We report a Johnson hexadecahedronal coordination cage, constructed via 10 Ni-4-p-tert-butylthiacalix[4]arene (Ni-4-TC4A) units as vertices and 16 5-(pyridin-4-yl)isophthalate (PIP) ligands as tiles. It features a gyroelongated square bipyramidal geometry, equivalent to two square pyramids pillared by a square antiprism, a J(17) Johnson solid. Remarkably, the cage compound exhibits a much higher uptake capacity of C3H8 than CH4, representing a promising material for separation of these two gases. In contrast, Co(4-)TC4A units are linked by PIP ligands and rare {Co4O4Cl2} clusters, providing a one-dimensional bamboo stick-like polymer.