Abstract
<h2>Summary</h2> An H-shaped [2]rotaxane with a biphenyl axle and a 24-crown-8 (<b>24C8</b>) macrocycle was inserted into the tetrahedral cavities of the isostructural <b>fcu</b> MOFs <b>PCN-57</b>, <b>UiO-68</b>-d<sub>4</sub>, and <b>UWCM-10</b>. The resulting rotaxane containing MOFs <b>UWDM-8</b>, <b>UWDM-9</b>-d<sub>4</sub>, and <b>UWDM-10</b> have precise spatial arrangements of two different mobile components—a rigid rotor (tetramethylphenyl, phenyl-d<sub>4</sub>, or tetrazine) and a rotaxane macrocycle (<b>24C8</b>). The mobility of these units was characterized by variable-temperature (VT) solid-state nuclear magnetic resonance (SSNMR). VT <sup>13</sup>C SSNMR showed that the translational position of the macrocyclic wheel along the [2]rotaxane axle is dictated by the bulk and rotational orientation of the central rotor, while VT <sup>2</sup>H SSNMR demonstrated that the dynamics of the rotor are influenced by the presence of the macrocycle.
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