Synthesis · Conductive metal–organic framework with redox metal center as cathode for high rate performance lithium ion battery

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

2 · 2.2. Synthesis and activation of Cu3(HHTP)2

Metal precursorsCobalt acetate substituted for copper acetate

Linker precursorsHHTP; amount not separately stated, apparently same procedure as Cu3(HHTP)2

Solventssame procedures and conditions as Cu3(HHTP)2 synthesis

Atmospherenot specified

Temperature85; 150 activation before cathode use

Time16; 4 activation before cathode use

Work-upSame procedures and conditions as Cu3(HHTP)2; exact cobalt precursor hydrate/amount not specified.

ActivationPowder heated to 150 degC for 4 h to remove guest DMF solvent molecules from pores before cathode use.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	cobalt acetate	Not specified	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Linker	HHTP	Not specified	2 · 2.2. Synthesis and activation of Cu3(HHTP)2

Complete recipeSource: Main

Route 2: Other

3 · 2.4. Fabrication of the electrodes and batteries

SolventsN-methyl pyrrolidone

AdditivesPVDF binder; no conductive carbon additives

Atmospherecoin cells assembled in argon-filled glovebox

Temperature60

Timeovernight

Substrate orientationaluminium foil current collector

Work-upMixed in N-methyl pyrrolidone, ball-milled into homogeneous slurry, coated on aluminium foil collectors.

ActivationComposite dried at 60 degC in vacuum oven overnight; coin cell assembled with Li chip anode, Celgard 2400 separator, 1.0 M LiPF6 in EC:DMC 1:1 v/v electrolyte.

Scalability contextStandard coin-cell electrode fabrication; no loading or film thickness reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2 crystalline powder	80 wt%	3 · 2.4. Fabrication of the electrodes and batteries
Additive	polyvinylidene fluoride (PVDF)	20 wt%	3 · 2.4. Fabrication of the electrodes and batteries
Solvent	N-methyl pyrrolidone	Not specified	3 · 2.4. Fabrication of the electrodes and batteries
Electrolyte	LiPF6 in EC:DMC	1.0 M; EC:DMC = 1:1 v/v · 1.0 M	3 · 2.4. Fabrication of the electrodes and batteries

Complete recipeSource: Main

Route 3: Solvothermal

2 · 2.2. Synthesis and activation of Cu3(HHTP)2

Metal precursorsCopper acetate monohydrate (8 mg, 0.04 mmol)

Linker precursorsHHTP (6.5 mg, 0.02 mmol)

Solvents0.8 mL Milli-Q water for copper acetate; 0.8 mL DMF for HHTP; deionized water and acetone for washing/solvent exchange

Atmospherenot specified for synthesis; capped vial during solvent exchange

Temperature85

Time16

Work-upNatural cooling to 25 degC; dark blue crystals washed with deionized water and acetone 6 times respectively; dried in vacuum oven at 60 degC for 8 h.

ActivationImmersed in deionized water in 4 mL capped vial at 85 degC for 4 h, repeated twice with final 16 h immersion; then acetone in capped vial at 65 degC for 8 h, repeated twice with final 16 h immersion; heated at 85 degC for 24 h to remove acetone.

Scalability contextSmall-batch beaker/vial synthesis; no scale-up data reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Copper acetate monohydrate	8 mg, 0.04 mmol	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Linker	HHTP	6.5 mg, 0.02 mmol	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Solvent	Milli-Q water	0.8 mL	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Solvent	dimethyl formamide (DMF)	0.8 mL	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Solvent	deionized water	Not specified	2 · 2.2. Synthesis and activation of Cu3(HHTP)2
Solvent	acetone	Not specified	2 · 2.2. Synthesis and activation of Cu3(HHTP)2