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Figure 4
In situ PXRD and PDF analysis of the reaction to Fe3O4. (a) Schematic of the reaction mechanism as determined by PXRD and PDF refinements. The initial complex Fe(acac)3 forms [Fe3(μ3-O)(AcOR)6(ROH)3]+ after reaching the reaction temperature of 180°C which further reacts to the final product Fe3O4. (b, c) Temperature profile and heatmap of PXRD and PDF data, respectively. (d, e) PXRD Rietveld and PDF refinements of the initial complex before heating, Fe(acac)3, the intermediate complex, [Fe3(μ3-O)(AcOR)6(ROH)3]+, at 5 min after reaching the reaction temperature of 180°C and Fe3O4. Since Rietveld refinement requires a crystalline structure only the refinement of Fe3O4 is shown for PXRD.

Journal logoJOURNAL OF
SYNCHROTRON
RADIATION
ISSN: 1600-5775
Volume 33| Part 1| January 2026| Pages 142-153
https://doi.org/10.1107/S1600577525009634
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