Synthesis · Two dimensional Conjugated Metal–Organic Frameworks with Multiple Redox-Active Sites towards High-Performance Sodium-Ion Battery

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S4

Metal precursors(C5H4F3O2)2Cu (7.4 mg, 0.02 mmol, 2 equiv.)

Linker precursors8OH-TPQ (6.1 mg, 0.01 mmol, 1 equiv.) with in situ conversion to DDQP analogue

SolventsDMF/H2O/MeOH (1.0 mL/1.5 mL/0.5 mL, 2:3:1)

Additivesnone specified

Atmospheresealed vial; atmosphere not specified

Temperature85

Time48

Substrate orientationnot applicable

Oxidant / reductantCu2+ source; no separate oxidant/reductant in MOF recipe

Work-upsonicate 30 min; heat; cool; isolate precipitate by filtration; wash with DMF, deionized water and acetone

Activationdried under vacuum; gas-sorption samples activated at 80 deg C for 12 h under vacuum (10^-5 bar)

Scalability contextPart of the one-pot synthesis strategy for analogous 2D c-MOFs.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	8OH-TPQ	6.1 mg · 0.01 mmol, 1 equiv.	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S4
Metal Source	(C5H4F3O2)2Cu	7.4 mg · 0.02 mmol, 2 equiv.	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S4
Solvent	DMF/H2O/MeOH	1.0 mL/1.5 mL/0.5 mL · 2:3:1	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S4

Complete recipeSource: Both

Route 2: Solvothermal

S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S3

Metal precursorsCu(NO3)2.3H2O (12 mg, 0.05 mmol, 2.5 equiv.)

Linker precursors8OH-TPAQ (12.8 mg, 0.02 mmol, 1 equiv.) with in situ conversion to TBPQ analogue

SolventsDMF/H2O (2 mL/0.5 mL, v/v = 4:1)

Additivesnone specified

Atmospheresealed vial; atmosphere not specified

Temperature85

Time72

Substrate orientationnot applicable

Oxidant / reductantCu2+ and DMF implicated as facilitating cyclodehydrogenation; no separate oxidant in MOF recipe

Work-upcool to room temperature; isolate precipitate by centrifugation; wash thoroughly with DMF, deionized water and acetone

Activationdried under vacuum; gas-sorption samples activated at 80 deg C for 12 h under vacuum (10^-5 bar)

Scalability contextPart of the one-pot synthesis strategy for analogous 2D c-MOFs.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	8OH-TPAQ	12.8 mg · 0.02 mmol, 1 equiv.	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S3
Metal Source	Cu(NO3)2.3H2O	12 mg · 0.05 mmol, 2.5 equiv.	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S3
Solvent	DMF/H2O	2 mL/0.5 mL · v/v = 4:1	S6 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S3

Complete recipeSource: Both

Route 3: Solvothermal

S5 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S2

Metal precursorsCu(NO3)2.3H2O (7.3 mg, 0.03 mmol, 1.5 equiv.)

Linker precursors8OH-TPPQ (13.0 mg, 0.02 mmol, 1 equiv.) dispersed in DMF; in situ Scholl cyclodehydrogenation/coordination assembly forms TTPQ framework

SolventsDMF (2.0 mL) and H2O (0.5 mL)

Additivesnone specified

Atmospheresealed screwed vial; atmosphere not specified

Temperature85

Time72

Substrate orientationnot applicable

Oxidant / reductantCu2+ precursor probably acts as Lewis acid/electron acceptor promoting dehydrogenation; no separate oxidant in MOF recipe

Work-upcool to room temperature; isolate precipitate by filtration; wash with DMF, deionized water and acetone

Activationdried under vacuum; gas-sorption samples activated at 80 deg C for 12 h under vacuum (10^-5 bar)

Scalability contextMain conclusion says the one-pot strategy offers convenience for large-scale synthesis and cost control.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	8OH-TPPQ	13.0 mg · 0.02 mmol, 1 equiv.	S5 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S2
Metal Source	Cu(NO3)2.3H2O	7.3 mg · 0.03 mmol, 1.5 equiv.	S5 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S2
Solvent	DMF	2.0 mL	S5 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S2
Solvent	H2O	0.5 mL	S5 · Section 2.2 Synthesis of 2D c-MOFs · Scheme S2