The X-ray crystal structure of a Corynanthé-type indole compound, C22H29N2O4+Br−, wherein an unprecedented triaxial conformation is preferred

1985 ◽  
Vol 63 (11) ◽  
pp. 2979-2982
Author(s):  
Angèle Chiaroni ◽  
Claude Riche ◽  
David S. Grierson ◽  
Henri-Philippe Husson
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
A Priori ◽  
X Ray ◽  
Indole Compound ◽  
Nmr Data ◽  
C Nmr

On the basis of 1H and 13C nmr data, a conformation was proposed for the Corynanthé type indole compound 8 in which the substituents at C-3 (indole), C-14 (ethyl), and C-15 (malonyl) were all axial. An X-ray crystal study on the HBr salt of 8 confirmed that this a priori unexpected conformation is also preferred in the solid state.

scholarly journals Structural Investigations of C-Nitrosobenzenes. Part 3.1 Solid-state and Solution 13C NMR Studies, and Crystal Structure of E-(4-CIC6H4NO)2

1999 ◽  
Vol 23 (3) ◽  
pp. 202-203
Author(s):  
Daniel A. Fletcher ◽  
Brian G. Gowenlock ◽  
Keith G. Orrell ◽  
David C. Apperley ◽  
Michael B. Hursthouse ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
13C Nmr ◽  
Nmr Studies ◽  
Structural Investigations ◽  
Nmr Data ◽  
C Nmr

Solid-state and solution 13C NMR data for the monomers and dimers of 3- and 4-substituted nitrosobenzenes, and the crystal structure of E-(4-CIC6H4NO)2 are reported.

Solid state stereochemistry of crown ethers: X-ray crystal structure and 13C NMR studies of the LiNCS complex of 1,4,7,11-tetraoxacyclotetradecane

2000 ◽  
Vol 78 (3) ◽  
pp. 316-321
Author(s):  
G W Buchanan ◽  
A B Driega ◽  
G PA Yap
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crown Ether ◽  
13C Nmr ◽  
Title Complex ◽  
Nmr Studies ◽  
Nmr Spectrum ◽  
X Ray ◽  
Large Amplitude Motion ◽  
C Nmr

The title complex is asymmetric in the crystal due to the spatial orientation of the NCS function. The space group has been determined to be P21 with a = 9.496(3), b = 8.736(3), c = 9.676(3) Å, β = 117.859(5)°, and Z = 2. The solid state 13C NMR spectrum is consistent with the lack of symmetry in the crystal and there is little evidence for large amplitude motion in the macrocycle as determined from the dipolar dephased spectrum.Key words: macrocyclic crown ether, lithium complex.

Synthesis, X-ray crystal structure, and solid-state 13C NMR study of tris(9-crown-3)triphenylene

2001 ◽  
Vol 79 (2) ◽  
pp. 195-200 ◽  
Author(s):  
Gerald W Buchanan ◽  
Majid F Rastegar ◽  
Glenn PA Yap
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crown Ether ◽  
Chemical Shifts ◽  
Aromatic Rings ◽  
X Ray ◽  
Nmr Study ◽  
Group A ◽  
C Nmr ◽  
Solid State 13C Nmr

Benzo-9-crown-3 ether trimerizes in the presence of FeCl3 and aqueous H2SO4 to produce tris(9-crown-3)triphenylene in 25.4% yield. This compound crystallizes in the monoclinic P21/c space group: a = 13.759(2) Å, b = 13.318(2) Å, c = 13.399(2) Å, β = 96.883(2)°, with Z = 4. The three 9-crown-3 ether units of the trimer possess different geometries and there is substantial deviation from coplanarity in the three aromatic rings. 13C NMR chemical shifts in the solid state are consistent with this lack of symmetry and are discussed in terms of the X-ray crystal-structure data.Key words: crown ether, trimerization, stereochemistry.

Oxidative coupling of naphtho-9-crown-3 ether: X-ray crystal structure and solution and solid-state NMR analysis of the dimer

2001 ◽  
Vol 79 (10) ◽  
pp. 1505-1510 ◽  
Author(s):  
G W Buchanan ◽  
M F Rastegar ◽  
G PA Yap ◽  
A Moghimi ◽  
M Ghandi
Keyword(s):  
Solid State ◽  
Oxidative Coupling ◽  
Solid State Nmr ◽  
Nmr Analysis ◽  
Oxidative Dimerization ◽  
Nmr Spectrum ◽  
X Ray ◽  
Nmr Data ◽  
Group A ◽  
C Nmr

Treatment of naphtho-9-crown-3 ether with FeCl3 and aqueous H2SO4 generates bis-naphtho-9-crown-3 ether in ca. 30% yield. This compound crystallizes in the monoclinic P21/n space group; a = 9.2004(9), b = 18.0868(17), and c = 13.2078(13) Å, β = 97.799(2)° and Z = 4. 1H and 13C NMR data have been obtained in solution, and the solid-state 13C NMR spectrum is included for comparison. A chemical shift range of ca. 12 ppm has been found for the oxygenated aliphatic carbons in the solid state, in contrast to the 3 ppm range in the solution 13C NMR spectrum. These results are discussed in terms of the torsional environments of the carbon sites in the crystal structure.Key words: crown ether, stereochemistry, oxidative dimerization.

Reactivity of diosmacycles: complementary syntheses and structure Of [(µ-η1,η2-CHCH2)OS2(CO)8][BF4]

1995 ◽  
Vol 73 (7) ◽  
pp. 1003-1009 ◽  
Author(s):  
R.G. Ball ◽  
Gong Y. Kiel ◽  
William A. Kiel ◽  
Josef Takats ◽  
Friedrich-Wilhelm Grevels
Keyword(s):  
Solid State ◽  
Traditional View ◽  
Cationic Complex ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Excellent Yield ◽  
Nmr Data ◽  
Hydride Abstraction ◽  
C Nmr

The vinyl-bridged cationic complex, [(µ-CHCH2)Os2(CO)8][BF4] (3), is obtained readily and in excellent yield either via hydride abstraction from octacarbonyl diosmacyclobutane, (µ-η1,η1-CH2CH2)Os2(CO)8 (1), or via protonation of octacarbonyl diosmacyclobutene, (µ-η1,η1-CHCH)Os2(CO)8 (2). It is argued that the 1H and 13C NMR data of complex 3 are consistent with the traditional view of bonding in µ-alkenyl complexes, involving substantial σ,π donation. The solid state X-ray structure of the complex lends support for this formulation. Complex 3 crystallizes in the orthorhombic space group, P212121, with a = 12.128(2) Å, b = 14.151(3) Å, c = 9.248(3) Å, V = 1587 Å3, and Z = 4. The final R and Rw values are 0.032 and 0.038, respectively. Keywords: µ-vinyl, diosmacycles, X-ray structure.

Dithiocarbonate and Trithiocarbonate Complexes of Palladium(II); Crystal Structure of Pd(Ph3P)2(CS2O)· CH2Cl2

1983 ◽  
Vol 38 (4) ◽  
pp. 449-453 ◽  
Author(s):  
Peter G. Jones ◽  
George M. Sheldrick ◽  
Rafael Usón ◽  
Juan Forniés ◽  
Miguel A. Usón
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Phosphine Ligand ◽  
X Ray ◽  
Nmr Data

Abstract Di-and trithiocarbonate complexes of palladium(II) have been prepared by the action of O2 or S8 on PdL2(η2 -CS2) in the presence of excess L (L = phosphine ligand). 31P NMR data for Pd(PPh3)2(CS2O) are consistent with the presence in solution of both S̱,S̱ and S̱,O̱ coordinated dithiocarbonate. An X-ray crystal structure of the dichloromethane solvate [P1̄, a = 1103.6(4), b = 1343.4(5), c = 1368.5(5) pm, α = 94.77(3), β = 94.67(3), γ = 113.64(3)°, Z = 2, R = 0.059] suggests that an equivalent disorder may occur in the solid state.

Tetrakis-pentamethylcyclopentadienyl-cyclotetrastiban (PcpSb)4 : Synthese, Molekül-und Kristallstruktur / Tetrakis-pentamethylcyclopentadienyl-cyclotetrastibane (PcpSb)4 : Synthesis, Molecular and Crystal Structure

1988 ◽  
Vol 43 (6) ◽  
pp. 744-748 ◽  
Author(s):  
Theo F. Berlitz ◽  
Heike Sinning ◽  
Jörg Lorberth ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Mass Spectra ◽  
High Yield ◽  
Crystal Data ◽  
State Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tetrameric Structure ◽  
C Nmr

AbstractReaction of SbCl3 with KPcp (Pep = pentamethylcyclopentadienyl) in etheral solution at -78 °C affords dimeric pentamethylcyclopentadiene and orange-red (PcpSb)4 in high yield. 1H, 13 C NMR, IR, UV and mass spectra are reported. The tetrameric structure was found by a crystal structure determination carried out with X-ray diffraction data collected at -50 °C (928 independent observed reflexions. R = 0.055). Crystal data: tetragonal, space group I41/amd, a = 2400.0(5), c = 781.7(5) pm, Z = 4. The (PcpSb)4 molecules have a non-planar Sb4 ring with Sb -Sb bond lengths of 285.6(1) pm, one η1-Pcp ring is attached to each Sb atom. Contrary to the solid state structure, monomeric molecules are found in benzene and hexane solutions.

Structural characterization of Cd3(O3PC2H4CO2)2·2H2O from in-house X-ray powder data and NMR

2005 ◽  
Vol 61 (6) ◽  
pp. 669-674 ◽  
Author(s):  
Naima Bestaoui ◽  
Xiang Ouyang ◽  
Florence Fredoueil ◽  
Bruno Bujoli ◽  
Abraham Clearfield
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Characterization ◽  
Title Compound ◽  
Solid State Nmr ◽  
Hydrothermal Reaction ◽  
X Ray ◽  
Space Groups ◽  
Nmr Data

The title compound poly[[bis(μ-2-carboxylatoethylphosphonato)cadmium] dihydrate], Cd3(O3PC2H4CO2)2·2H2O, was prepared by a hydrothermal reaction and its crystal structure determined from in-house powder data. The structure was solved in both P21/c and P21 space groups. The refinement converged with Rp = 0.1046, R wp = 0.1378 and Rf = 0.0763 in P21/c. However, the solid-state NMR data could not be explained. The structure was then solved in P21 and the refinement converged with Rp = 0.0750, R wp = 0.1022 and Rf = 0.0409 and satisfied the NMR requirements.

scholarly journals Studies of Dihydropyridines by X-Ray Diffraction and Solid State 13C NMR

2007 ◽  
Vol 62 (4) ◽  
pp. 549-555 ◽  
Author(s):  
Martha S. Morales-Ríos ◽  
Antonio Martínez-Richa ◽  
Zurisaddai Hernández-Gallegos ◽  
Angelina Hernández-Barragán ◽  
Ricardo Vera-Graziano ◽  
...  
Keyword(s):  
Solid State ◽  
Phenyl Ring ◽  
Chemical Shifts ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Substitution Pattern ◽  
Trans Orientation ◽  
X Ray ◽  
Nmr Data ◽  
C Nmr

Fourteen dimethyl 4-aryl-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylates (DHPs) were evaluated by means of single crystal X-ray diffraction in order to investigate the effects of the structure in the crystals on the solid state 13C NMR chemical shifts. These include the analysis of three DHPs containing two molecules per asymmetric unit. The chiral rotamer unit generated by the s-cis/s-trans orientation of the carbonyl groups, as well as by rotation of the 4-phenyl ring out of the bisecting plane containing the N1, C4, C7 atoms, resulted in a significant magnetic non-equivalence for the C2-CH3/C6-CH3 and the COOCH3 pairs of signals. The solid state 13C NMR data reveal that the substitution pattern of the phenyl ring has a marked effect on the extent to which the signals of the carbonyl carbon atoms and those of C-2/C-6 peaks are split.

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