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

Samples were prepared accroding to the following protocol:
Pentacene Thermolysis 
50?mg of as-received pentacene (Sigma Aldrich, sublimed grade, >99.9% trace metals basis) was pressed into a 5?mm diameter pellet under a pressure of 1 ton in an Ar-filled glovebox (with measured levels of O2 and H2O <1ppm). The pellet was then placed into a Pyrex tube (outer diameter ~9.5?mm, inner diameter ~5.5?mm), which was subsequently evacuated to a pressure of 2?×?10-5?mbar. The Pyrex tube was then sealed at a length of 10 – 12 cm and placed in a fan-assisted oven at room temperature. The oven was then heated to 300?°C at a heating rate of 5?°C?min-1. After heating for 24 – 300 hours, the oven was cooled to room temperature at a cooling rate of -5?°C?min-1. 
Heating at slightly lower temperatures (280 – 290?°C) yields the same reaction, albeit at a much reduced rate, necessitating heating times of over 1000 hours to achieve maximum conversion from pentacene to HBP. Heating pentacene at 320 °C failed to isolate HBP, instead a mixture containing only amorphous material and 2HP:P co-crystals were produced.  
Sublimation 
A subsequent sublimation step was used to separate crystalline, hydrogenated products from the amorphous, hydrogen-poor material which exhibits low volatility. The mixture was ground into a fine powder using a pestle and mortar and loaded into narrow Pyrex tube (outer diameter ~5?mm, inner diameter ~3?mm, length ~6 cm), which was then itself loaded into a Pyrex tube (outer diameter ~9.5?mm, inner diameter ~5.5?mm). The tube was then evacuated to 2?×?10-5?mbar and sealed at a length of ~30 cm. The tube was then placed in a three-zone tube furnace such that the sample was at the centre of the furnace and the opposing end was at room temperature (Figure S1a). The centre of the furnace was heated to 300 °C at a heating rate of 5 °C min-1. A thermocouple was used to determine the temperature profile along the length of the tube furnace (Figure S1b), which shows a gradient from 300 °C at the centre to 120 °C at the edge of the furnace. After 18 hours the furnace was cooled at a rate of 5 °C min-1 to room temperature. After heating, crystals of P and 2HP:P co-crystals were found to be sublimed at the cool end of the tube (Figure S1c). 

Powder X-ray diffraction:
Synchrotron powder X-ray diffraction patterns collected on Beamline I11 at Diamond Light Source. Data in a 2-column format (2theta, counts). All data were collected at ambient temperature. All data were collected using the wide-angle position sensitive detector, with a Si-calibrated wavelength of 0.82612(1) Angstroms and zero error of -0.0902(1) degrees. For samples containing internal standards Synchrotron powder X-ray diffraction patterns collected on Beamline I11 at Diamond Light Source. Data in a 2-column format (2theta, counts). All data were collected at ambient temperature. All data were collected using the wide-angle position sensitive detector, with a Si-calibrated wavelength of 0.82608(1) Angstroms and zero error of -0.0275(1) degrees

Electron ionised mass spectrometry was conducted at the EPSRC UK National Mass Spectrometry Facility using a Thermo Scientific DSQ-II. Data in two-column format (m/z; Normalised intensity, arbitrary units).

Gas chromatography (GC) to detect any hydrogen emission from the sample was carried out using an Agilent 6890N with He as the carrier gas. Data are in a two-column format: retention time (minutes) and signal (mV)

Raman spectroscopy data, collected using Renishaw inVia Spectrometer with a 785 nm excitation laser. Data in two column format (Raman shift, cm-1; Intensity, arbitrary units).