3.1.2. MAL for Compaction Study

Crystalline MAL from the supplier was ground using a mortar and pestle to obtain the desired particle size range of 5-40 μm. Prior to the compaction study, the powder was dried in a hot air oven at 50 ± 2 ◦C for 2 h to remove any adsorbed moisture from the surface.

## 3.1.3. RIV-MAL Co for Compaction Study

The compaction study requires a large quantity of material; hence the previously reported process was scaled up. Initially, a small batch (~150 mg) of RIV-MAL Co was prepared as per the reported method [10]. These crystals were used as "seeds" for preparing a batch of ~8.0 g.

For preparing 8.0 g batch of RIV-MAL Co, 6.0 g of RIV was dissolved in 30.1 mL of 2,2,2-trifluoroethanol (TFE) in a glass beaker (50 mL capacity) with stirring and heated using a water bath between 70 and 80 ◦C. MAL (2.07 g) was added to the hot solution of RIV and volume of the solution was reduced to approximately 55% by heating (70-75 ◦C) it in the open vessel for 1-2 h. Thereafter, the hot solution was transferred to another glass beaker. The resultant solution was seeded with the crystals of RIV-MAL Co and cooled to room temperature. After 10-20 min, the cocrystals crystallized from the solution were collected using vacuum filtration. The crystals were dried at 25 ◦C in a vacuum drier.

All three solids were stored in a desiccator at 43% RH (maintained using a saturated solution of potassium carbonate, K2CO3) until further use.
