Synthesis · Synthesis and Electric Properties of a Two-Dimensional Metal-Organic Framework Based on Phthalocyanine

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Drop Cast

S2 · Discharge and charge measurement · Figures 4, 5, S5

Solventswater in commercial PTFE dispersion

Additivescarbon black; PTFE binder

AtmosphereAr-filled glove box for cell fabrication

Temperature80 drying

Substrate orientationstainless mesh current collector

Work-upmixture deposited onto stainless mesh; dried at 80 C under vacuum; assembled with lithium foil anode, glass separator, and LiPF6 EC/DMC electrolyte

Activationdried at 80 C under vacuum before cell assembly

Scalability contextCathode weight 111.4 mg; exact mass of Cu-CuPc on stainless mesh 9.99 mg.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-CuPc	exact mass on stainless mesh 9.99 mg	S2 · Discharge and charge measurement · Figures 4, 5, S5
Additive	carbon black (KETJENBLACK EC600JD)	1 part by weight	S2 · Discharge and charge measurement · Figures 4, 5, S5
Additive	PTFE dispersion (Aldrich, 60 wt% in water)	SI: 1 part by weight; main caption: 0.6 part by weight · 60 wt% in water	S2 · Discharge and charge measurement · Figures 4, 5, S5
Electrolyte	LiPF6 in ethylene carbonate and dimethyl carbonate	1 M; EC:DMC 1:2 by volume	S2 · Discharge and charge measurement · Figures 4, 5, S5

Complete recipeSource: Both

Route 2: Solvothermal

S1 · Synthesis of 2D-MOF Cu-CuPc

Metal precursorsCu(II)(CF3acac)2 / copper(II) trifluoroacetylacetonate

Linker precursorsCuPcOH

SolventsDMF and water

Additives13.4 M aqueous NH3 solution

Temperature120

Time36

Work-upsolid filtered by PTFE filter, washed with DMF, decanted with DMF until colourless, soaked in fresh acetone overnight, filtered, washed with acetone, dried under reduced pressure

Activationfor gas adsorption, samples were activated at 80 C under vacuum overnight

Scalability contextSI reports 104 mg CuPcOH and 109 mg Cu(II)(CF3acac)2; reported product mass is '87 g' with 67% yield, likely a typographical mass-unit error but preserved in notes.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	CuPcOH	104 mg, 0.15 mmol	S1 · Synthesis of 2D-MOF Cu-CuPc
Solvent	DMF	81 ml plus 9 ml for Cu(II)(CF3acac)2 solution	S1 · Synthesis of 2D-MOF Cu-CuPc
Base	aqueous solution of NH3	6.6 ml, 89 mmol · 13.4 M	S1 · Synthesis of 2D-MOF Cu-CuPc
Solvent	water	90 ml	S1 · Synthesis of 2D-MOF Cu-CuPc
Metal Source	Cu(II)(CF3acac)2	109 mg, 0.30 mmol	S1 · Synthesis of 2D-MOF Cu-CuPc

Complete recipeSource: SI

Route 3: Other

S1 · Synthesis of CuPcOH

Metal precursorsCu(II) 2,3,9,10,16,17,23,24-octakisoctyloxy-29H,31H-phthalocyanine

Solventsdry dichloromethane; MeOH and water for quench/wash

Additivesboron tribromide, 17% in dichloromethane, ca. 1 M

AtmosphereN2

Temperaturereflux after 2 h stirring; cooled to room temperature

Time2 h stirring plus 20 h reflux

Oxidant / reductantboron tribromide dealkylation reagent

Work-upquenched with MeOH and water; filtered; washed with MeOH, water and dichloromethane; centrifuged repeatedly with water, MeOH and dichloromethane until supernatant almost transparent

Activationdried under reduced pressure

Scalability context1 g precursor scale; reported 75% yield.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	Cu(II) 2,3,9,10,16,17,23,24-octakisoctyloxy-29H,31H-phthalocyanine	1 g, 0.62 mmol	S1 · Synthesis of CuPcOH
Solvent	dry dichloromethane	300 ml	S1 · Synthesis of CuPcOH
Additive	Boron tribromide solution	25 ml, 25 mmol · 1 M	S1 · Synthesis of CuPcOH