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The 400 and 500 MHz  1 H NMR spectra of a series of η 1 ,η 2 -alkenyl- and η 3 -cycloalkenyl- η 5 -cyclopentadienylnickel complexes were analysed with the help of special NMR techniques like double resonance, automated spectra analysis, and nuclear Overhauser measurements. Ligands containing a 4-pentenyl unit adopt a certain conformation when complexed as bidentate to a transition metal (Ni, Ru). These η 1 ,η 2 -alkenyl complexes form a rigid ring in which the β-H atoms point away from the metal. This conformation is found independent of whether the chain is substituted with alkyl or cyclopropyl groups or if the 4-pentenylrest is part of a cyclo-4-octenyl ring. The structure of cyclic η 3 -alkenyl complexes can also be characterised with typical NMR parameters. The three carbon atoms of the η 3 -allyl group as well as their adjacent carbon atoms are in plane; in the greater rings (C 6 −C 8 ) the other carbon atoms point away from nickel. The nuclear Overhauser difference spectroscopy has been found to be an extremely sensitive tool for stereospecific assignments: in particular, very small intensity changes (below 1%) even of hidden protons can be detected. A procedure for the application of the automated spectra analysis is introduced. Based on these new experimental facilities a general strategy is proposed for the analysis of the  1 H NMR spectra of complex molecules.

zeitschrift für naturforschung b

Hochfeld-NMR-Spektroskopie. Analyse der  1 H-NMR-Spektren von η 1 .η 2 -Alkenyl-und η 3 -Cycloalkenyl-η 5  -cyclopeiitadienylnickelkomplexen / High Field NMR Spectroscopy. :  1 H NMR Spectra Analysis of η  1 ,η 2 -Alkenyl-and η 3 -Cycloalkenyl-η 5  -cyclopentadienylnickel Complexes