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Understanding and controlling nucleation is important for many crystallization applications. Calcium carbonate (CaCO₃) is often used as a model system to investigate nucleation mechanisms. Despite its great importance in geology, biology, and many industrial applications, CaCO₃ nucleation is still a topic of intense discussion, with new pathways for its growth from ions in solution proposed in recent years. These new pathways include the so-called nonclassical nucleation mechanism via the assembly of thermodynamically stable prenucleation clusters, as well as the formation of a dense liquid precursor phase via liquid–liquid phase separation. Here, we present results from a combined experimental and computational investigation on the precipitation of CaCO₃ in dilute aqueous solutions. We propose that a dense liquid phase (containing 4–7 H₂O per CaCO₃ unit) forms in supersaturated solutions through the …