Crystal and Molecular Structure of the Synthetic Intermediate, 2-Bromo-3-methoxy-5-hydroxy-5,6,7,8,9,10,13,14-octahydro-8-methyl-10,13-N-acetylaminomethano-phenanthrene, C19H24O3NBr

1973 ◽  
Vol 51 (16) ◽  
pp. 2637-2638 ◽  
Author(s):  
H. Lynton ◽  
P. Y. Siew
Keyword(s):  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Full Matrix ◽  
Cell Dimensions ◽  
Ring Nitrogen ◽  
Unit Cell Dimensions ◽  
Synthetic Intermediate ◽  
Heavy Atom Method

Crystals of the synthetic intermediate, 2-bromo-3-methoxy-5-hydroxy-5,6,7,8,9,10,13,14-octahydro-8-methyl-10,13-N-acetyl aminomethano-phenanthrene, C19H24O3NBr, are monoclinic, space group P21/n, unit cell dimensions a = 10.62(1), b = 14.47(2), c = 23.88(2) Å, β = 99.4(2)°, z = 8 with two molecules in the asymmetric unit. The structure was solved by the heavy atom method and refined by full matrix least squares to R = 0.096 for 2120 observed reflections. The conformation was found to be cis at the junction between rings A and B making further cyclization to obtain an A ring nitrogen bridge not possible.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

Crystal and molecular structure of the m-bromobenzoate derivative of bisnorquassin

1970 ◽  
Vol 48 (2) ◽  
pp. 307-311 ◽  
Author(s):  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Unit Cell ◽  
Anisotropic Temperature ◽  
Cell Dimensions ◽  
Final Agreement ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Atomic Parameters

The molecular structure of the m-bromobenzoate derivative of bisnorquassin, C27H27O7Br, has been determined by the heavy atom method. The compound crystallizes in the orthorhombic system, space group P212121, with unit cell dimensions a = 20.09 ± 0.02 Å, b = 14.63 ± 0.02 Å, c = 8.06 + 0.01 Å and 4 molecules in the unit cell. Final atomic parameters have been obtained from a blockdiagonal least-squares refinement using anisotropic temperature parameters. The final agreement residual for 1665 observed reflections is R = 0.107.The structure of bisnorquassin previously proposed by Findlay and Cropp, on the basis of spectroscopic and chemical evidence, is shown to be essentially correct.

Crystal structure of diethylammonium tetrachloro(p-phenoxyphenyl)tellurate

1984 ◽  
Vol 62 (1) ◽  
pp. 32-35 ◽  
Author(s):  
Raj K. Chadha ◽  
John E. Drake ◽  
Masood A. Khan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Heavy Atom ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Secondary Interaction ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Interionic Hydrogen

The crystal structure of diethylammonium tetrachloro(p-phenoxyphenyl)tellurate has been determined by the heavy atom method. The crystals are monoclinic, space group C2/c, with unit cell dimensions a = 19.675(5), b = 7.634(3), c = 28.716(6) Å, β = 105.58(2)°, and Z = 8. For 2636 "observed" reflections (I > 3σ(I)), R = 0.030. The primary geometry about tellurium is based on a square pyramid with a secondary interaction on the vacant side of the tellurium coordination octahedron. The ions are apparently linked by weak interionic hydrogen bonding along the crystallographic b axis.

scholarly journals Crystal and Molecular Structure of the 1:1 Complex of Chloral Hydrate and 7-Bromo-2,3-dihydro-1-methyl-5-phenyl-1,4-benzodiazepin-2-one

1971 ◽  
Vol 49 (20) ◽  
pp. 3401-3404 ◽  
Author(s):  
R. F. Dunphy ◽  
H. Lynton
Keyword(s):  
Chloral Hydrate ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Unit Cell ◽  
Orthorhombic System ◽  
Cell Dimensions ◽  
Final Agreement ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Atomic Parameters

The structure of a 1:1 complex of chloral hydrate and 7-bromo-2,3-dihydro-1-methyl-5-phenyl-1,4-benzodiazepin-2-one has been determined by the heavy atom method. The complex crystallizes in the orthorhombic system, space group Pbca, with unit cell dimensions a = 13.45(1), b = 26.74(2), c = 11.23(1) Å and 8 molecules in the unit cell. The 1:1 complex of chloral hydrate and diazepam, 7-chloro-2,3-dihydro-1-methyl-5-phenyl-1,4-benzodiazepin-2-one, is isomorphous with the above compound and has unit cell dimensions a = 13.43(1), b = 26.60(2), c = 11.20(1) Å. The final atomic parameters have been obtained from a block-diagonal least squares refinement using anisotropic thermal parameters. The final agreement residual for 575 observed reflections is R = 0.079.The structure consists of chains of chloral hydrate and Br-diazepam molecules linked by hydrogen bonds.

Crystal and Molecular Structure of 2-Bromo-11-ethyl-5,9-dimethoxytetracyclo[5.4.1.14,12•18,11]tetradecan-3-one, C18H27BrO3

1971 ◽  
Vol 49 (15) ◽  
pp. 2497-2500 ◽  
Author(s):  
R. F. Dunphy ◽  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Unit Cell ◽  
Monoclinic System ◽  
Cell Dimensions ◽  
Final Agreement ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Atomic Parameters

The molecular structure of 2-bromo-11-ethyl-5,9-dimethoxytetracyclo[5.4.1.14,12•18,11]tetradecan-3-one, C18H27BrO3, synthesized in an attempt to develop a method of conversion from an advanced relay compound to the alkaloid delphinine, has been determined by the heavy atom method. The compound crystallizes in the monoclinic system, space group P21/c, with unit cell dimensions a = 9.684(9), b = 13.481(15), c = 12.988(14) Å, β = 99.47(7)°, and four molecules in the unit cell. The atomic parameters were refined by block-diagonal least squares using anisotropic thermal parameters. The hydrogen atom positions were established but the parameters were not refined. The final agreement residual for 816 observed reflections is R = 0.044.The stereochemistry of the compound was found to be unsuitable for the delphinine synthesis.

The Molecular Conformation of 1e,2a,6e-Trimethyl-4e-phenyl-4a-acetoxypiperidine Hydrobomide in the Crystalline State

1973 ◽  
Vol 51 (10) ◽  
pp. 1535-1542 ◽  
Author(s):  
K. Hayakawa ◽  
M. N. G. James
Keyword(s):  
Molecular Conformation ◽  
Heavy Atom ◽  
Chair Conformation ◽  
Piperidine Ring ◽  
Monoclinic Space Group ◽  
Narcotic Analgesics ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
The Ideal

The title compound represents one analog of the synthetic 4-phenylpiperidine narcotic analgesics. The crystal structure was determined by the heavy-atom method from data collected on an automated diffractometer. The crystals are monoclinic, space group P21/c, with unit cell dimensions a = 11.833 Å, b = 11.551 Å, c = 14.659 Å and β = 121° 9′. The final residual, R, was 0.056. The stereochemistry of the substituents on the piperidine ring as deduced by this structural determination (1e,2a,6e-trimethyl-4e-phenyl-4a-acetoxypiperidine) confirms the p.m.r. results on the alcohol precursor as trans 2-Me/6-Me and trans 2-Me/4-Ph. There is a normal length N—H … Br hydrogen bond of 3.234 Å; most intramolecular bond lengths and angles are within the expected ranges but some distortion of the ideal chair conformation of the piperidine ring occurs.

Determination of the structure of bis(propyldithiocarbamate)nickel(II)

1990 ◽  
Vol 55 (4) ◽  
pp. 1010-1014 ◽  
Author(s):  
Jiří Kameníček ◽  
Richard Pastorek ◽  
František Březina ◽  
Bohumil Kratochvíl ◽  
Zdeněk Trávníček
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Planar Configuration ◽  
Compound C ◽  
Heavy Atom Method

The crystal and molecular structure of the title compound (C8H16N2NiS4) was solved by the heavy atom method and the structure was refined anisotropically to a final R factor of R = 0.029 (wR = 0.037) for 715 observed reflections. The crystal is monoclinic, space group P21/c with a = 948.3(2), b = 776.9(2), c = 1 167.4(2) pm, β = 125.14(2)°, Z = 2. The molecule contains two four-membered NiSCS rings of approximately planar configuration with the Ni atom situated at a centre of symmetry. The molecules are arranged in chains along the c-axis of the unit cell.

Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

The crystal and molecular structure of thiamine iodide hydroiodide

1976 ◽  
Vol 54 (19) ◽  
pp. 3001-3006 ◽  
Author(s):  
William Edward Lee ◽  
Mary Frances Richardson
Keyword(s):  
Heavy Atom ◽  
Pyrimidine Ring ◽  
Side Chain ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Iodide Ions ◽  
Cell Parameters ◽  
Weak Hydrogen Bonds ◽  
Ring Nitrogen ◽  
Heavy Atom Method

The X-ray crystal structure of thiamine iodide hydroiodide, C12H18N4OSI2, has been determined. The unit cell parameters are: a = 13.835(7), b = 7.442(4), c = 20.243(9) Å, β = 120.52(7)°, monoclinic space group P21/c, Z = 4. A total of 1445 reflections having F2 > 2σ(F2), 2θ < 40° were collected on a Picker 4-circle diffractometer with MoKα radiation by the 2θ scan technique. The structure was solved by the heavy-atom method. The iodide and sulphur atoms were refined anisotropically; only positional parameters were refined for the hydrogen atoms. Successive full-matrix least-squares refinements yielded an unweighted R-factor of 0.054. The pyrimidine ring is protonated on the ring nitrogen opposite the amino group. The relative disposition of the pyrimidine and thiazolium rings is similar to that observed in most other thiamine structures. The β-hydroxyethyl side chain of the thiazolium ring is folded in such a way that there is a short S … O contact, 2.97 Å in length. The iodide ions are involved in a number of weak hydrogen bonds.

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.

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