Synthesis · Iron-Based 2D Conductive Metal-Organic Framework Nanostructure with Enhanced Pseudocapacitance

3 structured synthesis routes

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

Complete recipeSource: SI

SI p.S2-S3 · Synthesis of Cu-HHTP · Figure S12

Metal precursorsCuSO4.5H2O (41 mg, 0.164 mmol)

Linker precursorsHHTP (23.3 mg, 0.72 mmol as reported)

Solvents0.3 mL DMF + 2.4 mL H2O for ligand; 0.9 mL H2O for metal salt

AtmosphereNot specified

Temperature80

Time6

Work-upCentrifuged and washed with water, methanol and acetone twice each; dried in vacuum oven for 1 h at 60 deg C before PXRD.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuSO4.5H2O	41 mg, 0.164 mmol	SI p.S2-S3 · Synthesis of Cu-HHTP · Figure S12
Linker	HHTP	23.3 mg, 0.72 mmol	SI p.S2-S3 · Synthesis of Cu-HHTP · Figure S12
Solvent	DMF	0.3 mL	SI p.S2-S3 · Synthesis of Cu-HHTP · Figure S12
Solvent	H2O	2.4 mL with ligand plus 0.9 mL with metal salt	SI p.S2-S3 · Synthesis of Cu-HHTP · Figure S12

Complete recipeSource: Both

SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7

Metal precursorsFe(OAc)2 (13.138 mg, 0.075 mmol)

Linker precursorsHHTP (36.72 mg, 0.113 mmol)

Solvents1:1 water:DMF mixture; text says HHTP dissolved in '10 9.6 mL' and Fe(OAc)2 in 10 mL solvent mixture

Additives293 uL of 1 M sodium acetate aqueous solution, 5 equivalents to HHTP

AtmosphereN2-degassed solutions; metal salt solution added to ligand solution under inert conditions; reaction under nitrogen

Temperature100

Time3

Oxidant / reductantOxygen excluded; oxygen-control experiments varied 0%, 50% and 100% O2 solvent fractions.

Work-upCooled to room temperature; washed and centrifuged with acetone (3 x 30 mL); dried in vacuum oven for 1 h at 60 deg C.

ActivationFor BET, sample evacuated to 50 umHg at 5 mmHg s-1, heated to 80 deg C at 10 deg C min-1 and held 2 h.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Fe(OAc)2	13.138 mg, 0.075 mmol	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7
Linker	HHTP	36.72 mg, 0.113 mmol	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7
Solvent	water:DMF mixture	HHTP in 10 9.6 mL; Fe(OAc)2 in 10 mL · 1:1 v/v	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7
Base	sodium acetate aqueous solution	293 uL; 5 equivalents to HHTP · 1 M	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7
Other	N2	bubbled through each solution for 30 min	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7
Other	acetone	3 x 30 mL washes	SI p.S2 · Synthesis of Fe-HHTP · Figures S1-S7

Complete recipeSource: SI

SI p.S3 · Synthesis of Ni-HHTP · Figure S12

Metal precursorsNi(OAc)2.4H2O (30 mg, 0.12 mmol)

Linker precursorsHHTP (21 mg, 0.66 mmol as reported)

Solvents12 mL H2O

AtmosphereNot specified

Temperature85

Time12

Work-upCentrifuged and washed with water, methanol and acetone twice each; dried in vacuum oven for 1 h at 60 deg C before PXRD.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	30 mg, 0.12 mmol	SI p.S3 · Synthesis of Ni-HHTP · Figure S12
Linker	HHTP	21 mg, 0.66 mmol	SI p.S3 · Synthesis of Ni-HHTP · Figure S12
Solvent	H2O	12 mL	SI p.S3 · Synthesis of Ni-HHTP · Figure S12