1：Experimental Design and Method Selection:

The superlattice was synthesized using an antisolvent diffusion method with PbI2 and EtDAB in DMF, diffused into CH3CN atmosphere. Characterization methods included single crystal X-ray diffraction, powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), electron spin resonance (ESR), UV/Vis/NIR spectroscopy, X-ray photoelectron spectroscopy (XPS), and electrical conductivity measurements using two-probe and four-probe methods on pressed pellets and single crystals.

2：Sample Selection and Data Sources:

Samples included pure PbI2, the radical form (1-G), and the non-radical form (1-Y) of the superlattice. Data were obtained from synthesized materials and standard analytical techniques.

3：List of Experimental Equipment and Materials:

PbI2, EtDAB (tetraethylbenzidine), DMF, CH3CN, X-ray diffractometer, TEM, ESR spectrometer, UV/Vis/NIR spectrometer, XPS instrument, conductivity measurement setup with electrodes, Xe lamp with bandpass filters, OPO laser.

4：Experimental Procedures and Operational Workflow:

Dissolve PbI2 and EtDAB in DMF, diffuse into CH3CN atmosphere for 2 weeks to obtain 1-G. Characterize structure with PXRD and TEM. Measure ESR, UV/Vis/NIR spectra, and XPS for electronic properties. Measure conductivity in vacuum using pressed pellets and single crystals with evaporated electrodes. Measure photoconductivity using Xe lamp and OPO laser with various wavelengths.

5：Data Analysis Methods:

Analyze diffraction data for crystal structure, ESR for radical presence, spectroscopy for absorption bands, XPS for elemental states, and I-V curves for conductivity. Use statistical methods for reproducibility across multiple samples.