The reaction of [HNBu3]3[Mo(CN)8] with a mixture of Fe(BF4)2.6H2O and v-im in DMF resulted in a green solution. Slow evaporation of the reaction mixture afforded analytically pure yellow plates shape crystals of 1•2DMF•H2O (Figure ) in good yield (details in supporting information). PXRD and elemental analysis were performed to check the purity of 1•2DMF•H2O in bulk (Figure ). 1•2DMF•H2O experiences a weight loss between 300 and 313 K (WL: 1.5%) and converts to partially desolvated form of 1•2DMF after losing one water molecule from the crystal structure, after which the complex is stable up to 430 K, confirmed by TGA analysis (Figure ). The minor deviation in the experimental PXRD data is seen due to the temperature difference between experimental and simulated data and the partial loss of interstitial solvent molecules during the sample preparation for the PXRD measurement at room temperature.