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The detectton of NMR spectra of less sertstttve nuclei coupled to protons may be s@ficantly unproved by a two-dimezsional Founer transform technique tnvolvmg a double transfer of pokuzatton. The method IS adequate to obtam natwaI abundance "N spectra m small sample volumes wth a commerctal spectrometer

Since the sign of V(P,F) in these metal complexes can be assumed to be negative52 from the twodimensional correlation experiments (cf. Figure 4b), it follows that V(F,Fe) is positive. Of particular value is the combination of two-dimensional experiments, e.g. ('H,57Fe) and (31,57Fe) for complex 1. In this way, the relative signs of a variety of scalar couplings in quasitrigonal and -tetragonal complexes can be obtained (cf. Chart IV). To the best of our knowledge, the signs (52) Staplin, D. C.;

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