Crystallographic studies on neuroleptics of the benzocycloheptapyridoisoquinoline series. The crystal structure of butaclamol hydrobromide and the absolute configuration and crystal structure of dexclamol hydrobromide

1976 ◽  
Vol 54 (17) ◽  
pp. 2715-2722 ◽  
Author(s):  
P. H. Bird ◽  
F. T. Bruderlein ◽  
L. G. Humber
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atom ◽  
Membered Ring ◽  
Axial Position ◽  
Aromatic Rings ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Cell Dimensions ◽  
R Value ◽  
Hydroxy Groups

The compound butaclamol hydrobromide crystallizes in space group P21/c with cell dimensions; a = 14.38(3), b = 13.31(3), c = 12.07(3) Å, β = 101.64(8)°. The structure was solved by Patterson methods and non-hydrogen atoms have been refined isotropically using a full-matrix least-squares to an R value of 0.17 for 779 observed reflections.The compound dexclamol hydrobromide crystallizes in space group P212121 with a = 8.412(2), b = 24.392(7), c = 10.465(2) Å. Refinement of non-hydrogen atoms using isotropic thermal parameters and rigid aromatic rings converted at R = 0.090 using 1249 observed reflections, for the preferred enantiomorph, and R = 0.099 for the other enantiomorph.Both compounds have their hydroxy groups in the axial position, and both adopt conformations of the seven membered ring such that the C13b hydrogen atom experiences a flagpolebowsprit interaction with a hydrogen atom of C9.

Refinement of the structure of Mg2As2O7

1970 ◽  
Vol 48 (6) ◽  
pp. 890-894 ◽  
Author(s):  
C. Calvo ◽  
K. Neelakantan
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Central Oxygen ◽  
R Value ◽  
Unit Cell Dimensions

The crystal structure of Mg2As2O7 has been refined by full matrix least squares procedures using 587 observed reflections. The structure of Mg2As2O7 is of the thortveitite type, as reported by Łukaszewicz, with space group C2/m and unit cell dimensions a = 6.567(2) Å, b = 8.524(4) Å, c = 4.739(1) Å, β = 103.8(1)°, and Z = 2. The As—O—As group in the anion appears to be linear but the central oxygen atom undergoes considerable disorder in the plane perpendicular to this group. The AsO bond distances uncorrected for thermal motion are 1.67 Å for the As—O(—As) bond and 1.66 and 1.65 Å for the terminal As—O bonds. The final R value obtained is 0.088.

The Crystal Structure of Caesium Oxotetrafluorovanadate(V)

1972 ◽  
Vol 50 (22) ◽  
pp. 3700-3705 ◽  
Author(s):  
G. W. Bushnell ◽  
K. C. Moss
Keyword(s):  
Crystal Structure ◽  
Chain Structure ◽  
Vanadium Atom ◽  
Tetragonal Pyramid ◽  
Space Group ◽  
Bond Lengths ◽  
Structural Relationships ◽  
Cell Dimensions ◽  
R Value ◽  
Anionic Chain

The crystal structure of caesium oxotetrafluorovanadate(V) has been solved and refined to an R-value of 0.070 using diffractometer measurements. The cell dimensions are: a = 548.4(2) pm, b = 634.2(2) pm, c = 1403.4(3) pm. The space group is Pnma (No. 62) with four formula units per cell. Each vanadium atom lies 32.6 pm above the base of a tetragonal pyramid with oxygen at the apex (V=O length = 152.9 pm) and fluorine at the four base corners (mean V—F length = 178.8 pm). The tetragonal pyramids are linked by cis-fluorine bridges involving a long V—F bond (V—F(21) = 231.2 pm) to give an anionic chain structure. Structural relationships with other fluorides and oxide-fluorides are noted, and the bond lengths are discussed.

An X-Ray Study of the Synthetic Intermediate 9-Cyano-1,10-Dimethyl-6-Ethylenedioxy-1-Octalin

1975 ◽  
Vol 53 (2) ◽  
pp. 192-194 ◽  
Author(s):  
Harry Lynton ◽  
Pik-Yuen Siew
Keyword(s):  
Crystal Structure ◽  
Total Synthesis ◽  
Direct Methods ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Ring Junction ◽  
Cell Dimensions ◽  
R Value ◽  
Synthetic Intermediate

The crystal structure of the synthetic intermediate, 9-cyano-1,10-dimethyl-6-ethy]enedioxy-1-octalin, C15H21O2N, was solved by direct methods. The compound crystallizes in the space group p21/c with cell dimensions a = 12.282(4), b = 7.144(3), c = 15.619(5) Å, β = 104.04(1)°. Refinement was carried out isotropically for hydrogen and anisotropically for non-hydrogen atoms using full matrix least squares to an R-value of 0.043 for 1669 observed reflections.This compound, which has a cis configuration at the octalin ring junction, is a precursor to a moiety of the alkaloid thelepogine. The cis conformation is essential for total synthesis of thelopogine by this route.

The crystal and molelcular structure of benzil bisthiosemicarbazonatocopper(II) and the antitumour mechanism of related compounds

1979 ◽  
Vol 57 (6) ◽  
pp. 603-607 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Annie Y. M. Tsang
Keyword(s):  
Crystal Structure ◽  
Hydrogen Atoms ◽  
Copper Coordination ◽  
Cell Dimensions ◽  
Phenyl Rings ◽  
The Mean ◽  
R Value ◽  
Related Compounds ◽  
Double Hydrogen ◽  
Coordination Plane

The crystal structure of benzil bisthiosemicarbazonatocopper(II) has been solved and refined to an R-value of 0.082. The dark red triclinic crystal has cell dimensions a = 960.8(4), b = 1090.7(6), c = 895.8(4) pm, α = 106.23°(4), β = 92.36°(7), γ = 99.50°(7), and belongs to space group [Formula: see text] with two molecules per cell. The measured and calculated densities are 1.571 and 1.568 g cm−3, respectively, using C16H14CuN6S2 (mol. wt. 417.99). The copper coordination is significantly non-planar. The five non-hydrogen atoms of each original thiosemicarbazide molecule lie close to planes set at a dihedral angle of 8.9°. The fold is away from the origin and the neighbouring molecule. Bond lengths to copper are: Cu—S(1) = 223.7(3), Cu—S(2) = 223.4(3), Cu—N(13) = 197.1(6), Cu—N(23) = 197.0(7) pm. The bond angles at the Cu atom are S(1)—Cu—S(2) = 108.62°(9), N(13)—Cu—N(23) = 81.1°(3), N(13)—Cu—S(1) = 85.1°(2), and N(23)—Cu—S(2) = 85.0°(2). The first and second phenyl rings are at 100.3° and 93.0° to the mean Cu coordination plane, which is at a perpendicular distance of 330 pm from a similar plane in the inverse molecule. Intermolecular double hydrogen bonding occurs at each side of the complex between the uncoordinated nitrogen atoms, thus linking the molecules into parallel ribbons.

scholarly journals The Crystal Structure of bis-(μ-N-ethyl-Nphenyldithiocarbamato- S,S’)-bis[(N-ethyl-Nphenyldithiocarbamato- κ2S,S’)zinc(II)]

2021 ◽  
Author(s):  
Robert A Gossage ◽  
Hilary A Jenkins
Keyword(s):  
Crystal Structure ◽  
Metal Atom ◽  
Unit Cell ◽  
Secondary Amines ◽  
Triclinic Crystal System ◽  
Space Group ◽  
Crystal System ◽  
Cell Dimensions ◽  
R Value ◽  
Unit Cell Dimensions

The title material crystallises in the triclinic crystal system in space group P-1 with Z = 2. The unit cell dimensions are a = 8.7365(6)Å, b = 10.6009(7)Å, c = 12.0210(8)Å with α = 66.343(1)°, β = 79.566(1)°, γ = 83.150(1)° and V = 1001.6(1)Å3. The final R value is 0.0307 (3905 observed reflections: I >2σ(I)). The compound is best described as a species in which each metal atom is coordinated to two dithiocarbamato groups, one of which forms a secondary bridging interaction (through a S-atom) to a second [Zn(S2CNEtPh)2] unit. Thus, the title material is in the form of a dimeric aggregate. This complex is compared to related materials which contain N-atoms within the dithiocarbamato ligand that are derived from secondary amines containing two different organic functionalities.

scholarly journals The Crystal Structure of bis-(μ-N-ethyl-Nphenyldithiocarbamato- S,S’)-bis[(N-ethyl-Nphenyldithiocarbamato- κ2S,S’)zinc(II)]

2021 ◽  
Author(s):  
Robert A Gossage ◽  
Hilary A Jenkins
Keyword(s):  
Crystal Structure ◽  
Metal Atom ◽  
Unit Cell ◽  
Secondary Amines ◽  
Triclinic Crystal System ◽  
Space Group ◽  
Crystal System ◽  
Cell Dimensions ◽  
R Value ◽  
Unit Cell Dimensions

The title material crystallises in the triclinic crystal system in space group P-1 with Z = 2. The unit cell dimensions are a = 8.7365(6)Å, b = 10.6009(7)Å, c = 12.0210(8)Å with α = 66.343(1)°, β = 79.566(1)°, γ = 83.150(1)° and V = 1001.6(1)Å3. The final R value is 0.0307 (3905 observed reflections: I >2σ(I)). The compound is best described as a species in which each metal atom is coordinated to two dithiocarbamato groups, one of which forms a secondary bridging interaction (through a S-atom) to a second [Zn(S2CNEtPh)2] unit. Thus, the title material is in the form of a dimeric aggregate. This complex is compared to related materials which contain N-atoms within the dithiocarbamato ligand that are derived from secondary amines containing two different organic functionalities.

Über die Kristallstruktur von KSc2 F7 / The Crystal Structure of KSc2 F7

1985 ◽  
Vol 40 (6) ◽  
pp. 726-729 ◽  
Author(s):  
Klaus Güde ◽  
Christoph Hebecker
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Unit Cell ◽  
Space Group ◽  
X Ray ◽  
Monoclinic Unit Cell ◽  
R Value ◽  
Ray Methods

Abstract Single crystals of KSc2F7 have been prepared from a mixture of KF and ScF3 . The samples were investigated by X-ray methods. KSc2F7 crystallizes orthorhombically with a = 10.643(2), b = 6.540(1), c = 4.030(1) Å. These data indicate a close crystallographic connection to the monoclinic unit cell of KIn2F7 [1], But in contrast to KIn2F7 , KSc2 F7 crystallizes in space group No. 65. Cmmm - D192h. The R-value for 341 observed independent reflections is 0.060.

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.

Crystal structure of N,N '-Ethylenebis(1,1,1-Trifluoro-4-iminopentan-2-one)

1984 ◽  
Vol 37 (4) ◽  
pp. 879 ◽  
Author(s):  
R Cea-Olivares ◽  
I Rodriguez ◽  
MJ Rosales ◽  
A Toscano
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Enamino Ketone ◽  
Space Group ◽  
R Value ◽  
Intramolecular Hydrogen

The crystal structure of N,N'-ethylenebis(1,1,1-trifluoro-4-iminopentan-2-one) (tfaen) was determined: C12H14F6N2O2, M 342.04, monoclinic, space group P21/n, a 6.939(2), b 20.529(5), c 10.662(2) �, V 1507.84 �3 β 96.87(2)�, p(calc.) 1.506 g cm-3 (Z = 4), F(000)680, �(Cu Kα) 13.15 cm-1. The structure was solved by direct methods and refined to a final R value of 0.073 for 1198 unique reflections. Discrete molecules in the crystal are characterized by a conjugated enamino ketone structure with intramolecular hydrogen bridges.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

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