Two new acylamide metal-organic frameworks (MOFs), based on mixed N- and O-donor ligands, with 4-connected topologies have been obtained, namely poly[[μ2-N(1),N(4)-bis(pyridin-3-yl)terephthalamide]bis(μ3-4,4'-oxydibenzoato)dizinc(II)], [Zn2(C14H8O5)2(C18H14N4O2)]n, (1), and poly[[(μ2-benzene-1,4-dicarboxylato)[μ2-N(4),N(4')-bis(pyridin-3-yl)-[1,1'-biphenyl]-4,4'-dicarboxamide]dicadmium(II)] dihydrate], {[Cd(C8H4O4)(C24H18N4O2)]·2H2O}n, (2). Complex (1) is a 4-connected CdSO4 net with no interpenetration, where the Zn(II) cation is regarded as a 4-connecting node with square geometry. Complex (2) is a 4-connected dia net with threefold interpenetration, where the Cd(II) cation acts as a 4-connecting node with tetrahedral geometry. The results of thermogravimetric and luminescence analyses are described in detail.