Synthesis · Constructing a Redox-Active Cu(I)-Pyridyltriazine Framework for Catalytic Photoreduction of Nitrobenzenes and Carboxylic Cyclization of Alkynol with CO2

3 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: SI

Route 1: Drop Cast

S5 · 1.2.3 Photo-electrochemistry property test

Solvents300 uL ethanol and 700 uL ultra-pure water dispersion; Nafion:Ethanol = 1:3 solution

AdditivesNafion binder

Atmosphereambient drying; electrochemical tests under N2 atmosphere

Temperatureroom temperature

Timeultrasonic treatment at least 0.5 h; drying time not specified

Substrate orientationprecleaned ITO conductive electrode

Work-upDrop-cast 80 uL Cu(I)-TPT dispersion plus 40 uL Nafion solution and dry under ambient conditions.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu(I)-TPT powder	10 mg	S5 · 1.2.3 Photo-electrochemistry property test
Solvent	ethanol	300 uL dispersion plus Nafion:Ethanol solution	S5 · 1.2.3 Photo-electrochemistry property test
Solvent	ultra-pure water	700 uL	S5 · 1.2.3 Photo-electrochemistry property test
Additive	Nafion solution	40 uL · Nafion:Ethanol = 1:3	S5 · 1.2.3 Photo-electrochemistry property test

Complete recipeSource: Main

Route 2: Solvothermal

p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT

Metal precursorsCu(OAC)2.H2O (65 mg, 0.33 mmol)

Linker precursorsTPT (8 mg, 0.03 mmol); acetonitrile acts as in situ CN source

Solvents6 mL distilled water/acetonitrile = 2:1

Additives[(n-C4H9)4N]4[W10O32] (61 mg, 0.02 mmol)

Atmospheresealed Teflon-lined autoclave; atmosphere not specified

Temperature120

Time72 plus 10 h pre-stirring

Oxidant / reductantCu(II) precursor is reduced to Cu(I) during synthesis; W10O32(4-) reported to synergistically promote acetonitrile C-C cleavage

Work-upCool to room temperature; wash orange rhombus single crystals with distilled water and acetonitrile.

ActivationFor catalysis, guest CH3CN can be removed by soaking 1.00 g Cu(I)-TPT in 10 mL CH3OH for 48 h, then heating/drying at 150 C under high vacuum.

Scalability contextSingle-crystal solvothermal synthesis in a 25 mL Teflon-lined autoclave; no scale-up study reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAC)2.H2O	65 mg, 0.33 mmol	p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT
Additive	[(n-C4H9)4N]4[W10O32]	61 mg, 0.02 mmol	p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT
Linker	TPT	8 mg, 0.03 mmol	p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT
Solvent	distilled water:acetonitrile = 2:1	6 mL	p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT
Solvent	methanol for guest exchange	10 mL per 1.00 g Cu(I)-TPT	p007 / 20663 · Experimental Section - Preparation of Cu(I)-TPT

Complete recipeSource: Main

Route 3: Other

p007 / 20663 · Electronic Conductivity Measurement

Additivessilver paste; sacrificial electron donor ethanol used in illuminated test

Atmosphereambient conditions

Temperatureroom temperature

Substrate orientationglass substrate for irradiated ethanol condition

Oxidant / reductantethanol sacrificial electron donor in highest-conductivity measurement

Work-upGrind 15 mg crystal with agate mortar, prepare tablet, attach two gold wires (0.05 mm diameter) with silver paste.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu(I)-TPT crystal	15 mg	p007 / 20663 · Electronic Conductivity Measurement
Additive	silver paste	Not specified	p007 / 20663 · Electronic Conductivity Measurement
Reductant	ethanol	Not specified	p007 / 20663 · Electronic Conductivity Measurement