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A series of Cp*Rh‐based discrete architectures was constructed by selecting four ether bipyridyl ligands and three half‐sandwich rhodium(III) bimetallic construction units, respectively. This study demonstrates a strategy for making the transition from a binuclear D‐shaped ring to a tetranuclear [2]catenane by adjusting the length of bipyridyl ligands. In addition, changing the position on the naphthyl...
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