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The complete *H NMR spectra of five nickel cyclidene macrocyclic complexes are assigned by using DEPT (distortionless enhancement by polarization transfer) and 2-D NMR techniques: *H-13C shift correlation, COSY (correlated shift), and NOESY (nuclear Overhauser enhanced correlated shift). The *H NMR assignments are consistent with the complexes having an overall saddle shape with the two saturated six-membered rings (composed of nickel, two nitrogens, and a trimethylene chain) adopting a chair and a boat configuration similar to those observed in the X-ray crystal structures of these complexes. The *H NMR spectra can distinguish between two possible configurations for the bridging moiety (lid-off and lid-on). The vinyl methyl groups, labeled as O and N, have a chemical shift separation greater than 0.35 ppm for a lid-off configuration and less than 0.15 ppm for a lid-on configuration.