Using bis-pyridyl-bis-amide ligands N,N′-bis-(4-pyridyl)phthalamide (L1), N,N′-bis-(4-pyridyl)iso -phthalamide (L2), hexanedioic acid bis-pyridin-4-ylamide (L3), and carboxylates, six metal(II) complexes formulated as Cd2(1,4-chdc)(L1)2·4H2O (1,4-H2chdc = 1,4-cyclohexanedicarboxylic acid) (1), Cd2(L1)2(in)4·3DMF (Hin = isonicotinic acid) (2), Zn(L1)(1,4-bdc) (1,4-H2bdc = 1,4-benzenedicarboxylic acid) (3), Cd(L2)(1,4-chdc) (4), Zn2(L2)2(tdc)2·DMF (H2tdc = thiophene-2,5-dicarboxylic acid) (5), and Zn(2,6-ndc)0.5(L3)0.5(SO4)·(CH3NHCH3) (2,6-H2ndc = 2,6-naphthalene- dicarboxylic acid) (6) have been hydro(solvo)thermally synthesized and structurally characterized by single-crystal X-ray diffraction. Complex 1 is a uninodal 6-connected noninterpenetrated three-dimensional (3D) network with {44.610.8}-mab topology, complex 2 exhibits a uninodal 6-connected 2-fold interpenetrated 3D framework with {412.63}-pcu topology, complex 3 shows a uninodal 8-fold interpenetrated 3D diamondoid framework, complexes 4 and 5 possess similar uninodal 2D layer with 44-sql topology, and complex 6 shows a framework of 2D → 3D inclined polycatenation based on 44-sql layer. The six complexes show different thermal stability and photoluminescence properties. The emission band of complex 1 becomes strong after dehydration, and water can reduce the emission intensities of the six complexes to some extents.