Preparation and properties of rhodium(I) and iridium(I) diolefin complexes of heterodifunctional phosphorus–imine chelating ligands and a related iminophosphine. 103Rh NMR parameters of the rhodium complexes obtained via indirect two-dimensional 31P, 103Rh{1H} NMR spectroscopy

1995 ◽  
Vol 73 (5) ◽  
pp. 635-642 ◽  
Author(s):  
David J. Law ◽  
Glen Bigam ◽  
Ronald G. Cavell
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
1H Nmr Spectroscopy ◽  
Rhodium Complexes ◽  
Chelating Ligands ◽  
Two Dimensional ◽  
H Nmr ◽  
Nmr Parameters ◽  
Nmr Data

Treatment of [M(cod)Cl]2 (M = Rh, Ir) with iminophosphoranophosphine ligands of the type Ph2PQP(Ph2)=NSiMe3 (Q = CH2, CH2CH2, 1,2-C6H4) afforded the new metallacycles [Formula: see text] through elimination of Me3SiCl, ultimately "anchoring" the ligand to the metal through a metal–nitrogen σ bond. The phosphine functionality completes the chelate. Cationic complexes of the type [M(cod)L2]+PF6− (M = Rh or Ir; L2 = Ph2PQPPh2NR where Q = CH2, CH(CH3), 1,2-C6H4, and R = p-C6F4CN, C6H2F(NO2)2, and C6H3(NO2)2 or L = Ph2PN=C(H)Ph) were readily prepared by treating [M(cod)Cl]2 with L2 and KPF6. The detection and chemical shift determination of the insensitive 103Rh nucleus was easily accomplished via 31P detected indirect two-dimensional 31P, 103Rh{1H} NMR spectroscopy. The 103Rh, 1H, and 31P NMR data are discussed. Keywords: rhodium, iridium, phosphoranimine, iminophosphine, Rh NMR.

scholarly journals An ingenious method for the determination of the relative and absolute configurations of compounds containing aryl-glycerol fragments by 1H NMR spectroscopy

RSC Advances ◽  
2021 ◽  
Vol 11 (14) ◽  
pp. 8107-8116
Author(s):  
Xu Zhang ◽  
Kai-Zhou Lu ◽  
Hai-Wei Yan ◽  
Zi-Ming Feng ◽  
Ya-Nan Yang ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
H Nmr ◽  
Ingenious Method

A concise method was established to determine the relative and absolute configurations of aryl-glycerols that depend on the chemical shift differences (Δδ) of the diastereotopic methylene protons (H-3) by 1H NMR spectroscopy.

Anwendungen der 2 D-NMR-Spektroskopie in der Organophosphorchemie Beispiel: L-Menthyldichlorphosphan / Applications of the 2D NMR Spectroscopy in the Organophosphorus Chemistry Example: L-Menthyldichlorophosphine

1982 ◽  
Vol 37 (12) ◽  
pp. 1661-1664 ◽  
Author(s):  
Martin Feigel ◽  
Gerhard Hägele ◽  
Axel Hinke ◽  
Gudrun Tossing
Keyword(s):  
Nmr Spectroscopy ◽  
2D Nmr ◽  
2D Nmr Spectroscopy ◽  
H Nmr ◽  
Nmr Parameters ◽  
Nmr Data ◽  
Organophosphorus Chemistry ◽  
C Nmr

2D NMR ist used to determine the 1H NMR parameters of L-Menthyldichlorophosphine. 13C NMR data are given

Chemical Shift Nonequivalence of Enantiomers of Amino Acid Derivatives in 1H NMR and 19F NMR Spectroscopy Induced by L-Chirasil- Val.

1992 ◽  
Vol 47 (7) ◽  
pp. 1034-1036 ◽  
Author(s):  
Bernhard Koppenhoefer ◽  
Michael Hummel
Keyword(s):  
Amino Acid ◽  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
Methyl Esters ◽  
Enantiomeric Purity ◽  
Peak Splitting ◽  
H Nmr ◽  
Acid Methyl ◽  
Amino Acid Methyl Esters

Enantiomers of N-trifluoroacetyl-amino acid methyl esters in CC14 solution, after addition of the chiral polysiloxane (L)-Chirasil-Val, display a chemical shift nonequivalence ΔΔδ in both 1H NMR and 19F NMR spectroscopy. The effects found for the leucine and valine derivatives can be correlated with the thermodynamic parameters of interaction in the undiluted system, as determined by gas chromatography. In CDC13 solution, no peak splitting was observed. The method is potentially useful for the determination of the enantiomeric purity of substrates of low volatility.

1H—NMR-spektroskopische Bestimmung der diastereomeren Reinheit und der absoluten Konfiguration am Phosphoratom von tButyl-phenyl-phosphinsäure-(—)-menthylester / Determination of the Diastereomeric Purity and the Absolute Configuration at Phosphorus of tButyl-phenyl-phosphinic Acid (—)-Menthyl Ester by Means of 1H NMR Spectroscopy

1977 ◽  
Vol 32 (5) ◽  
pp. 589-593 ◽  
Author(s):  
Reiner Luckenbach ◽  
Hans-H. Bechtolsheimer
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Absolute Configuration ◽  
1H Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Phosphinic Acid ◽  
H Nmr ◽  
The Absolute ◽  
Diastereomeric Purity

The preparation and separation into diastereomers of tbutyl-phenyl-phosphinic acid (—)-menthyl ester (1a) is reported. The diastereomeric purity as well as the absolute configuration at phosphorus of 1 a can be deduced from the detailed analysis of the 1H NMR spectra of samples of 1a differing in their diastereomer ratios.

scholarly journals Determination of Absolute Stereochemistry of Natural Alicyclic Glycosides by 1H NMR Spectroscopy without Application of Chiral Reagents – An Indication

2011 ◽  
Vol 6 (5) ◽  
pp. 1934578X1100600 ◽  
Author(s):  
Tatyana N. Makarieva ◽  
Larisa K. Shubina ◽  
Alla G. Guzii ◽  
Natalya V. Ivanchina ◽  
Vladimir A. Denisenko ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
Absolute Configuration ◽  
1H Nmr Spectroscopy ◽  
Nmr Spectra ◽  
H Nmr ◽  
Steroid Glycosides ◽  
The Absolute ◽  
Absolute Stereochemistry

A study has been made of the 1H NMR spectra of peracetylated β-glucopyranosides and α-arabinopyranosides obtained by reaction of D- and L-glucoses, and L- and D-arabinoses with either ( R)- or ( S)-2-octanols. The obtained and literature data show that 1H NMR spectra may be used to determine the absolute configuration of the aglycone moieties of some alicyclic glycosides without the need to synthesize derivatives with chiral reagents, as long as the absolute configuration of their monosaccharide moiety is known or vice versa. Spectra of marine steroid glycosides and their acetates containing glycosylated side chains as alicyclic fragments were also examined. It was shown that analysis of 1H NMR spectra for the determination of the absolute configuration is more applicable in the cases when glycosides have the same substitution in the D-ring of the aglycone moiety.

Introducing a novel procedure for peak alignment in one-dimensional 1H-NMR spectroscopy: a prerequisite for chemometric analyses of wine samples

2020 ◽  
Vol 12 (28) ◽  
pp. 3626-3636
Author(s):  
Keshav Kumar ◽  
Ralf Schweiggert ◽  
Claus-Dieter Patz
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Current Work ◽  
Peak Alignment ◽  
One Dimensional ◽  
H Nmr

In the current work, a novel procedure for correcting the peak drifts of 1H-NMR was introduced that involved mapping NMR spectra on a common chemical shift axis followed by interval-wisely applying the correlation optimized warping (COW) algorithm.

Conformational study on ribonucleoside O-phosphonylmethyl derivatives by 1H NMR spectroscopy

1985 ◽  
Vol 50 (8) ◽  
pp. 1899-1905 ◽  
Author(s):  
Milena Masojídková ◽  
Jaroslav Zajíček ◽  
Miloš Buděšínský ◽  
Ivan Rosenberg ◽  
Antonín Holý
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Conformational Study ◽  
H Nmr ◽  
Conformational Properties

Conformational properties of ribonucleoside 5'-O-phosphonylmethyl derivatives have been determined by 1H NMR spectroscopy and compared with those of natural nucleosides and 5'-nucleotides.

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