Spectroscopy — From 2D to 3D: Postsynthetic Pillar Insertion in Electrically Conductive MOF

3 measurement groups · 8 results

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

Digestive 1H NMR spectroscopy

Nuclear magnetic resonance

Cu-THQ-BPY, Cu2+:BPY feed ratio 1:1 · Powder

5 mg sample digested in 0.5 mL D2O and 0.1 mL HCl (20 wt% in D2O), filtered through 0.45 um nylon membrane; Bruker AV-III 300 MHz.

Temperature: 298
Geometry: Solution NMR after acid digestion
Context: Cu-THQ-BPY feed-ratio series.
Measurement source: SI p.S9 · NMR spectroscopy · Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Experimental THQ:BPY molar ratio for 1:1 feedMarked as a best value within this paper	2:3.1	0.6452 THQ/BPY	—	SI Table Exact Reported	SI p.S9 · NMR spectroscopy · Table S2
Experimental THQ:BPY molar ratio for 1:2 feedMarked as a best value within this paper	1:2.8	0.3571 THQ/BPY	—	SI Table Exact Reported	SI p.S9 · NMR spectroscopy · Table S2
Experimental THQ:BPY molar ratio for 2:1 feedMarked as a best value within this paper	3.5:3	1.1667 THQ/BPY	—	SI Table Exact Reported	SI p.S9 · NMR spectroscopy · Table S2

UV-vis-NIR spectroscopy, Tauc analysis, and cyclic-voltammetry-derived LUMO estimate

UV-visible and optical absorption spectroscopy Voltammetry

Cu-THQ-BPY, Cu2+:BPY feed ratio 1:1 · Powder

MOFs dispersed in isopropyl alcohol for UV-vis-NIR; LUMO measured with 0.01 M Ag/AgNO3 in 0.1 M TBAPF6 acetonitrile reference, Pt counter, glassy carbon working electrode, 0.1 M TBAPF6 acetonitrile electrolyte, Fc/Fc+ reference.

Geometry: Dispersed optical sample and MOF on glassy carbon electrode
Context: Cu-THQ and Cu-THQ-BPY electronic structure comparison.
Measurement source: SI pp.S11-S12 · UV-Vis-NIR spectroscopy; Measurement of LUMO by cyclic voltammetry · Figures S10-S13

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Optical bandgap change after BPY insertion	No significant changes throughout the series	—	—	Text Qualitative	main p.4 · Results and Discussion · Figure S11
Strong absorption maximum/feature	650 nm extending to near-infrared	—	—	Text Rounded Reported	main p.4 · Results and Discussion · Figure S10

Cu 2p3/2 XPS and ATR FT-IR spectroscopy

Infrared spectroscopy X-ray photoelectron spectroscopy

Cu-THQ-BPY, Cu2+:BPY feed ratio 1:1 · Powder

XPS using K-alpha spectrometer with Al Kalpha source; ATR FT-IR on Cary 630.

Geometry: Powder/solid samples
Context: Cu-THQ compared with Cu-THQ-BPY.
Measurement source: main pp.3-4 · Results and Discussion · Figure 3b-c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
BPY FT-IR band shift upon coordination	1585 to 1608 cm-1	—	—	Text Rounded Reported	main p.4 · Results and Discussion · Figure 3c
Cu-THQ dominant Cu 2p3/2 XPS peak	approximately 933 eV	—	—	Text Approximate	main p.3 · Results and Discussion · Figure 3b
Reduced copper character after BPY insertion	notable increase around 932 eV	—	—	Text Approximate	main p.4 · Results and Discussion · Figure 3b