Abstract
AbstractThe synthesis and characterization 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 complementary data during structural determination, and that even electrophilic metals are susceptible to desolvation under micro‐ED measurements.
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