The use of both 5-methylisophthalic acid (H2mip) and 4,4′-dipyridyldisulfide (dpds) with Zn(II) ion under hydrothermal conditions has provided a new zinc(II) coordination polymer, [Zn(mip)(dps)]n (1), and it has been characterized by elemental analysis, FT-IR spectroscopy, and X-ray single-crystal diffraction. The starting reagent dpds ligand was converted to dps (4,4′-dipyridylsulfide) in the resulting complex. It crystallizes in monoclinic space group P21/n with a = 12.0091(12), b = 10.9122(11), c = 13.4699(14) Å, β = 95.1890(10)°, C19H14N2O4SZn, Mr = 431.75, V = 1757.9(3) Å3, Z = 4, μ = 1.545 mm-1, Dc = 1.631 g·cm-1, F(000) = 880, R = 0.0380, wR = 0.1050 (I > 2σ(I)). The title complex has a 3-D 4-fold interpenetrating diamondoid network with (66) topology. Photoluminescence measurements show that 1 has medium fluorescent emissions at 458 nm and 543 nm upon excitation at 322 nm.