Communication: Inclusion compounds have significant potential as chemical receptors for sensors; however, it is necessary to understand the encapsulation and release processes for such applications. These authors have utilized the powerful combination of simultaneous thermogravimetry and differential scanning calorimetry and X-ray diffraction to study the decomposition mechanism of the clathrates between 1,1'-binaphthyl-2,2'-dicarboxylic acid (BNDA) and dimethyl formamide (DMF). Decomposition was found to proceed via three intermediate phases whose structures were determined by single crystal X-ray crystallography.