A new type of crown ether. III. Triethylene glycolic diester of naphthalene dithioglycolic acid

1983 ◽  
Vol 61 (8) ◽  
pp. 1756-1759
Author(s):  
Lidia Prajer-Janczewski ◽  
Krystyna Rudolk ◽  
Tadeusz Lis ◽  
Marian Janczewski ◽  
Janina Biskup
Keyword(s):  
Mass Spectrometry ◽  
Crown Ether ◽  
Crystalline State ◽  
Structural Investigation ◽  
X Ray ◽  
New Type ◽  
C Nmr

The structure of 2,7-(11,22-diono-12, 15,18.21-tetroxa-9,24-dithia)-hexadecylene-naphthalene was investigated by 1H and 13C nmr and mass spectrometry. An X-ray structural investigation indicated the dissymmetric ansa structure of this compound in the crystalline state.

Syntheses, Spectroscopy And Crystal Structures Of (R)-N-(1-Aryl-Ethyl)Salicylaldimines And [Rh{(R)-N-(1-Aryl-Ethyl)Salicylaldiminato}(η4-Cod)] Complexes

2007 ◽  
Vol 62 (6) ◽  
pp. 807-817 ◽  
Author(s):  
Mohammed Enamullah ◽  
A.K.M. Royhan Uddin ◽  
Anne-Christine Chamayou ◽  
Christoph Janiak
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Schiff Bases ◽  
Structure Determination ◽  
Chelate Ring ◽  
Optical Rotation ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Chiral Schiff Base ◽  
C Nmr

Condensation of salicylaldehyde with enantiopure (R)-(1-aryl-ethyl)amines yields the enantiopure Schiff bases (R)-N-(1-aryl-ethyl)salicylaldimine (HSB*; aryl = phenyl, 2-methoxyphenyl, 3- methoxyphenyl, 4-methoxyphenyl (4), 4-bromophenyl (5), 2-naphthyl). These Schiff bases readily react with dinuclear (acetato)(η4-cycloocta-1,5-diene)rhodium(I), [Rh(μ-O2CMe)(η4-cod)]2, to afford the mononuclear complexes, cyclooctadiene-((R)-N-(1-aryl-ethyl)salicylaldiminato-κ2N,O)- rhodium(I), [Rh(SB∗)(η4-cod)] (SB* = deprotonated chiral Schiff base = salicylaldiminate; aryl = phenyl (7), 2-methoxyphenyl, 4-methoxyphenyl, 4-bromophenyl, 2-naphthyl). The complexes have been characterized by IR, UV/vis, 1H/13C NMR and mass spectrometry, optical rotation as well as by single-crystal X-ray structure determination for 4, 5 and 7. The structure of 5 shows C-Br· · ·π contacts. Compound 7 is only the second example of a Rh(η4-cod) complex with a six-membered Rh-N,O-chelate ring

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.

scholarly journals Simple Methylcadmium Alkoxides

2007 ◽  
Vol 62 (10) ◽  
pp. 1339-1342 ◽  
Author(s):  
Surajit Jana ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Molecular Formula ◽  
Equimolar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Elemental Analyses ◽  
Solid State Structures ◽  
Structural Aspects ◽  
C Nmr

The reaction of dimethylcadmium with alcohols R-OH in equimolar ratio leads to the formation of tetrameric methylcadmium alkoxides with molecular formula [(MeCd)4 (OR)4] [R = Me (1), Et (2) and iPr (3)]. These compounds have been characterised by 1H, 13C NMR and IR spectroscopy, by mass spectrometry, elemental analyses and by X-ray crystallography (for 2 and 3). The solid state structures show distorted cubane-type aggregates with Cd4O4 cores. The structural aspects and the spectroscopic characterisations of these compounds are discussed.

Sur une nouvelle méthode de synthèse de δ-lactones cyclopenténiques

1986 ◽  
Vol 64 (4) ◽  
pp. 831-836 ◽  
Author(s):  
Jean Claude Caille ◽  
Michel Farnier ◽  
Roger Guilard ◽  
André Aubry ◽  
Claude Lecomte
Keyword(s):  
Mass Spectrometry ◽  
Carbon Atom ◽  
X Ray ◽  
Nmr Data ◽  
C Nmr

Synthesis of two cyclopentenic δ-lactones, 1,3,4,4a,5,6-hexahydrocyclopenta[c]pyran-1-one and its analogue possessing a cyclopentenyl group bonded to the carbon atom 4a is described, starting from the cyclopentanone or cyclopentylidene cyclopentanone. The remarkable reactivity of the tosylhydrazones allows transformation of these compounds into substituted cyclopentenes, which lead to δ-lactones by cyclization. The conditions of cyclization depend on the nature of the cyclopentanone. The structure of the two δ-lactones is established by 1H and 13C nmr data, mass spectrometry, and, in one case, by X-ray analysis.

Crystal structure of 3-chlorobenzo[b]thiophene-2-carbonyl chloride

2009 ◽  
Vol 2009 (7) ◽  
pp. 437-439 ◽  
Author(s):  
Sara Tarighi ◽  
Alireza Abbasi ◽  
Sara Zamanian ◽  
Alireza Badiei ◽  
Mahmood Ghoranneviss
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Cinnamic Acid ◽  
Thionyl Chloride ◽  
Structure Determination ◽  
X Ray ◽  
Packing Structure ◽  
H Nmr ◽  
Carbonyl Chloride ◽  
C Nmr

3-Chlorobenzo[b]thiophene-2-carbonyl chloride was synthesised from cinnamic acid and thionyl chloride. The single crystal X-ray structure determination confirmed the earlier proposed structure and the product was further characterised by 1H NMR, 13C NMR and mass spectrometry. The X-ray structure determination revealed two sets of symmetry related molecules along the b-axis that are loosely connected by relatively weak CH…π ( 3.626, 3.628 Å) interactions, giving rise to two infinite chains. The packing structure is dominated by Van der Waals forces between these chains. No significant π–π interactions are found in the crystal structure.

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.

Synthesis and Single Crystal X-Ray Structure of Ethyl 2-(1,3-Benzoxazol- 2-yl)-5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate

2007 ◽  
Vol 62 (5) ◽  
pp. 705-710 ◽  
Author(s):  
Ali Souldozi ◽  
Jabbar Khalafy ◽  
Ahmad Poursattar Marjani ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Structure Determination ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
X Ray ◽  
C Nmr

Abstract Ethyl 5-oxo-3-(4-toluidino)-2,5-dihydro-4-isoxazolecarboxylate was prepared from the reaction of diethyl 2-(4-toluidinocarbothioyl)malonate with hydroxylamine. Its reaction with 2- chlorobenzoxazole gave the corresponding N-substituted isoxazolone. The structure of the final product 4 was confirmed by IR, 1H and 13C NMR spectroscopy and mass spectrometry, and by X-ray single crystal structure determination.

The structures of indoiyl(alkoxy)carbenium tetrafluoroborates: a new class of highly stabilized carbenium ions

1989 ◽  
Vol 44 (6) ◽  
pp. 659-665 ◽  
Author(s):  
Ulf Pindur ◽  
Ludwig Pfeuffer ◽  
Camran Flo ◽  
Werner Massa ◽  
Karin Seitz
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Crystalline State ◽  
X Ray Diffraction ◽  
Carbenium Ions ◽  
X Ray ◽  
Axial Chirality ◽  
New Class ◽  
Charge Distributions ◽  
C Nmr

The conformations of and charge distributions in indolyl(alkoxy)carbenium tetrafluoroborates 2, a new class of highly stabilized carbenium ions, were investigated by 1H and 13C NMR spectroscopy and the crystal structure of indol-3-yl(methoxy)phenylcarbenium tetrafluoroborate (2e) was determined by X-ray diffraction methods. The phenyl-substituted cation of 2e exhibits axial chirality in the crystalline state

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