5-Allyl-9-oxobenzomorphans. Part 2. The Crystal and Molecular Structure of an Unusual Product of Dequaternization of 5-Allyl-9-oxobenzomorphan Methobromide

1975 ◽  
Vol 53 (21) ◽  
pp. 3276-3284 ◽  
Author(s):  
Farid R. Ahmed ◽  
Michel Saucier ◽  
Ivo Monković
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Methoxy Derivative ◽  
X Ray ◽  
Unusual Product ◽  
Single Crystal Analysis

The synthesis of 5-allyl-2'-methoxy-9-oxo-6,7-benzomorphan (5b) is described. The 10-hydroxy-2-methyl-1,11-propano-9H-indeno-1,2,10,11-tetrahydro[2,1-c]pyridine (7a) and the corresponding 6-methoxy derivative (7b) are unexpected products of pyrolysis of 5-allyl-2-methyl-9-oxobenzomorphan methobromide (4a) and 5-allyl-2′-methoxy-2-methyl-9-oxobenzomorphan methobromide (4b) respectively. The molecular structure of 7a (C16H19NO) has been determined from spectral and microanalytical data, and confirmed by X-ray single crystal analysis on its hydrobromide salt using the heavy atom technique. The crystals of [C16H20NO]+Br− are monoclinic, P21/a, with a = 13.724(2), b = 14.022(3), c = 7.495(2) Å, β = 97.33(5)°, and Z = 4. The crystal structure has been refined by block-diagonal least-squares calculations to R and Rw = 0.036 for the 2197 observed reflections. The N atom has planar trigonal coordination, and forms one double and two single C—N bonds of lengths 1.273(4), 1.465(4), and 1.474(4) Å, respectively. The Br is hydrogen-bonded to O. The N and O atoms are trans.

Studies of the rhenium–oxygen bond. II. The crystal and molecular structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2ORe(C5H5N)2Cl2O

1978 ◽  
Vol 56 (2) ◽  
pp. 179-188 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Full Matrix ◽  
X Ray ◽  
Ray Methods ◽  
Oxygen Bond

The crystal structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2•O•Re(C5H5N)2Cl2O bas been studied by single crystal X-ray methods. The crystals were orthorhombic with lattice parameters a = 15.367(2), b = 10.283(2), c = 16.685(2) Å. The space group was Pna21 and there were four formula weights per unit cell. A total of 3339 reflections, of which 2990 were observed, were examined, and the structure refined by full matrix least squares (treating the pyridine rings as groups) to an R2 value of 0.0449. The dimer had a roughly rectilinear O—Re—O—Re—O backbone with pairs of chlorine atoms and pyridine molecules arranged cis in each half of the dimer. The two halves of the dimer were arranged such that the pairs of cis atoms in one half were rotated about the Re(1)–Re(2) axis almost 113 ° when compared to the corresponding pair in the other half. Important bond lengths (Re—O(terminal), 1.715(16), 1.764(16); Re—O(bridging), 1.943(16), 1.903(16); Re—Cl, 2.356(5)–2.390(5); Re—N, 2.116(16)–2.180(16)) were close to previously observed values. The molecule was markedly disturbed from the idealized structure and this was caused by intramolecular non-bonded interactions.

The crystal and molecular structure of (±)-('E')-N-Acetylpiperidine-2-carboxylic acid

1980 ◽  
Vol 33 (1) ◽  
pp. 215 ◽  
Author(s):  
ID Rae ◽  
CL Raston ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Carboxylic Acid ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of N-acetylpiperidine-2-carboxylic acid has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined by least squares to a residual of 0.039 for 846 'observed' reflections. Crystals are orthorhombic, with space group Pbca, a 13.684(6), b 11.602(4), c 11.171(4)Ǻ, Z 8. The ring is a chair structure in which, contrary to an earlier proposal based on 1H n.m.r. studies, there is almost perfect staggering about the C(2)-C(3) bond.

Studies of β-Diketone Complexes of Rhenium. VII. The Crystal and Molecular Structure of Oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V)

1975 ◽  
Vol 53 (11) ◽  
pp. 1548-1553 ◽  
Author(s):  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Bonding Interaction ◽  
Ray Methods

The crystal structure of oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V) has been studied by single crystal X-ray methods. The crystals are triclinic with lattice parameters a = 11.023(8) Å, b = 13.523(8) Å, c = 9.360(7) Å, α = 90.2(1)°, β = 114.1(1)°, γ = 67.7(2)°. The space group is [Formula: see text] and there are two formula weights per unit cell. A total of 2891 reflections, of which 2447 were observed, were examined, and the structure was refined by full matrix least squares to an R2 value of 0.0782. The ligands are arranged around the rhenium atom such that the nearest six atoms are at the corners of a very distorted octahedron. Most of this distortion appears to be caused by nonbonding repulsive interactions. The short oxo–phosphine distance, 2.85(1) Å, suggests the possibility of a weak bonding interaction. Observed bond distances (Re—Cl, 2.35 Å av; Re—O(oxo), 1.69(1) Å; Re—O(diketone), 1.99(1), 2.10(1) Å; Re—P, 2.431(4) Å) are close to those observed previously in similar compounds.

The crystal and molecular structure of dipyrrolidylthiuram disulfide

1983 ◽  
Vol 36 (7) ◽  
pp. 1371 ◽  
Author(s):  
GA Williams ◽  
JR Statham ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Structural Parameters ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray

The crystal structure of dipyrrolidylthiuram disulfide has been determined by single-crystal X-ray diffraction techniques at 295 K. Crystals are monoclinic, space group C2/c, unit cell a 13.835(3), b 10.422(2), c 9.427(3) �, β 97.08(2)� and Z 4. Automatic diffractometry has provided significant Bragg intensities for 1402 independent reflections, and the structure has been refined by least-squares methods to R 0.037. The structure consists of discrete C4H8NC(S)S2C(S)NC4H8 molecules. Half of each molecule is crystallographically unique with distances S-S 2.002(1), and C-S 1.804(2) and 1.645(2) �. The dihedral angle between planar C2NC(S)S portions is 87.9�. The relevance of the derived structural parameters to the question of why the tris(pyrrolidine-1-carbodithioato)iron(III) complex is, uniquely, high spin is discussed.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

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.

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

Crystal and Molecular Structure of Dithiocyanato(triphenylarsine)mercury(II)

1975 ◽  
Vol 53 (22) ◽  
pp. 3383-3387 ◽  
Author(s):  
Joseph Hubert ◽  
André L. Beauchamp ◽  
Roland Rivest
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Coordination Number ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heavy Atom Method

The crystal and molecular structure of dithiocyanato(triphenylarsine)mercury(II) has been determined from X-ray diffraction data. The crystals are monoclinic, space group P21/c, with a = 10.290(7), b = 21.199(23), c = 10.719(7) Å, β = 112.00(2)°, and Z = 4. The structure has been solved by the heavy-atom method and refined by block-diagonal least-squares calculations. The agreement factor R obtained for 2607 'observed' reflections is 0.030. The crystal consists of single molecules. The 'characteristic' coordination number of mercury is three, with two sulfur and one arsenic atoms at the apexes of a triangle. The nitrogen atoms of the thiocyanate groups are at 2.67 and 2.74 Å from the adjoining mercury atoms and therefore link the different molecules together.

The coordination of the dimethylthallium ion in the crystal and molecular structure of 1,10-phenanthroline-dimethylthallium (III) perchlorate

1972 ◽  
Vol 331 (1585) ◽  
pp. 161-169 ◽  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Pentagonal Bipyramid ◽  
Equatorial Position ◽  
Polymeric Structure ◽  
X Ray

A single crystal X-ray analysis of the crystal structure of [TlMe 2 1,10-phen]ClO 4 confirms the presence of a bent dimethylthallium group with a C-Tl-C angle of 168.3 (1.5)°. The thallium coordination is best described as a distorted pentagonal bipyramid with one equatorial position vacant. The equatorial bonds are predominantly electrostatic, and the perchlorate ions are bidentate giving rise to a polymeric structure in the crystal.

The crystal structure of nickel(II) dimethyldithiocarbamate

1980 ◽  
Vol 45 (8) ◽  
pp. 2147-2151 ◽  
Author(s):  
Jan Lokaj ◽  
Ján Garaj ◽  
Viktor Kettmann ◽  
Viktor Vrábel
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Special Position ◽  
X Ray ◽  
Triclinic Unit Cell

Crystal and molecular structure of nickel(II) dimethyldithiocarbamate, Ni[S2CN(CH3)2]2 was solved by X-ray structural analysis and refined by the least squares method to R = 0.06 for 1065 reflections. The compound crystallizes in a space group P I and the triclinic unit cell has the dimensions: a = 6.521 (7), b = 6.798 (9), c = 7.633 (4), α = 67.21 (8)°, β = 67.34 (6)° γ =85.59 (9)°. The experimentally observed density is 1.75 g cm-3 and the calculated value for Z = 1 is 1.73 g cm-3. In the structure , the Ni atom occupies a special position in the centre of symmetry and is coordinated by four sulphur atoms in a plane: Ni-S 0.2218 (4) and 0.2198 nm S1-Ni-S2 angle 79.62 (8)°. The ligand S2CNC2 is nearly planar.

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