DOI: 10.5061/dryad.wh70rxwtp
title: Data from: Reactive high-spin iron(IV)-oxo sites through dioxygen activation in a metal–organic framework

description: In nature, nonheme iron-containing enzymes use dioxygen to generate
 high-spin iron(IV)=O species for a variety of oxygenation reactions.
 Although scientists have long sought to mimic this reactivity, the
 enzyme-like activation of dioxygen to form high-spin iron(IV)=O species
 remains an unrealized goal in synthetic chemistry. Here, we report a
 metal–organic framework featuring iron(II) sites with a local structure
 similar to that in α-ketoglutarate-dependent dioxygenases. The framework
 reacts with dioxygen at low temperatures to form high-spin iron(IV)=O
 species that are characterized using in situ diffuse reflectance infrared
 Fourier transform, in situ and variable-field Mössbauer, Fe Kβ x-ray
 emission, and nuclear resonance vibrational spectroscopies. In the
 presence of dioxygen, the framework is competent for catalytic oxygenation
 of cyclohexane and the stoichiometric conversion of ethane to ethanol.
description: # Reactive high-spin iron(IV)-oxo sites through dioxygen activation in a
 metal–organic framework: PXRD and XES data
 [https://doi.org/10.5061/dryad.wh70rxwtp](https://doi.org/10.5061/dryad.wh70rxwtp) ## Description of the data and file structure Powder x-ray diffraction (PXRD) data collected at the Advanced Photon Source at Argonne National Laboratory, and iron Kβ x-ray emission spectroscopy (XES) data collected at the PINK tender x-ray beamline at the BESSY II lightsource at the Helmholtz-Zentrum Berlin. Experimental details can be found in the Supplementary Materials pdf file, which is available online (free of charge): https://www.science.org/doi/full/10.1126/science.add7417. Details about PXRD files: The respective files listed below contain the collected data. The sample description, measurement temperature, and the figure in the Supplementary Materials, in which the plotted data appears, are denoted in the file name. The first column of each file is the 2theta value in degrees, which is the scattering angle of the x-ray beam (wavelength = 0.045 nm), the second column is the diffraction intensity in counts, and the third column is the error in intensity of the measurement: * PXRD\_Fe1.8Zn3.2(prv)4(btdd)3\_S3.txt * PXRD\_FeZn4(prv)4(btdd)3\_S3.txt * PXRD\_FeZn4(prv)4(btdd)3\_\_100K\_O2\_dosed\_S24.xye * PXRD\_FeZn4(prv)4(btdd)3\_150K\_O2\_dosed\_S24.xye * PXRD\_FeZn4(prv)4(btdd)3\_200K\_O2\_dosed\_S24.xye * PXRD\_FeZn4(prv)4(btdd)3\_250K\_O2\_dosed\_S24.xye * PXRD\_FeZn4(prv)4(btdd)3\_298K\_O2\_dosed\_S24.xye * PXRD\_FeZn4(prv)4(btdd)3\_pristine\_100K\_S24.xye * PXRD\_FeZn4(moba)4(btdd)3\_\_100K\_O2\_dosed\_S27.xye * PXRD\_FeZn4(moba)4(btdd)3\_\_150K\_O2\_dosed\_S27.xye * PXRD\_FeZn4(moba)4(btdd)3\_\_200K\_O2\_dosed\_S27.xye * PXRD\_FeZn4(moba)4(btdd)3\_\_250K\_O2\_dosed\_S27.xye * PXRD\_FeZn4(moba)4(btdd)3\_\_298K\_O2\_dosed\_S27.xye * PXRD\_FeZn4(moba)4(btdd)3\_pristine\_S27.xye Details about the XES data files: The respective files listes below contain the collected data (T = 30 K). The sample description and the figure in the Supplementary Materials, in which the plotted data appears, are denoted in the file name. The first column of each file is the emitted energy in eV, the second column in the is the normalized emission intensity of the dioxygen dosed Fe(II) sample ("norm" file) or the absolute intensity ("sum" file), and the third column is the normalized intensity of the pristine Fe(II) sample ("norm" file) or or the absolute intensity ("sum" file). * XES\_FeII\_FeIV\_norm\_S39.txt * XES\_FeII\_FeIV\_sum\_S39.txt <br>