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Darstellung und Kristallstrukturen einiger mit N,N' ‐Dimethylharnstoff verbrückter Diphosphorverbindungen; NMR‐Untersuchung einer λ 4 P + λ 4 P + ‐Diphosphorverbindung
Author(s) -
Ernst Ludger,
Jones Peter G.,
LookHerber Petra,
Schmutzler Reinhard
Publication year - 1990
Publication title -
chemische berichte
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 0009-2940
DOI - 10.1002/cber.19901230108
Subject(s) - chemistry , crystal structure , diastereomer , crystallography , nmr spectra database , nuclear magnetic resonance spectroscopy , stereochemistry , spectral line , physics , astronomy
Preparation and Single‐Crystal X‐ray Structure Investigations of some N,N′‐Dimethylurea‐Bridged Diphosphorus Compounds: NMR Studies of a λ 4 P + λ 4 P + ‐Diphosphorus Compound The synthesis of N,N′ ‐dimethylurea‐bridged diphosphorus compounds involving the structural elements λ 3 Pλ 4 P + ( 3b, 3c , and 7 ) and λ 4 P + λ 4 P + ( 4 and 8 ) is described. The salts 4 and 8 were obtained by methylation of the λ 3 Pλ 4 P + compounds 3c and 7 with MeOSO 2 CF 3 . The λ 3 P atom in 3c and 7 coordinates to tungsten(0) with formation of the ionic pentacarbonyl derivatives 9 and 10 . The NMR spectra of the diphosphonium salt 4 were completely analyzed using NOE and 2D shift correlation experiments ( 13 C, 1 H and 31 P, 1 H). The single crystal X‐ray structure determinations of 3b and 9 are reported. 3b found to crystallize as a hemisolvate with dichloromethane. The RR/SS diastereomer is present in the crystal. The PP distance amounts to 219.1 pm. Both phosphorus atoms interact weakly with the chloride ion (293, 312 pm). 9 crystallizes as a hemisolvate with toluene, the RS/SR diastereomer being present. A PP distance of 224.7 pm and weak interactions between the phosphorus atoms and an oxygen atom of the anion (305, 308 pm) are found.