Two novel cadmium-based 2D coordination polymers have been synthesized and characterized. Experimental results evidence that the best delamination processes occurs when weak interactions dominate the cohesion between layers and solvent molecules are occluded within the crystalline network. In this case, the delamination of the crystals occurs spontaneously in water. On top of that, and thanks to the high stability of the resulting (flake) colloidal dispersions, we have completed a detailed study of the sonication assisted delamination impact by: I) comparison of two different sonication approaches (bath vs. tip sonication) and II) optimization of final flake morphology and yield by controlling solvent and sonication time. Our results definitely pave the way for the fabrication and implementation of 2D coordination polymers using ultrasound.