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Three new Metal-Organic Frameworks, containing mesitylene tribenzoic acid as a linker and zinc (<b>1</b>) or cadmium as metals (<b>2</b>,<b>3</b>), were synthesized through solvothermal reactions, using DMF/ethanol/water as solvents, at temperatures of 80 °C (structures <b>1</b> and <b>3</b>) and 120 °C (structure <b>2</b>). Following single-crystal X-ray diffraction, it was found that <b>1</b> and <b>3</b> crystallize in the <i>P</i>2₁/<i>c</i> and C2/<i>c</i> space groups and form 2D networks, while <b>2</b> crystallizes in the <i>Fdd</i>2 space group, forming a 3D network. All three frameworks, upon heating, were found to be stable up to 350 °C. N₂ sorption isotherms revealed that <b>1</b> displays a BET area of 906 m²/g. Moreover, the porosity of this framework is still present after five cycles of sorption/desorption, with a reduction of 14% of the BET area, down to 784 m²/g, after the fifth cycle. The CO₂ loading capacity of <b>1</b> was found to be 2.9 mmol/g at 0 °C.