2,6-Bis(5-trifluoromethylpyrazol-3-yl)pyridine (H2L) and its mono-, tri-, and tetranuclear NiII complexes were synthesized for the first time. All the obtained compounds were characterized by single-crystal X-ray diffraction analysis. In the complexes, 2,6-bis(5-trifluoromethylpyrazol-3-yl) pyridine exists in the neutral and dianionic forms and exhibits different coordination modes (κ3-, μ2-κ3: κ1-, and μ3-κ3: κ1:κ1). The electrochemical and magnetic properties of all compounds were studied. The tetranuclear NiII complex with the L2- dianion is reduced in two sequential reversible one-electron steps