3D ED data for the crystal structure in the title publication (https://doi.org/10.31635/ccschem.025.202507155). Data were collected using continuous rotation in selected area mode. The table below summarizes generic data collection parameters for the data collection. General Collection site University of Southampton, NCS/NEDF Sample label(s) 2024NCS0111 Crystal structure deposit CSD 2415735 Instrumental Instrument Rigaku XtaLAB Synergy-ED, electron diffractometer Radiation source LaB6 Accelerating voltage [kV] 200 Wavelength [Å] 0.0251 Probe type Parallel beam (SAED) Beam convergence Parallel beam Detector Hybrid Pixel Array Detector Number of pixels 775 × 385 Pixel size [µm] 100 Hardware binning 1 Experimental Data type electron diffraction data - 3D ED Data collection method continuous rotation electron diffraction Collection temperature [K] 175(5) Sample description Name Na2_26NDC Chemical composition C12 H6 Na2 O4 Sample source synthesis Grid lacey carbon coated copper grid, 200 mesh (Agar Scientific, UK) Sample preparation sample gently ground between glass slides, grid dabbed, cryo-transfer at 175(5) K Sample holder GATAN Elsa cryo-transfer holder 698 Software & Files Software for data collection CrysAlisPro system (CCD 43.107a 64-bit (release 07-02-2024)) Software for data processing CrysAlisPro 1.171.44.82a (Rigaku OD, 2024) Diffraction frame folders ./frames/xxx.rodhypix./frames/TIFF/xxx.tiff Diffraction frame file format .rodhypix.tiff (converted with CrysAlisPro) Additional files CrysAlisPro files: ./expinfo/./expinfo/exp_XXXX_datacoll.ini ./plots_dc.plots_dc/exp_XXX_hypix.dat.plots_dc/exp_XXX_Jeol_MicroED.dat.plots_dc/exp_XXX_primarybeam.dat.plots_dc/exp_XXX_primarybeam_0.jpg ./CrysalisExpSettings.ini./exp_XXX.par./exp_XXX.run./exp_XXX_videosetup.ini./new.ccd