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A series of hierarchical three-dimensional (3D) manganese-cobalt BTC (Mn-Co BTC; BTC = benzene-1,3,5-tricarboxylate ) metal–organic frameworks (MOFs) with controllable sub-units and interior architectures have been synthesized at room temperature without templates, etchants, or high-pressure conditions. The assembling sub-units of the hierarchical 3D Mn-Co BTC MOFs can be controlled by tuning the Mn/Co ratio, with higher Mn content favoring one-dimensional (1D) sub-units, while higher Co content favors two-dimensional (2D) sub-units. The hierarchical hollow Mn-Co BTC spheres (M₂C-BTC) exhibit a frequency change (ΔF) of 383.7 Hz to 69.5 ppm of NH₃ which is ∼1.7-, 2.1-, 4.2-, and 8.3-times higher than the ΔFs of hierarchical Mn-Co BTC nanorods (M₁C-BTC), hierarchical flower-like Mn-Co BTC (M_0.5C-BTC), Mn-BTC nanospheres, and Co-BTC nanoplates, respectively. In addition, they exhibit …