The macrocyclic [LnNiL]Cl-3 complexes (Ln = La-III, Ce-III, Pr-III, Nd-III, Sm-III, Eu-III) contain both lanthanide and transition metal ions. The crystal structure of [LaNiL]Cl-3 reveals a square planar environment of Ni(II) ion and an 8-coordinate, irregular coordination sphere of La(III) ion. The H-1 and C-13 NMR spectra of these compounds have been assigned on the basis of 2D techniques. The analysis of isotropic shifts of paramagnetic [LnNiL]Cl-3 complexes shows the importance of both contact and dipolar contributions.