Readme file for data relating to Control of Ionic Conductivity by Lithium Distribution in Cubic Oxide Argyrodites Li6+xP1–xSixO5Cl

Samples were prepared according to the following protocoll: 

The starting materials: Li4SiO4, Li3PO4, Li2O, and LiCl were vacuum dried overnight (under 10-4 mbar) before placing them in an Ar-filled glove box. 
All precursors and resulting powders were then handled in an Ar-filled glove box. Li4SiO4, Li3PO4, Li2O, and LiCl were mixed in the stoichiometric 
ratio using ball milling under an Ar atmosphere. The resulting powder was then pressed into 5 mm diameter pellets and placed into alumina crucible.
The crucible was placed in a quartz tube which was sealed under vacuum (<10-4 mbar). The tubes were heated to 823 K for x = 0.1, 0.3, 0.5, 0.6, 0.7, 
0.75, 0.8, 0.85, and 0.9, and to 873 K for x = 1 at a ramp rate of 5 K min –1, held at the reaction temperature for 3 h and cooled . Once cool, the 
quartz tube was opened inside the Ar glovebox, and the powder ground in a pestle and at a rate of 5 K min–1. The quartz tubes were opened inside the 
Ar dry box, and the powders were ground in an agate mortar for further characterisation.  


X-ray Diffraction: 
High resolution synchotron data was ccollected at on Beamline I11 at Diamond Light Source in transmission geometry using a multi analyser 
crystal (MAC)detetor (room temperatuer measurement) and a point sensitive (PSD) detector (Variable temperature measurements), all XRD data
is presented in a 3 column format: 2Theta, counts and error. 


Single crystal Diffraction:

Single crystal diffraction data was collected at 100 K. 300 K and 500 K on a twinned crystal using a Rigaku MicroMax-007 HF X-ray generator equipped with a 
Mo-Ka rotating-anode microfocus source and a Saturn 724+ detector. Data is presented as .img files.

AC Impedance Spectroscopy:

Data was collected on an impedance analyser (Keysight impedance analyser E4990A) and using a sputtered gold coating of 300 nm 
thickness as the ion blocking electrodes. Measurements were performed from 25 °C - 150 °C in 25°C steps. Data is presented in 4 column format: 
frequency (Hz), Z' (Ohmcm-1), Z''(Ohmcm-1) and temperature (°C)

Nuclear Magentic Resonace Spectroscopy:

6Li, 29Si and 31P magic-angle spinning (MAS) NMR spectra were recorded with a 4mm HXY MAS probe in double resonance mode on a Bruker 9.4 T Avance III HD 
spectrometer. 
Variable temperature 7Li NMR experiments were recorded with a 4mm HX High-Temperature MAS Probe on a 9.4 T Bruker Avance III HD spectrometer.


DC Polarization:

DC polarization data was collected at 25 °C on a Au|Li6+xP1-xSixO5Cl|Au symmetric cell by applying constant potentials of 0.3, 0.4, 0.5, 0.6,0.8 and 
1 V and monitoring the current variation with time. Data is presented in 3 column format: time(s),  current (A) and Voltage applied (V)

Platting and Stripping:

Platting and stripping data was collected on a symmetric Li|Li6.75P0.25Si0.75O5Cl|Li cell. Ggalvanostatic Li plating/stripping tests were performed at 298 K
at a current density of 20 µA cm-2 (20 min per half-cycle) using a BioLogic VSP 300 potentiostat. Data is presented in xxxxx

Differential Scanning Calorimetry:

Data was collected from 16.3 mg of powdered sample in a 40 µL aluminium crucible cold-welded under Ar atmosphere (<0.1 ppm O2, H2O) 
using a Netzsch DSC 404 F1 differential scanning calorimeter. Data were collected from 298 K to 523 K at heating and cooling rates of 10 K min–1 under a flow of helium (50 mL min–1).
Data is presented in 4 column fromat: Temp./°C; Time/min; DSC/(uV/mg); Sensit./(uV/mW)