*2.2. Infrared Spectroscopy*

IR spectra were measured on a PerkinElmer Spectrum Two FTIR spectrometer equipped with an ATR Diamond accessory for powder samples. Samples were scanned over a range of 400–4000 cm<sup>−</sup>1.

### *2.3. Nuclear Magnetic Resonance (NMR)*

Solids containing the gues<sup>t</sup> species were soaked into DMSO-*d*6 and heated in order to release the guests into the solution for the NMR analysis. 1H NMR spectra were recorded in DMSO-*d*6 solution using a BRUKER 300 MHz spectrometer at 303 K. Appropriate signals were integrated to determine the ratio of the respective guests in the MOFs.

### *2.4. Powder X-ray Di*ff*raction (PXRD)*

Powder X-ray diffraction (PXRD) patterns were measured on a Bruker D8 Advance X-ray diffractometer operating in a DaVinci geometry equipped with a Lynxeye detector using CuKα-radiation (λ = 1.5406 Å). X-rays were generated at 30 kV and 40 mA. Samples were placed on a zero-background sample holder and scanned over a range of 4–40◦ in 2θ.
