is formed. The crystal structure of [(PPh3)2B6H10]·CH2Cl2 has been determined by single crystal X-ray diffraction analysis: orthorhombic, space group Pbnb with a = 9.804(3), b = 17.864(4), c = 21.334(2) Å, Z = 4.

scholarly journals Synthese und Kristallstruktur von (S4N3)2Se2Cl10, (S4N3)2Se2Cl6 und [(S4Ν3)SeSeCl5]n / Synthesis and Crystal Structure of (S4N3)2Se2Cl10, (S4N3)2Se2Cl6, and [(S4N3)SeCl5]n

1989 ◽  
Vol 44 (12) ◽  
pp. 1483-1487 ◽  
Author(s):  
Hans Georg Stammler ◽  
Johannes Weiss
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Octahedral Environment ◽  
Square Planar ◽  
Distorted Octahedra

(S4N3)2Se2Cl10, (S4N3)2Se2Cl6 and [(S4N3)SeCl5]n are formed by the reaction of S4N4, Se2Cl2, and SOCl2. The structures of the three compounds where determined by X-ray diffraction. The yellow crystals of (S4N3)2Se2Cl,10 are monoclinic, space group P21/a, a = 817.5(2) pm, b = 1790.4(5) pm, c = 843.1(6) pm, β = 104.31(4)°, Z = 2. The Se2Cl,102- anion consists of 2 Cl-bridged distorted octahedra. (S4N3)2Se2Cl6 forms red monoclinic crystals, space group P21/c, a = 1036.5(3) pm, b = 1376.5(5) pm, c = 1400.4(4) pm, β = 100.65(2)°, Ζ = 4. In the Se2Cl62- anion the Se atoms have a square planar environment. The yellow crystals of (S4N3)SeCl5 are orthorhombic, space group P212121, a = 734.2(3) pm, b = 989.4(4) pm, c = 1627.4(6) pm, Z = 4. In the SeCl5- anion the Se atom has an octahedral environment of chlorine atoms, thus forming a polymeric structure.

scholarly journals β-Y(BO2)3 – a new member of the β-Ln(BO2)3 (Ln=Nd, Sm, Gd–Lu) structure family

2017 ◽  
Vol 72 (12) ◽  
pp. 983-988 ◽  
Author(s):  
Martin K. Schmitt ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Abstractβ-Y(BO2)3 was synthesized in a Walker-type multianvil module at 5.9 GPa/1000°C. The crystal structure has been elucidated through single-crystal X-ray diffraction. β-Y(BO2)3 crystallizes in the orthorhombic space group Pnma (no. 62) with the lattice parameters a=15.886(2), b=7.3860(6), and c=12.2119(9) Å. Its crystal structure will be discussed in the context of the isotypic lanthanide borates β-Ln(BO2)3 (Ln=Nd, Sm, Gd–Lu).

The X-Ray Crystal Structure of 1,2-3,4-Di-O-isopropylidene-4-C-methylthiomethoxy-β-L-arabino-hexoseptanos-5-ulose

1990 ◽  
Vol 43 (12) ◽  
pp. 2083 ◽  
Author(s):  
DC Craig ◽  
VJ James ◽  
JD Stevens
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Membered Ring ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The crystal structure of the title compound (1) has been determined by X-ray diffraction. Crystals of (1) are orthorhombic, space group P21212 with a 11.425(1), b 24.916(1), c 5.8952(3)Ǻ, Z 4. Refinement on 1675 observed reflections measured with Cu Kα radiation converged at R 0.034. The seven- membered ring adopts a boat conformation in which the pseudo plane of symmetry passes through the ring oxygen.

scholarly journals Zur Darstellung und Kristallstruktur von β-NbO2 / Synthesis and Crystal Structure of β-NbO2

1982 ◽  
Vol 37 (11) ◽  
pp. 1361-1368 ◽  
Author(s):  
H.-J. Schweizer ◽  
Reginald Gruehn
Keyword(s):  
Crystal Structure ◽  
Long Range ◽  
Chemical Transport ◽  
Range Order ◽  
Long Range Order ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

By using chemical transport reactions with various transporting agents (HgCl2, NbCl5, Nb3O7Cl) a slightly substoiehiometric NbO2-phase, β-NbO2, was obtained from samples with O/Nb ∼ 1.5 (source; T > 1373 K) and with deposition temperatures > 1273 K (sink). The rango of composition of β-NbO2 was found to exist from NbO1.990 to NbO1.998.The structure of the tetragonal, column-shaped black crystals was determined by X-ray diffraction. It crystallizes tetragonally in the space group I41 with lattice constants a = 9.693(3) Å, c = 5.985(1) Å and Z = 10 formula units.The crystal structure of β-NbO2 is shown to be a deformed rutile type. As in α-NbO2 the Nb-atoms are grouped in pairs. However, both oxides are different with respect to their long-range order.

Preparation and Structure of Tetraphenylarsonium Tris(1,2-dicyanoethenedithiolato)technetate(IV)

1988 ◽  
Vol 41 (7) ◽  
pp. 1127 ◽  
Author(s):  
SF Colmanet ◽  
MF Mackay
Keyword(s):  
Crystal Structure ◽  
Distorted Octahedron ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ethanol Yields

The reaction of sodium 1,2-dicyanoethenedithiolate [( mnt )Na2] with (NH4)2 [TcBr6] in ethanol yields crystals of (AsPh4)2 [ Tc ( mnt )3] (1) after precipitation with AsPh4Cl. The crystal structure of (1) has been determined by X-ray diffraction. Crystals are orthorhombic, space group Pbcn , a 20.256(1), b 15.513(1), c 18.274(1)Ǻ, Z 4. Refinement on 2910 diffractometer data measured with Cu Kα radiation converged at R 0.056. The structure consists of [ Tc ( mnt )3]2- anions and (AsPh4)+ cations . The technetium(IV) atom is coordinated to six sulfur atoms to give a distorted octahedron.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Polysulfonylamine, CIII [1] Ein Hydroxylamin mit bemerkenswert kurzer O-N-B Bindung: Kristall- und Molekülstruktur von MeO-N(SO2Me)2 / Polysulfonylamines, C III [1] A Hydroxylamine with a Remarkably Short O-N Bond: Crystal and Molecular Structure of MeO-N(SO2Me)2

1998 ◽  
Vol 53 (5-6) ◽  
pp. 634-636 ◽  
Author(s):  
Martina Näveke ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Low Temperature ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles

Abstract The crystal structure of the known title compound was determined by low-temperature X-ray diffraction (orthorhombic, space group Pbcn, Z = 4). The molecule displays an unusually short O-N bond, a relatively long C-O bond and a moderately pyramidal O-NS2 skeleton (O-N 133.1, C-O 148.5 pm, sum of bond angles at N: 347.4°).

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Synthese und Kristallstruktur von [Hg2(p-SC6H4NO2)]NO3 / Synthesis and Crystal Structure of [Hg2(p-SC6H4NO2)]NO3

1990 ◽  
Vol 45 (8) ◽  
pp. 1193-1196 ◽  
Author(s):  
Klaus Brodersen ◽  
Axel Knörr
Keyword(s):  
Crystal Structure ◽  
Chain Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrate Ions ◽  
R Value ◽  
A Chain

[Hg2(p-SC6H4NO2)]NO3 is formed by the reaction of p-nitrothiophenol with dimercury(I)-dinitrate in methanol. It crystallizes in the monoclinic space group P21/n with a = 1175.5(9) pm, b = 1079.8(8) pm, c = 876.2(8) pm, β = 110.74(4)° and Z = 4. The crystal structure has been determined by X-ray diffraction and refined to an R-value of 0.052. The results show that the compound exists as a chain structure of [—®S(C6H4NO2)— Hg— Hg—]n with nitrate ions connecting the chains.

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