Single-crystal X-ray structure diffraction studies of complex 1•2DMF•H2O were performed with a Bruker SMART APEX CCD diffractometer equipped with graphite-monochromated Mo K radiation ( = 0.71073 Å). The single crystal was mounted on a crystal mounting loop with the help of Paratone oil at 296 K and slowly cooled down to the measured temperature 120 K with 2 K/min ramping rate using a liquid nitrogen gas-stream cooling device, followed by data collection at respective temperatures. Data integration and reduction were carried out using SAINT software, and empirical absorption corrections were performed using SADABS program. The structures were solved by direct methods and refined using full-matrix leastsquares method on F2 with SHELXL-2014. The packing diagrams were made using Mercury 4.2.0. The disordered non-hydrogen atoms belonging to the solvent molecules were refined isotropically. Moreover, hydrogen atoms could not be assigned to the solvent molecules, though, considered in the molecular formula. All other non-hydrogen atoms of complex 1•2DMF•H2O were refined anisotropically and hydrogen atoms were labeled to ideal positions and refined isotropically using a riding model. Complex 1•2DMF•H2O at 120 and 240 K contains severely disordered BF4 -molecules, which were treated by using SOLVENT MASK procedure in OLEX 2 which is equivalent to SQUEEZE in PLATON. Additional information about the SOLVENT MASK procedure and corresponding results can be found in the cif files. The Single-crystal X-ray structure diffraction studies of complex 1•2DMF was performed at the X-ray diffraction beamline (XRD1) of the Elettra Synchrotron (Trieste, Italy). The crystals were dipped in NHV oil (Jena Bioscience, Jena, Germany) and mounted on the goniometer head with nylon loops (MiTeGen, Ithaca, USA). Data were acquired using a monochromatic wavelength of 0.70 Å through the rotating crystal method on a Pilatus 2M hybrid-pixel area detector (DECTRIS Ltd., Baden-Daettwil, Switzerland). The diffraction data were indexed and integrated using XDS. The structure was solved with Olex2 44 by using ShelXT structure solution program by Intrinsic Phasing and refined with the ShelXL 46 refinement package using least-squares minimization. In the last cycles of refinement, non-hydrogen atoms were refined anisotropically. Hydrogen atoms were included in calculated positions, and a riding model was used for their refinement. The crystal 1•2DMF•H2O was mounted directly at 350 K using XRD1 beamline at Elettra Sincrotrone to remove the water molecule (confirmed by TGA data) and then we measured the structure at 270 K quickly. The data quality of 1•2DMF was not great due to the degradation of the crystal at high temperature. However, we were able to see the structure of partially desolvated 1•2DMF form which has no water molecule present. We have