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To develop heterogeneous catalysts for ethylene polymerization, bis(imino)pyridineiron(III), α-diiminenickel(II), and iminopyridinenickel(II) complexes were immobilized in the clay mineral (montmorillonite, fluorotetrasilicic mica or saponite) interlayers by a one-pot preparation method. In this method, the Fe3 +- and Ni2 +-exchanged clay minerals as an acid catalyst promoted the ligand formation from a ketone derivative and an aniline derivative, and then the formed ligand simultaneously coordinated to the metal ions located in the clay mineral interlayer. The obtained heterogeneous catalysts showed 100–3,000 g-PE g-cat− 1 h− 1 as activities for the ethylene polymerization/oligomerization.