Three different Co-MOFs, [Co3(L)2(DPDP)]n (1), [Co(HL)(DPDP)]n (2) and {[Co(HL)(1/2DPDP)3(H2O)]·H2O}n (3) (H3L = 4,4',4''-(nitrilotris(methylene))tribenzoic acid, DPDP = 4,4'-(2,5-dibutoxy-1,4-phenylene)dipyridine) have been co-crystallized in a one-pot reaction. Based on the significant differences between the three structures, we adopt solvents to ultimately regulate acquisition of pure crystals of the three compounds.