Three zinc(II) metal-organic frameworks (xF-MAC-3) have been synthesized by using Zn(II) salts, 3,5-dimethyl-1H-1,2,4-triazole (Hdmtrz) and different fluorination degree carboxylate ligands, which are analogic structures and can be described as (6,6)-connected pcu-b net. We find that the fluorine atoms have structural regulation effect on xF-MAC-3, which can not only enlarge the torsion angle 𝜑 of carboxylate ligands but also elevate the space group of structures. Besides, the CO₂-273 K uptake increased from 23.21 cm³·g^-1 (MAC-3) to 36.13 cm³·g^-1 (4F-MAC-3) and H₂-77 K uptake increased from 24.33 cm³·g^-1 (MAC-3) to 59.79 cm³·g^-1 (4F-MAC-3), which means fluorination can enhance the gas adsorption uptake of xF-MAC-3 analogues. Furthermore, the results of fluorination in xF-MAC-3 analogues offer a potential way to study the ligand pre-functionalization effect on the structures and properties of MOFs analogues.