Carbon-13 NMR and x-ray structure determination of 1-(arylazo)-2-naphthols. Intramolecular proton transfer between nitrogen and oxygen atoms in the solid state

1989 ◽  
Vol 111 (15) ◽  
pp. 5525-5532 ◽  
Author(s):  
Alejandro C. Olivieri ◽  
Roxy B. Wilson ◽  
Iain C. Paul ◽  
David Y. Curtin
Keyword(s):  
Solid State ◽  
Proton Transfer ◽  
Structure Determination ◽  
Intramolecular Proton Transfer ◽  
X Ray ◽  
Oxygen Atoms

Structural Properties of a Dimeric Phenylcyanamidocopper(I) Complex, [{Cu(PPh3)2(C6H5NCN)}2]

2000 ◽  
Vol 53 (12) ◽  
pp. 971 ◽  
Author(s):  
Eric W. Ainscough ◽  
Andrew M. Brodie ◽  
Peter C. Healy ◽  
Joyce M. Waters
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Properties ◽  
Structure Determination ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
X Ray ◽  
Angle Spinning

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

Die Kristallstrukturen von Magnesiumdibromid-Diglym-Addukten / Crystal Structures of Magnesium Dibromide Diglyme Adducts

1994 ◽  
Vol 49 (10) ◽  
pp. 1448-1452 ◽  
Author(s):  
Nils Metzler ◽  
Heinrich Nöth ◽  
Martin Schmidt ◽  
Andreas Treitl
Keyword(s):  
Crystal Structures ◽  
Structure Determination ◽  
Mononuclear Complex ◽  
Common Edge ◽  
X Ray ◽  
Ether Solution ◽  
In Cis ◽  
Tetrahydrofuran Solution ◽  
Oxygen Atoms

Abstract(MgBr2·diglyme)2 (1) crystallized in low yield from an ether solution of the Grignard compound mesMgBr (mes = mesityl) on adding diglyme. It is more conveniently prepared from an ether solution of MgBr2 by addition of diglyme. The mixed solvate MgBr2·diglyme thf (2) crystallized from a diglyme/tetrahydrofuran solution of 1 after addition of ether. An X-ray structure determination of 1 reveals dimeric units containing hexacoordinated Mg atoms surrounded by three oxygen atoms and three bromide atoms, with each kind of atoms arranged in a meridional fashion. The two octahedral MgO3Br3 units share a common edge with two Br atoms. Compound 2 is a mononuclear complex with the Br atoms in cis-position. The diglyme ligand occupies meridional positions of a distorted MgBr2O4 octahedron.

scholarly journals Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

2013 ◽  
Vol 117 (23) ◽  
pp. 12258-12265 ◽  
Author(s):  
Dmytro V. Dudenko ◽  
P. Andrew Williams ◽  
Colan E. Hughes ◽  
Oleg N. Antzutkin ◽  
Sitaram P. Velaga ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Molecular Solids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy

scholarly journals Metallation of Isatin (2,3-Indolinedione). X-Ray Structure and Solution Behavior of Bis(Isatinato)Mercury(II)

1995 ◽  
Vol 2 (2) ◽  
pp. 81-90 ◽  
Author(s):  
Angel Garcia-Raso ◽  
Juan J. Fiol ◽  
Elies Molins ◽  
Antonia M. Calafat ◽  
Patricia A. Marzilli ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Metal Complex ◽  
Bond Length ◽  
Spectral Data ◽  
Structure Determination ◽  
Monoclinic System ◽  
Heterocyclic Nitrogen ◽  
X Ray

The first X-ray structure of an isatin (2,3-indolinedione, isaH) metal complex, bis(isatinato)memury(II) (C16H8N2O4Hg) (1), was determined. (1) was obtained from the reaction of isaH with mercury(II) acetate in methanol. Analogously, treatment of sodium saccharinate and mercury(II) acetate in methanol yielded Hg(saccharinato)2•0.5CH3OH (3). (1) crystallizes in the monoclinic system, space group P21/a with a = 7.299(1) Å, b = 8.192(1) Å, c = 11.601(1) Å , β = 105.82(1)°, V = 667.4 Å3, Z = 2, Dcalc = 2.452 g cm−3, MoKα radiation(λ = 0.71073 Å), μ = 115.5 cm-1, F(000) = 460, 21(1) °C. The structure was refined on the basis of 2023 observed reflections to R= 0.044. The two deprotonated, non coplanar isa ligands are trans to each other in a head to tail orientation and bound to the Hg through the nitrogen in a linear N-Hg-N arrangement. The Hg atom is at the center of symmetry of the complex and displaced by 0.62 Å from the two planes of the isa ligands (τ Hg-N1-C2-O2= -16°). The Hg-N bond length is 2.015 Å. Noπ-aryl-memury(ll)-π-aryl stacking interaction was observed either in the solid state or in the solution state. The IR, electronic, and H1 and C13NMR spectral data of (1) and (3) suggest binding of the memury to the heterocyclic nitrogen, in agreement with the crystal structure determination of (1).

Potential Anticancer Agents, XI. X-Ray Structure Determination of Acantholide [1]

1979 ◽  
Vol 34 (9-10) ◽  
pp. 677-682 ◽  
Author(s):  
H. Lotter ◽  
H. Wagner ◽  
A. A. Saleh ◽  
G. A. Cordell ◽  
N. R. Famsworth
Keyword(s):  
Solid State ◽  
Antitumor Activity ◽  
Sesquiterpene Lactone ◽  
Anticancer Agents ◽  
Structure Determination ◽  
Direct Methods ◽  
X Ray ◽  
Activity Evaluation ◽  
Nmr Data

Abstract The X-ray structure of acantholide, a melampolide sesquiterpene lactone from Acanthosper­mum glabratum (D C .) Willd. was determined by the aid of direct methods. The compound was cy­totoxic but displayed no antitumor activity. Evaluation of the X-ray and NMR data indicated that the same conformation exists in the solid state as in solution.

Sign in / Sign up

Export Citation Format

Share Document