Spectroscopy

CV and UV-vis-derived HOMO/LUMO/band-gap estimates

UV-visible and optical absorption spectroscopy Voltammetry

NiCB@NU-1000 powder · Powder

CV of NiCB and TBAPy solutions converted to NHE by adding 0.21 V; UV-vis absorption used for TBAPy band gap; NU-1000 values from previous electrochemically addressable thin-film and diffuse-reflectance estimates.

Geometry: Pt working electrode for solution CV
Context: Energy alignment rationale for NiCB loading into NU-1000.
Measurement source: S8 · S2 · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Band gap of NU-1000	2.57 eV	—	—	SI Table Exact Reported	S8 · S2 · Table S1
Band gap of TBAPy linker	2.92 eV	—	—	SI Table Exact Reported	S8 · S2 · Table S1
HOMO of NU-1000	1.43 E vs NHE	—	—	SI Table Exact Reported	S8 · S2 · Table S1
HOMO of TBAPy linker	1.23 E vs NHE	—	—	SI Table Exact Reported	S8 · S2 · Table S1
LUMO of NiCB	0.57 E vs NHE	—	—	SI Table Exact Reported	S8 · S2 · Table S1

steady-state emission and diffuse-reflectance UV-vis

UV-visible and optical absorption spectroscopy

NiCB@NU-1000 powder · Powder

Emission excited at 380 nm and monitored 400-700 nm; diffuse reflectance UV-vis collected from 1600 to 360 nm using PTFE baseline.

Geometry: finely ground MOF crystals
Context: NU-1000, bulk NiCB, and NiCB@NU-1000 compared.
Measurement source: S15 · S7 · Figures S6-S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
NiCB@NU-1000 charge-transfer band range	between about 950 nm and 550 nm	—	—	Text Range	S15 · S7 · Figure S7
Charge-transfer-band-derived band gap	about 1.3 eV	—	—	Text Approximate	S15 · S7 · Figure S7
NU-1000 emission maximum	500 nm	—	—	Text Rounded Reported	S15 · S7 · Figure S6

2 measurement groups · 8 results