| Summary: | Two new lanthanide-based coordination polymers, [Sm<sub>2</sub>(bzz)(ben)<sub>6</sub>(H<sub>2</sub>O)<sub>3</sub>]·0.5H<sub>2</sub>O (<b>1</b>) and [Eu(bbz)(ben)<sub>3</sub>] (<b>2</b>), were synthesized and characterized. The described products were formed from in situ-generated benzoate (ben) and <i>N</i>’-benzoylbenzohydrazide (bbz) ligands, which were the products of transformation of originally added benzhydrazide (bzz) under hydrothermal conditions. Compound <b>1</b> exhibits a one-dimensional (1D) double-chain structure built up from the connection of the central Sm<sup>3+</sup> ions with a mixture of bzz and ben ligands. On the other hand, <b>2</b> features a 3D network with a 4-connected (6<sup>6</sup>) dia topology constructed from dinuclear [Eu<sub>2</sub>(ben)<sub>6</sub>] secondary building units and bbz linkers. High-pressure CO<sub>2</sub> sorption studies of activated <b>1</b> show that maximum uptake increases to exceptionally high values of 376.7 cm<sup>3</sup> g<sup>−1</sup> (42.5 wt%) under a pressure of 50 bar at 298 K with good recyclability. Meanwhile, <b>2</b> shows a typical red emission in the solid state at room temperature with the decay lifetime of 1.2 ms.
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