Synthesis and Characterization of a Calcium-Pyrazolonato Complex. Observation of In-Situ Desolvation During MicroElectron Diffraction.

The synthesis and characterisation of a calcium pyrazolonato complex is reported. X-Ray diffraction (XRD) of single crystals revealed an octahedral geometry with two axial solvent ligands. Analysis of the bulk sample by means of microcrystal electron diffraction (micro-ED) measurement revealed a polymeric pentagonal bipyramidal coordination geometry joined via a central Ca2O2 ring with axial water ligands. During the micro-ED measurement, loss of water was observed resulting in a secondary structure with a polymeric distorted octahedral coordination geometry joined via a central Ca2O2 ring. These findings demonstrate that XRD and micro-ED methods can provide complemetary data during structural determination, and that even electrophilic metals are susceptible to desolvation under micro-ED measurements.