Alkaline earth metal ion doped Zn(II)-terephthalates, [Zn2Mg(PBDC)(3)(DMA)(2)](n) (1), [ZnCa(PBDC)(2)(DMA)(2)](n) (2), [ZnSr(PBDC)(2)(DMA)(2)](n) (3) and [Zn2Ba(PBDC)(3)(mu(2)-O1w)(2)(DMF)](n)center dot n(DMF) (4) (H2PBDC = terephthalic acid, DMA = N,N'-dimethylacetamide, DMF = N,N'-dimethylformamide), have been solvothermally synthesized and characterized by single-crystal X-ray diffraction, powder X-ray diffraction, elemental analyses, IR spectra, and thermal analyses. Different secondary building subunits, [Zn2Mg(mu(2)-COO)(3)] for 1, [ZnCa(mu(2)-COO)(3)] for 2, [ZnSr(mu 2COO)(3)] for 3, and [Zn2Ba(mu(2)-COO)(4)(mu(2)-O1w)(2)] for 4, are realized by the introduction of different alkaline earth ions. Compound 1 is a two-dimensional (2D) layer structure with 6-connected hxl topology. Compounds 2 and 3 are isostructural and exhibit a three-dimensional (3D) framework with (3,5)-connected {4.6(2)}{4.6(6).8(3)} topology owing to their similar secondary building subunits. Compound 4 is a three-dimensional (3D) opened framework with the channels occupied by the disordered lattice DMF molecules and can be simplified into a (3,8)-connected {4(2).6}(2){4(4).6(14).7(8).8(2)} topology. Moreover, the solid-state fluorescence of compounds 1-4 have also been investigated at room temperature.