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The zirconocene complexes L2ZrCl2 (L = C5H5, C5H4Me, Ind, C5Me5; L2 = rac-Me2C­(2-Me-4-But-C5H2)2, meso-Me2C­(2-Me-4-But-C5H2)2, rac-Me2C­(3-But-C5H3)2, rac-Me2C­(Ind)2, rac-Me2Si­(Ind)2, and rac- C2H4(Ind)2) were tested as catalysts in alkene hydroalumination by the isobutylalanes XAlBui 2 (X = H, Cl, Bui). A low-temperature NMR spectroscopy study on the structure and dynamics of Zr,Al intermediates formed in the L2ZrCl2–XAlBui 2 systems showed that the intra- and intermolecular exchange in the bimetallic clusters, controlled by the steric factor of the η5 ligand and organoaluminum compound nature, determines the activity of the whole catalytic system.