Complete analysis of the 1H nmr spectrum of tetrahydrothiophene

1980 ◽  
Vol 58 (22) ◽  
pp. 2340-2348 ◽  
Author(s):  
Angel Luis Esteban ◽  
Ernesto Díez
Keyword(s):  
Potential Energy ◽  
1H Nmr ◽  
Time Scale ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Karplus Relationship ◽  
The One

The 1H nmr spectrum of tetrahydrothiophene has been analyzed. The best set of coupling values (Hz) is: [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text] (A and B refer to α-and β-protons and c and t denote respectively the same and opposite sides of the ring). The variances observed between the values of this set and those reported by Lozach etal., particularly the interchange of the [Formula: see text] and [Formula: see text] couplings, are discussed and it is concluded that our set is the one that reproduces the most fine details of the spectrum profile. The proposed set has been selected as being the most physically meaningful, from amongst 24 equally valid sets of couplings, on the basis of a better agreement with the [Formula: see text] and [Formula: see text] values calculated from a Karplus relationship and from the INDO-FPT method respectively. In these calculations it was assumed that the molecule was interconverting rapidly (on the nmr time scale) between two puckered conformations with C2 symmetry. A detailed discussion of the dependence of the couplings on the height of the pseudorotational barrier and on the temperature indicate that the minimum values of the potential energy correspond to these conformations.

21,22-Disubstituted 18α,19βH-Ursane Derivatives with Oxabicyclooctane System in Ring E

1993 ◽  
Vol 58 (1) ◽  
pp. 173-190 ◽  
Author(s):  
Eva Klinotová ◽  
Jiří Klinot ◽  
Václav Křeček ◽  
Miloš Buděšínský ◽  
Bohumil Máca
Keyword(s):  
Spectral Data ◽  
Spin Systems ◽  
Coupling Constants ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
Proton Proton ◽  
H Nmr ◽  
Proton Coupling ◽  
C Nmr

Reaction of 3β-acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) and 20β,28-epoxy-21,22-dioxo-19α,19βH-ursan-3β-yl acetate (IIIb) with diazomethane afforded derivatives XII-XIV with spiroepoxide group in position 21 or 22, which were further converted into hydroxy derivatives XV and XVII. Ethylene ketals VIII-X were also prepared. In connection with the determination of position and configuration of the functional groups at C(21) and C(22), the 1H and 13C NMR spectral data of the prepared compounds are discussed. Complete analysis of two four-spin systems in the 1H NMR spectrum of bisethylenedioxy derivative Xb led to the proton-proton coupling constants from which the structure with two 1,4-dioxane rings condensed with ring E, and their conformation, was derived.

scholarly journals Complete Analysis of the 100 MHz 1H NMR Spectrum of Triphenylphosphine.

1974 ◽  
Vol 28a ◽  
pp. 249-250 ◽  
Author(s):  
S. Sørensen ◽  
H. J. Jakobsen ◽  
F. Lindeløv ◽  
Terje Østvold ◽  
Alf Bjørseth ◽  
...  
Keyword(s):  
1H Nmr ◽  
Complete Analysis ◽  
Nmr Spectrum

scholarly journals Beiträge zur Chemie des Phosphors, 204. Zur Existenz eines Triphosphacyclobutenid-Ions P3CH2Ɵ / Contributions to the Chemistry of Phosphorus, 204. On the Existence of a Triphosphacyclobutenide Ion P3CH2e

1990 ◽  
Vol 45 (8) ◽  
pp. 1139-1142 ◽  
Author(s):  
Marianne Baudler ◽  
Josef Hahn
Keyword(s):  
White Phosphorus ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Low Field

The structure of the reaction product of white phosphorus and sodium in diglyme which exhibits a low field AB2 system in the 31P{1H} NMR spectrum [4] has been reexamined. According to the results of a complete analysis of its proton coupled 31P NMR spectrum (ABB′XX′ system), the compound is the hitherto unknown 1,2,3-triphosphacyclopentadienide ion P3(CH)2⊖ (4), and not the triphosphacyclobutenide ion P3CH2⊖(3) previously assumed [4]. The parameters of the Ρ,Η-coupled 31P NMR spectrum of the tetraphosphacyclopentadienide ion P4CH⊖ (2) have also been calculated.

Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

Beiträge zur Chemie des Phosphors, 234 [1,2] Lithium-tetrahydrogencyclopentaphosphid: Synthese, Struktur und Reaktionen / Contributions to the Chemistry of Phosphorus, 234 [1,2] Lithium Tetrahydrogen Cyclopentaphosphide: Synthesis, Structure and Reactions

1995 ◽  
Vol 50 (5) ◽  
pp. 786-790 ◽  
Author(s):  
Marianne Baudler ◽  
Rudolf Heumüller ◽  
Wolfgang Faber
Keyword(s):  
Low Temperature ◽  
Complete Analysis ◽  
Lemon Yellow ◽  
Compound I ◽  
Polar Solvents ◽  
Open Chain ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Nmr Parameters ◽  
Reaction Compound

Abstract Lithium tetrahydrogen cyclopentaphosphide. LiH4P5 (I). has been obtained by metalation of P2H4 at -78 °C with either n-BuLi or LiPH2 in polar solvents. Upon suitable performance of the reaction, compound I can be isolated at low temperature as a lemon-yellow solvent adduct. The structure as the monolithium salt of (PH)5 was confirmed by a complete analysis of the 31P{1H}-NMR spectrum. On warming above -35 °C, disproportionation occurs yield­ing Li2HP7. P2H4. and PH3. The reaction with n-BuLi produces the open-chain phosphides LiH4P3. LiH3P2, and LiPH2. The NMR parameters of LiH3P2 and LiH4P3 are reported. Reac­tion of 1 with P2H4 gives rise to the bicyclic and polycyclic phosphides LiH4P7, LiH5P8 and Li2H2P14, respectively.

Darstellung, 11B-, 13C-, 1H-NMR-Spektren und Schwingungsspektren von 1,2-Xylylen-pentahydro-closo-hexaborat,cis-[B6H5(CH2)2C6H4]- , sowie Kristallstrukturen von cis-[P(C6H5)4][B6H5(CH2)2C6H4] und cis-[(n-C4H9)4N][B6H5(CH2)2C6H4] / Preparation, 11B, 13C, 1H NMR Spectra and Vibrational Spectra of 1,2-Xylylene-pentahydro-closo-hexaborate, cis-[B6H5(CH2)2C6H4]-, and the Crystal Structures of cis-[P(C6H5)4][B6H5(CH2)2C6H4] and cis-[(n-C4H9)4N ][B6H5(CH2)2C6H4]

1996 ◽  
Vol 51 (5) ◽  
pp. 691-697 ◽  
Author(s):  
W. Lübbe ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Diethylaminoethyl Cellulose

By reaction of [B6H6]2- with ω,ω′-dibromo-o-xylene in acetonitrile the 1,2-xylylenepentahydro-closo-hexaborat, cis-[B6H5(CH2)2C6H4]- , is formed. The new ansa compound has been separated from excess [B6H6]2- and other reaction products by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of cis-[P(C6H5)4][B6H5(CH2)2C6H4] (I) and as-[(n-C4H9)4N][B6H5(CH2)2C6H4] (II) have been determined by single crystal X-ray diffraction analysis: I is monoclinic, space group P 21/n with a = 13.715(5), b = 11.118(1) and c = 19.702(2) Å, β = 103.47(2)°; II is orthorhombic with a = 10.204(7), b = 13.352(4) and c = 20.824(8) Å. The 11B NMR spectrum confirms the structure with a hetero disubstituted octahedral B6 cage with local C2v symmetry. The 13C and 1H NMR spectra have been assigned in term of such a configuration. The IR and Raman spectra exhibit characteristic CH, BH, BC, B6 and arene vibrations.

Synthese, Kristallstruktur und 1H-NMR-Spektrum des vierkernigen Komplexes [{LTi(OCH3)}2(μ-O)4{Ti(acac)2}2](C104)2·2 H2O / Synthesis, Crystal Structure and 1H NMR Spectrum of the Tetranuclear Complex [{ LTi(OCH3)}2(μ-O)4{Ti(acac)2})2](C104)2·2 H2O

1992 ◽  
Vol 47 (11) ◽  
pp. 1621-1627 ◽  
Author(s):  
Peter Jeske ◽  
Karl Wieghardt ◽  
Bernhard Nuber
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Crystal Data ◽  
Nmr Spectrum ◽  
Tetranuclear Complex ◽  
H Nmr

Reaction of LTiCl3 (L = 1,4,7-trimethyl-1,4,7-triazacyclononane) in CH3OH with sodium 2,4-pentanedionate (acac) in the presence of air yields upon addition of NaClO4 yellow crystals of the tetranuclear complex [{LTi(OCH3)}2(μ-O)4{Ti(acac)2}2](ClO4)2·2H2O (1), the crystal structure of which has been determined. Crystal data: monoclinic, P21/c, a = 9.563(4), b = 22.695(8), c = 13.842(5)Å, β = 93.69(3)°; Z = 2. The 400 MHz 1H NMR spectrum shows that two different isomers with Δ, Λ -configuration at the Ti(acac)2(μ-O)2- and (δδδ) or (λλλ) conformation at the LTi(OCH3)(μ-O)2-fragment cocrystallize.

Darstellung, 11B-, 1H-NMR und Schwingungsspektren von 4-Aminopyridylundecahydro-closo-dodecaborat(1-) sowie Kristallstruktur von (Ph4As)[(4-(NH)-C5H4N)B12H11]·2CH3CN / Synthesis, 11B , 1H NMR and Vibrational Spectra of 4-Aminopyridylundecahydro-closo- dodecaborate(1-) and Crystal Structure of (Ph4As)[(4-(NH)-C5H4N)B12H11]·2CH3CN

1997 ◽  
Vol 52 (8) ◽  
pp. 939-942 ◽  
Author(s):  
T Koch ◽  
W Preetz
Keyword(s):  
1H Nmr ◽  
Deae Cellulose ◽  
Exchange Chromatography ◽  
Orthorhombic Space Group ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Stretching Vibrations ◽  
Ir And Raman

By reaction of (n-Bu4N)2[B12H12] with 4-aminopyridine at 190°C the 4-aminopyridylundecahydro- closo-dodecaborate anion [(4-(NH)-C5H4N)B12H11]- is obtained which can be separated from excess [B12H12]2- by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The X-ray structure determination of (Ph4As)[(4-(NH)-C5H4N)B12H11]-2CH3CN (orthorhombic, space group Pbca, a = 14.294(2), b = 19.587(2), c = 27.279(5)Å, Z = 8) reveals that the 4-aminopyridine substituent is bonded via the nitrogen atom of the amino group. The 11B NMR spectrum exhibits the characteristic feature (1:5:5:1) of a monosubstituated B12 cage with a downfield shift of ipso-B1 to -5.4 and antipodal-B12 to -18.1 ppm. The 1H NMR spectrum reveals the pattern of a monosubstituated pyridine. The IR and Raman spectra exhibit characteristic BH stretching vibrations between 2489 and 2521 cm-1 and the CC and CN stretching vibrations in the range of 1405 to 1636 cm-1.

1H NMR, 31P NMR and Raman Study of CaHPO4 and SrHPO4

2005 ◽  
Vol 60 (1-2) ◽  
pp. 121-126 ◽  
Author(s):  
B. Louati ◽  
K. Guidara ◽  
M. Gargouri ◽  
M. Fourati
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
31P Nmr ◽  
Cross Polarization ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Nmr Techniques ◽  
Raman Study

CaHPO4 and SrHPO4 were investigated using Raman, 1H NMR and 31P NMR techniques to study the environment of their PO3−4 tetrahedra and the percentage of mobile protons. 1H NMR spectra at room temperature suggest the presence of three types of protons, in agreement with RX investigation. The percentage of mobile protons in SrHPO4 is greater than in CaHPO4 because Sr2+ is bigger than Ca2+. 31P NMR spectra at room temperature show two lines in the spectrum of SrHPO4, revealing an equal environment of two sets of pairs of PO3− 4 . The 31P NMR spectrum of CaHPO4, however, exhibits three lines. This result was confirmed using a cross polarization (CP) sequence program. The first peak is attributed to the first set of pairs of P(1)O4 units and the two other ones to P(2)O4 and P(2)O4 units.

THE STEREOCHEMISTRY OF 2-t-BUTYL-2-CYANO-3-PHENYLCYCLOBUTANONE BY COMPLETE ANALYSIS OF ITS 1H NMR SPECTRUM

1982 ◽  
pp. 143-147
Author(s):  
MIRCEA D. GHEORGHIU ◽  
LUMINITA PÂRVULESCU ◽  
CONSTANTIN DRÂGHICI ◽  
MIHAI ELIAN
Keyword(s):  
1H Nmr ◽  
Complete Analysis ◽  
Nmr Spectrum
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