DOI: 10.34810/data1222
title: Replication Data for "Lead-Free Semiconductors: Phase-Evolution and Superior Stability of Multinary Tin Chalcohalides"

description: Raw data files for the research article "Lead-Free Semiconductors: Phase-Evolution and Superior Stability of Multinary Tin Chalcohalides". This paper describes the preparation and characterization of quaternary tin chalcohalides for their potential use in light harvesting applications.
description: MS Office, null
description: METHODOLOGICAL INFORMATION

1. Description of methods used for collection-generation of data: 

Powder X-ray diffraction (XRD): was measured on a Rigaku Ultima IV diffractometer (40 kV, 44 mA) using Cu Kα radiation on a zero-background quartz sample holder
 
Scanning electron microscopy (SEM): images were acquired on a JEOL JSM-IT200 scanning electron microscope

Diffuse-reflectance: spectra were collected using a SL1 Tungsten Halogen lamp (vis–IR), a SL3 Deuterium Lamp (UV), and a BLACK-Comet CSR-100 spectrometer (200–1080 nm)

Cyclic voltammetry (CV): cyclic voltammograms were collected with the potentiostat Workstation CHInstrument that was controlled by the software CHI660e V14.08

Thermogravimetric analysis/differential scanning calorimetry (TGA DSC): was performed using a Netzsch DSC/TGA (STA449 F1) and alumina (Al2O3) crucibles

Nuclear Magnetic Resonance (NMR): solid state NMR spectra were collected using 9.4 T NMR spectrometer and a 14.1 T NMR spectrometer in a 4 mm H-X-Y probe. Sn2SI2 NMR spectra was collected in a 2.5 mm probe.


2. Methods for processing the data: 

Raw XRD data files were converted to text files using PowDLL Converter. The text files were then processed and plotted in Microsoft Excel, including performing a 5-point smooth and normalization of the intensity values.

Diffuse reflectance data files were processed and plotted in Microsoft Excel, including normalization of the absorbance values.

TGA/DSC data files were processed and plotted in Microsft Excel.

SEM images were processed and analyzed using ImageJ (Schneider, C. A., Rasband, W. S., & Eliceiri, K. W. (2012). NIH Image to ImageJ: 25 years of image analysis. Nature Methods, 9(7), 671–675. doi:10.1038/nmeth.2089).

Semiquantification of phases observed in XRD patterns were determined using the reference intensity ratio (RIR) method applied within Match! (Visser, J. W.; De Wolff, P. M. Absolute Intensities. ReportVisser, J. W.; De Wolff, P. M. Absolute Intensities. Report 641.109, Technisch Physische Dienst: Delft, Netherlands, 1964.

NMR spectra were analyzed in the program " Bruker Topspin 3.6.1". The NMR spectra for Sn2BiS2I3, Sn2SI2, Sn2SbS2I3, and Sn2BiSI5 at 9.4 T was summed from previous experiments to produce the NMR spectra in figure 6. At 14.1 T, NMR spectra for Sn2SbS2I3 was summed from previous experiments to product the NMR spectra in figure 6.


3. Instrument- or software- specific information needed to interpret the data:

XRD patterns were analyzed using Match!: (Putz, H.; Brandenburg, K. Match! Version 3.11.5.203 (64-bit); Crystal Impact: Bonn, Germany, 2021, https://www.crystalimpact.941de/match.)

Cyclic voltammograms were collected with the potentiostat Workstation CHInstrument that was controlled by the software CHI660e V14.08

NMR spectra were analyzed in the program "Bruker Topspin 3.6.1".