The synthesis and crystal structure of the metal-organic framework {[Co(acetate)2(rctt-tetrakis(4-pyridyl)cyclobutane)] · 2(methanol)}∞ (1) are described. The structure of 1 is based on a (4,4)-grid topology with Co(II) ions and 4,4′-tpcb cyclobutane molecules as 4-connected nodes and two different rhombus-shaped cavities in the framework. Solvent methanol molecules are clathrated between the grids. A model involving pseudo-merohedral twinning was required to arrive at a satisfactory single-crystal structure solution. Crystal data for 1: triclinic, space group P, a=9.006(2), b=9.127(2), c=9.129(2), α=78.57(3), β=88.99(3), γ=88.98(3), V=735.4(3), and Z=1 for R=0.0362 (2539 reflections with I>2σ(I), 184 parameters).