By introducing different surfactants into a reaction system, two previous mixed-phase Ni(II)-MOFs constructed from an undeveloped pyridyl-tetracarboxylate and Ni(II) salts were successfully isolated to obtain two pure products. Compound 1 exhibits a 3D H-bonded network with (3,8)-connected {4.5(2)}2{4(2).5(6).6(14).7(2).8(4)} topology, while 2 features a 3D 2-fold interpenetrating framework with a self-penetrating (3,4,4)-connected {6(2).10(3).12}{6(3)}2{6(4).8.10}2 topological net.