Spectroscopy — Highly Selective CO2 Electroreduction to CH4 by In Situ Generated Cu2O Single-Type Sites on a Conductive MOF: Stabilizing Key Intermediates with Hydrogen Bonding

4 measurement groups · 19 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Cu2O@CuHHTP, -1.2 V 30 min · Electrode

HHTP, CuHHTP, and Cu2O@CuHHTP comparison

Geometry: VERTEX70 (Bruker)
Context: linker, pristine MOF and target composite
Measurement source: p007 / SI p6 · Supporting Figures and Tables · Figure S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
HHTP hydroxyl FTIR peak	1626 cm^-1	—	—	Caption Exact Reported	p007 / SI p6 · Figure S4
HHTP hydroxyl FTIR peak	3427 cm^-1	—	—	Caption Exact Reported	p007 / SI p6 · Figure S4

Cu2O@CuHHTP, -1.2 V 30 min · Electrode

-1.4 V vs RHE in CO2-saturated 0.1 M KCl/0.1 M KHCO3 electrolyte; home-made cell

Atmosphere: CO2
Geometry: ATR-FTIR cell with Ge crystal
Context: target composite
Measurement source: p006 / 23646 · Results and Discussion · Figure 4a-c; Figure S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
*CHO intermediate peak	1033 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*OCH3 intermediate peak	1160 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*OH deformation of COOH**	1250 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*C-O stretch of COOH**	1334 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*symmetric stretch of COOH**	1400 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*CH2O intermediate peak	1473 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*asymmetric stretch of COOH**	1565 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c
*CO intermediate peak	2080 cm^-1	—	—	Text Exact Reported	p005-p006 / 23645-23646 · Figure 4a-c

Cu2O@CuHHTP, -1.2 V 30 min · Electrode

synchrotron XAFS at BL14W1

Geometry: Shanghai Synchrotron Radiation Facility BL14W1
Context: pristine CuHHTP and target composite
Measurement source: p003-p004 / 23643-23644 · Results and Discussion · Figure 1e-f

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu-O EXAFS scattering path	1.5 A	—	—	Text Exact Reported	p004 / 23644 · Figure 1f
Cu-Cu EXAFS scattering in Cu2O@CuHHTP	No Cu-Cu peak at 2.21 A observed	—	—	Text Qualitative	p004 / 23644 · Figure 1f
Cu+ XANES feature in Cu2O@CuHHTP	8982.1 eV	—	—	Text Exact Reported	p003 / 23643 · Figure 1e

Cu2O@CuHHTP, -1.2 V 30 min · Electrode

Cu2O@CuHHTP quickly collected and stored in sealed Schlenk tube under nitrogen before XPS

Atmosphere: nitrogen storage before measurement
Geometry: ESCALAB 250Xi XPS
Context: pristine CuHHTP versus electroreduced composite
Measurement source: p003 / 23643 · Results and Discussion · Figure 1c-d; Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu2+ LMM Auger peak in CuHHTP	570.4 eV	—	—	Text Exact Reported	p003 / 23643 · Figure 1d
Cu+ LMM Auger peak after electroreduction	569.5 eV	—	—	Text Exact Reported	p003 / 23643 · Figure 1d
Cu0 LMM Auger contribution	Cu0 peak at 567.7 eV negligible	—	—	Text Qualitative	p003 / 23643 · Figure 1d
Cu2+ 2p binding energy	934.4 eV	—	—	Text Exact Reported	p003 / 23643 · Figure 1c
Cu+ or Cu0 2p binding energy in Cu2O@CuHHTP	933.1 eV	—	—	Text Exact Reported	p003 / 23643 · Figure 1c
Fraction of Cu centres reduced to Cu2O	ca. 33%	—	—	Text Approximate	p003 / 23643 · Figure S3