Synthesis and Characterization of a Calcium‐Pyrazolonato Complex. Observation of <i>In‐Situ</i> Desolvation During Micro‐Electron Diffraction

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