A laboratory experiment for students in advanced inorganic chemistry is described. Students prepare palladium(II) cyclometalated complexes. A terdentate [C,N,O] Schiff base ligand is doubly deprotonated upon reaction with palladium(II) acetate in a self-assembly process to give a palladacycle with a characteristic tetranuclear structure. This complex reacts with triphenylphosphine in a ligand-substitution process, cleaving of the tetranuclear structure. Students assign the resonances in the [superscript 1]H, [superscript 13]C-{[superscript 1]H}, and [superscript 31]P-{[superscript 1]H} NMR spectra of the prepared compounds, whose 3D structure is given to understand the relative spatial disposition of the cyclometalated fragments. Mass spectra are interpreted taking into account the characteristic isotopic pattern originated by the tetranuclear [Pd[subscript 4]L[subscript 4]]+ molecular ion. (Contains 2 figures and 4 schemes.)