The Mo-C bond distances at 120 K in 1•2DMF•H2O lie in the range of 2.144(3) -2.158(3) Å for bridging cyanides and for the non-bridging cyanide the value ranges from 2.161(4) -2.167(3) Å which is typical for Mo(V) state (Table ). The Fe1-N bond lengths vary from 2.152(3) to 2.174(3) Å which is very similar to those of Fe2-N bond lengths ranging between 2.119(3) -2.162(3) Å. This suggests that both Fe1 and Fe2 centers are present in a high-spin Fe(II) state at 120 K. At 240 K, the average Mo-C bond distance is observed to be 2.161 Å whereas the average Fe1-N and Fe2-N bond distances are found to be 2.167 and 2.175 Å respectively indicating the presence of Fe(II) HS state (Table ) at this temperature. After that we have measured the single crystal XRD structure using synchrotron beamline where we introduced the crystal directly at 350 K and rapidly cooling it down to 270 K in order to get the structure of the partially desolvated complex 1•2DMF as suggested by the TGA analysis (vide supra). Complex 1•2DMF also crystalizes in monoclinic space group C2/c with Mo center adopting distorted square antiprism geometry and Fe centers adopting distorted octahedral geometry (Table &). Similar values of Mo-C, Fe1-N and Fe2-N bond distances (avg. Mo-C=2.172; avg. Fe1-N=2.172; avg. Fe1-N=2.161) are observed for the partially desolvated complex (1•2DMF) at 270 K indicating the presence of Fe(II) HS and Mo(V) states at that temperature (Table ). -S6).