Raw and processed anomalous diffraction data for crystals of metal-free Geobacillus kaustophilus R2-like ligand-binding oxidase (R2lox) soaked with 5 mM each MnCl2, (NH4)2Fe(SO4)2 and CoCl2 or ZnCl2. Data were collected on two crystals each after soaking with Mn, Fe and Co or Mn, Fe and Zn, respectively. For each crystal, one dataset each was collected at the Fe K edge (7162 eV), Mn K edge (6589 eV) and Co K edge (7721 eV) or Zn K edge (9664 eV; X-ray energies corresponding to the theoretical K edge + 50 eV). Data were collected at 100 K on a Pilatus 6M detector at beamline X06SA of the Swiss Light Source (SLS, Villigen, Switzerland) on September 23, 2012, and processed with XDS and XSCALE. All raw and processed diffraction data for each crystal are compressed into one file.

We thank Matthew D. Bennett and the staff at beamline X06SA/SLS for assistance with X-ray data collection. Financial support was provided by the Swedish Research Council (2016-03770 to J.J.G. and 2017-04018 to M.H.), the European Research Council (HIGH-GEAR 724394), the Knut and Alice Wallenberg Foundation (2012.0233 and 2017.0275), and the European Community's Seventh Framework Programme (FP7/2007-2013) under grant agreement n.°283570 (for BioStruct-X) (M.H.).