Nowadays, zirconium metal–organic frameworks attract more attention because of their robustness and their easier predictability in terms of topology. Herein, we have been able to control synthetic parameters in order to construct two new 2D MOFs with the same sql topology. Both materials, ACM-10 and ACM-11, have been characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and UV–vis spectroscopy. Their textural, electrochemical, and conductivity properties are presented along with the opportunities that these new topologically interesting scaffolds offer for the design of new structures.