Diffraction Structure

Post-electrolysis PXRD and XPS

X-ray photoelectron spectroscopy X-ray diffraction and scattering

KGF-9 electrode after electrolysis · Electrode

KGF-9/KB electrode after electrolysis at -0.6 to -1.0 V vs RHE for 120 min under CO2 or Ar.

Atmosphere: CO2 and Ar
Geometry: post-mortem electrode characterisation
Context: Derived electrode state after electrochemical operation.
Measurement source: S-12-S-14 · Supporting Information · Figures S16-S20

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
No KGF-9 structural transformation without KB	bare KGF-9 electrode remained unchanged after electrolysis	—	—	Text Qualitative	7 · 2.6 Structure Transformation during Electrocatalysis · Figure S16
Post-electrolysis phase after -0.8 V with KB	KGF-9 transformed to PbCO3/Pb3(CO3)2(OH)2 mixed phase	—	—	Text Qualitative	7 · 2.6 Structure Transformation during Electrocatalysis · Figure S16
Post-electrolysis Pb-CO3 Pb 4f binding energies	4f5/2 144.8 eV and 4f7/2 139.9 eV	144.8 eV Pb 4f5/2	—	Text Exact Reported	8 · 2.6 Structure Transformation during Electrocatalysis · Figure S19
Post-electrolysis Pb-OH Pb 4f binding energies	4f5/2 144.1 eV and 4f7/2 139.2 eV	144.1 eV Pb 4f5/2	—	Text Exact Reported	8 · 2.6 Structure Transformation during Electrocatalysis · Figure S19

Powder X-ray diffraction (PXRD), Rigaku MiniFlex600, Cu-Kalpha

X-ray diffraction and scattering

MW_x KGF-9/KGF-17 comparison powder series · Powder

PXRD patterns compared for simulated/ordinary KGF-9, KGF-17 and MW_x powders.

Context: Pristine and mixed CP powder phase comparison.
Measurement source: 2 · 2.1 Physicochemical Properties · Figure 1A

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
MW sample crystallite size by Scherrer equation	ca. 32-54 nm	—	range 32-54 nm	Text Range	2 · 2.1 Physicochemical Properties · Table S1
FWHM of prominent 2theta = 15.4 deg reflection for MW KGF-9Marked as a best value within this paper	0.15-0.18 deg	—	range 0.15-0.18 deg	Text Range	2 · 2.1 Physicochemical Properties
FWHM of prominent reflection for ordinary KGF-9	0.24 deg	—	—	Text Exact Reported	2 · 2.1 Physicochemical Properties
KGF-9 formation onset during MW synthesis	KGF-9 begins to form within 10 min	—	—	Text Rounded Reported	2 · 2.1 Physicochemical Properties · Figure 1A
Phase-pure KGF-9 MW synthesis thresholdMarked as a best value within this paper	Phase-pure KGF-9 at 60, 90, and 120 min	—	—	Text Exact Reported	2 · 2.1 Physicochemical Properties · Figure 1A
MW-10 KGF-17 (010) 2theta	10.9 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-10 KGF-17 (010) FWHM	0.2302 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-10 KGF-17 (010) crystallite size	36.2 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-10 KGF-9 (021) 2theta	15.6 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-10 KGF-9 (021) FWHM	0.1548 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-10 KGF-9 (021) crystallite size	54.1 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-120 KGF-9 (021) 2theta	15.4 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-120 KGF-9 (021) FWHM	0.1543 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-120 KGF-9 (021) crystallite size	54.3 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-2 KGF-17 (010) 2theta	10.8 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-2 KGF-17 (010) FWHM	0.2365 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-2 KGF-17 (010) crystallite size	35.2 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-17 (010) 2theta	10.8 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-17 (010) FWHM	0.2583 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-17 (010) crystallite size	32.3 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-9 (021) 2theta	15.4 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-9 (021) FWHM	0.1823 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-30 KGF-9 (021) crystallite size	45.9 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-60 KGF-9 (021) 2theta	15.4 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-60 KGF-9 (021) FWHM	0.1795 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-60 KGF-9 (021) crystallite size	46.7 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-90 KGF-9 (021) 2theta	15.4 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-90 KGF-9 (021) FWHM	0.1695 deg	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1
MW-90 KGF-9 (021) crystallite size	49.2 nm	—	—	SI Table Exact Reported	S-2 · Supporting Information · Table S1

PXRD stability test after soaking

X-ray diffraction and scattering

MW_60 fibrous KGF-9 powder · Powder

MW_60 soaked in water, 0.1 M NaOH, 0.5 M KHCO3, DMSO and 0.1 M HCl.

Context: Pristine MW_60 KGF-9 stability before photocatalysis.
Measurement source: S-7 · Supporting Information · Figure S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
MW_60 acid instability	structural change in 0.1 M HCl	—	—	Text Qualitative	3 · 2.2 Photocatalytic CO2 Reduction Activity · Figure S5
MW_60 chemical stability in neutral/basic/DMSO media	maintained KGF-9 structure after water, 0.1 M NaOH, 0.5 M KHCO3 and DMSO soaking	—	—	Text Qualitative	3 · 2.2 Photocatalytic CO2 Reduction Activity · Figure S5

3 measurement groups · 35 results