Readme file for data relating to The reactivity of solid rubrene with potassium: competition between intercalation and molecular decomposition:

All data files are named according to the sample designation described in the published paper; i.e. "potassium precursor"-"K:rubrene ratio"-"reaction temperature in ºC", e.g. the reaction of 2 equivalents of potassium hydride with rubrene at 250ºC will be KH-2-250

Sample preparation. All reagents and samples were stored and handled in an argon-filled glove box (O2 and H2O <1 ppm). All reactions were carried out in Pyrex ampoules with an internal diameter of 5 mm and an approximate length of 10 cm and sealed under vacuum (<10-4 mbar). Pre-reactions were performed on the mixture (ca. 80 mg) of K chunks (99.99% from Sigma Al-drich) and rubrene powder (sublimed grade, 99.9% from TCI Chemicals) at 210 °C (see SI) with a heating rate of 1 °C/min and dwelling time of 3 days. All other reactions were performed on pellets (ca. 80 mg each) of materials from pre-reaction, or mixtures of rubrene and KH (Sigma Aldrich, washed with anhydrous pentane under inert atmosphere and containing minor unidenti-fied impurities, see Figure S7) at 210, 230, 250 °C with a heating rate of 1°C/min. Reactions were performed with four different starting K:R ratios of 1:1, 2:1, 3:1 and 4:1. All reactions of pellets were performed first for 3 days, and then the products were reground and repelletized and then reacted for an additional 3-day at the same temperatures to yield the final products.


Powder X-ray diffraction. All PXRD data were collected in capillary mode at room temperature. PXRD data collections were first carried out us-ing a laboratory X-ray diffractometer (Bruker D8, with monochromated MoKa, ?=0.71073 Å. Samples exhibiting the best crystallinity were chosen for synchrotron PXRD on the I11 beam line at Diamond Light Source (?=0.82566(1) Å) at room temperature using 0.5 mm or 0.7 mm di-ameter borosilicate capillaries. All structural anal-ysis on PXRD data (including indexing, Pawley fitting, simulated annealing and Rietveld refine-ments) were performed using Topas Academic (Version 5).


NMR. THF-d8 was dried with Na metal. NMR tubes were purged with high purity N2 gas using Schlenk techniques prior to sample preparation. Sample powders of ca. 16 mg were loaded into NMR tubes with Schlenk connectors inside glove boxes. 0.5 ml of dried THF-d8 was then trans-ferred into the NMR tube. The solution was fro-zen by submersing the bottom of the NMR tube in liquid N2. The tube was evacuated and sealed using a micro torch. NMR spectra were collected immediately on a Bruker AVANCE 400 MHz NMR spectrometer once the solution had thawed. The NMR spectra of KH-1-250 were collected using anhydrous Toluene-d8 (anhy-drous, Sigma Aldrich). All analyses of NMR spectra were performed using MestReNova (version 11).

Data are in .csv format and so can be opened by any data analysis software.