Multiple data sets were collected but none gave rise to reliable solutions and therefore it was decided to use a calculated model of a MOF structurally analogous to 1, i.e. a doubly interpenetrated pcu framework, to predict a powder X-ray diffraction (PXRD) pattern for this MOF. PXRD patterns were collected for samples of 2 revealing relatively poor crystallinity for this material (Fig. ). Comparison of the simulated PXRD data from the calculated MOF structure with the experimental data (Fig. ) suggests that 2 adopts the same framework structure as 1. The adoption of a doubly interpenetrated structure is supported by calculations of the energy of interaction between two interpenetrating frameworks of -207 kJ/mol (see SI for more details). To investigate the effect of incorporating the PDI moiety into the MOF, electrochemical and spectroscopic measurements were undertaken. For comparison the electronic behaviour of L 1 was studied using cyclic voltammetry (CV), UV-vis spectroelectrochemistry (SEC), electron paramagnetic resonance (EPR) spectroscopy and fluorescence techniques. Most PDIs are known to exhibit two one-electron reversible reductions, as determined by cyclic voltammetry, and L 1 is no exception (Figure ). UV-visible spectroelectrochemistry (SEC) was used to confirm the reduction of L 1 to its mono-and dianionic forms. The conversion of the neutral compound to the charged delocalised radical monoanion (L 1•-) and the interconversion between the monoand dianionic species, (L 1 ) 2-, were successfully probed. L 1•-exhibits intense absorbance peaks at longer wavelengths, as anticipated for PDI monoanions and the overall profile for the interconversion between the monoanion and dianion agrees well with those that have been reported previously in the literature (see Figure and Table ). To further support evidence for the existence of radical anions as probed by the CV and SEC measurements, EPR studies were employed. (L 1 ) •-produces a complex 23-line EPR spectrum centred at giso = 2.0035 (Figure ).