Inorganic Chemistry

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

Authors

Abstract

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.

Content

Thumbnail image of 2022.08.04 Ca-complex micro-ED manuscript ChemRxiv.pdf

Supplementary material

Thumbnail image of 2022.05.31 Dalton Trans. Ca-complex micro-ED SI (6).pdf
Synthesis and Characterization of a Calcium-Pyrazolonato Complex. Observation of In-Situ Desolvation During Micro-Electron Diffraction. Supporting Information
SI