Water addition to a two-electron mixed-valence bimetallic centerWe dedicate this paper to the memory of our colleague and friend, Ian P. Rothwell.Electronic supplementary information (ESI) available: 1H NMR spectra of 2 and 2(D) and 31P NMR spectrum of 2 and tables for X-ray structure determination of 2 and 3. See http://www.rsc.org/suppdata/cc/b4/b402426e/

2004 ◽  
pp. 1958 ◽  
Author(s):  
Adam S. Veige ◽  
Daniel G. Nocera
Keyword(s):  
1H Nmr ◽  
Structure Determination ◽  
Nmr Spectra ◽  
31P Nmr ◽  
Mixed Valence ◽  
Supplementary Information ◽  
Water Addition ◽  
Nmr Spectrum ◽  
X Ray

scholarly journals Zur Chemie der 1,3,5-Triaza-2-phosphinan-4,6-dione, Teil V Darstellung der Phosphoryl(III)(λ4P)- und Thiophosphoryl(III)(λ4P)-Derivate der 1,3,5-Triaza-2-phosphinan-4,6-dione. Umsetzungen mit Ketonen Chemistry of the 1,3,5-Triaza-2-phosphinane-4,6-diones, Part V / Synthesis of Phosphoryl(III)(λ4P) and Thiophosphoryl(III)(λ4P) Derivatives of 1,3,5-Triaza-2-phosphinane-4,6-diones. Reactions with Ketones

1993 ◽  
Vol 48 (7) ◽  
pp. 860-866 ◽  
Author(s):  
Ion Neda ◽  
Michael Farkens ◽  
Axel Fischer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Mass Spectrum ◽  
Hydrogen Sulphide ◽  
Structure Determination ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Structural Element ◽  
Nmr Spectrum ◽  
X Ray ◽  
Derivatives Of

The phosphoryl(III)(λ4P) and thiophosphoryl(III)(λ4P) derivatives, 1,3,5-trimethyl-2-hydro-1,3,5-triaza-2-oxo-2λ4-phosphinane-4,6-dione 2 and 1,3,5-trimethyl-2-hydro-1,3,5-triaza-2-thio-2λ4-phosphinane-4,6-dione 3 were obtained from 2-chloro-1,3,5-trimethyl-1,3,5-triaza-2λ3-phosphinane-4,6-dione 1, by reaction either with water or with hydrogen sulphide. The reactions of 2 and 3 with the fluorine-containing ketones, hexafluoroacetone and trifluoroacetophenone, led to the compounds 4-7 with the P(:O)–O or P(:S)–O structural element. The compounds 2-6 were characterized via their 1H, 13C and 31P NMR spectra, mass spectra and through the X-ray structure determination of 4. Compound 7 was characterized from its 1H and 31P NMR spectrum and mass spectrum, only.

scholarly journals Darstellung und Charakterisiening der Spezies R-C7H7Mo(CO)3 und die Röntgenstrukturanalyse von / Synthesis and Characterisation of the Species R-C7H7Mo(CO)3 and the X-ray Structure Determination of

1978 ◽  
Vol 33 (4) ◽  
pp. 361-365 ◽  
Author(s):  
Margret Sommer ◽  
Klaus Weidenhammer ◽  
Henning Wienand ◽  
Manfred L. Ziegler
Keyword(s):  
Carbon Atom ◽  
Structure Determination ◽  
Nmr Spectra ◽  
X Ray ◽  
Ethyl Group ◽  
H Nmr

The species R−C7H7Mo(CO)3 (R=−CH2COCH3,−CH(CH3)COCH3,−CH(CH)(CH3)2COCH3) have been synthesized by electrolysing [η7-C7H7Mo(CO)3]+, η7-C7H7Mo(CO)2Br and the dimers [C7H7Mo(CO)3]2 and (C7H7)2Mo(CO)3, respectively, in suitable ketones and HBr. 1H NMR spectra and the X-ray structure determination of (CH3−CO−CH(CH3)−C7H7)Mo(CO)3 revealed the CH3−CO−CH(CH3)-group being bonded to the cycloheptatriene ligand via the α-carbon atom of the ethyl group.

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.

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