Synthesis · Promoting electromagnetic wave absorption for conductive metal-organic frameworks through crystal morphology controlling

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

main p.2 / journal p.11526 · Synthesis of Ni-TABQ-1

Metal precursorsNi(OAc)2.4H2O (0.132 g, 0.530 mmol)

Linker precursorsTABQ (0.060 g, 0.357 mmol)

SolventsH2O (1.5 mL) and aqueous NH3.H2O (7.2 mL)

AdditivesNH3.H2O base

AtmosphereSealed pressure tube; gas atmosphere not specified

Temperature120

Time48

Oxidant / reductantNo separate oxidant/reductant specified for MOF assembly; authors propose water-mediated oxidation-reduction during heating.

Work-upCool to room temperature; filter; wash with a large amount of H2O and MeOH; dry at room temperature for at least 24 h.

ActivationRoom-temperature drying for at least 24 h

Scalability contextPressure-tube batch; yield not reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	TABQ	0.060 g, 0.357 mmol	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-1
Metal Source	Ni(OAc)2.4H2O	0.132 g, 0.530 mmol	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-1
Solvent	H2O	1.5 mL	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-1
Base	NH3.H2O	7.2 mL · 25% aqueous ammonia listed in materials	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-1

Partial recipeSource: Main

Route 2: Other

main p.2 / journal p.11526 · Synthesis of Ni-TABQ-2

Metal precursorsNi(NO3)2.6H2O (0.097 g, 0.033 mmol)

Linker precursorsTABQ (0.056 g, 0.033 mmol)

SolventsDMSO (10.0 mL for solution A and 10.0 mL for solution B)

AdditivesNH3.H2O (1.0 mL)

AtmosphereNot specified

Time3

Oxidant / reductantNo separate oxidant/reductant specified for MOF assembly

Work-upFilter under decreased pressure; wash with H2O, acetone, and EtOH until filtrate colourless; dry in vacuum at 60 C.

ActivationVacuum drying at 60 C

Scalability contextSmall solution-stirring batch; yield not reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.097 g, 0.033 mmol	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-2
Base	NH3.H2O	1.0 mL · 25% aqueous ammonia listed in materials	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-2
Solvent	DMSO	10.0 mL in solution A; 10.0 mL in solution B · 99% listed in materials	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-2
Linker	TABQ	0.056 g, 0.033 mmol	main p.2 / journal p.11526 · Synthesis of Ni-TABQ-2

Complete recipeSource: SI

Route 3: Other

SI pp.1-2 · 1. Synthesis of TABQ

Linker precursorsTetrachloro-1,4-benzoquinone (20 mmol, 4.92 g); phthalimide potassium salt (82.30 mmol, 15.24 g)

Solventsacetonitrile (80 mL); DMF (100 mL); ethanol; hydrazine (75 mL)

Additiveshydrazine in second step

AtmosphereN2 for first reflux step; second step atmosphere not specified

Temperature80; 100; 65

Time12; 0.5; 2

Oxidant / reductanthydrazine (N2H4, reductive deprotection/amination step)

Work-upCool; filter and collect slurry; wash with acetonitrile; suspend in DMF at 100 C for 30 min and hot filter; wash with DMF; suspend in ethanol, boil, hot filter, dry; then hydrazine treat, filter under reduced pressure, wash with deionised water and ethanol until colourless filtrate.

ActivationDried overnight under vacuum at 60 C

Scalability contextTABQ precursor route reports masses, molar amounts, solvents, atmosphere for first step, temperatures, times, workup, drying, and yield 50.60%.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	Tetrachloro-1,4-benzoquinone	20 mmol, 4.92 g	SI pp.1-2 · 1. Synthesis of TABQ
Other	Phthalimide potassium salt	82.30 mmol, 15.24 g	SI pp.1-2 · 1. Synthesis of TABQ
Solvent	acetonitrile	80 mL	SI pp.1-2 · 1. Synthesis of TABQ
Solvent	DMF	100 mL	SI pp.1-2 · 1. Synthesis of TABQ
Reductant	hydrazine	75 mL · 50% hydrazine listed in main materials	SI pp.1-2 · 1. Synthesis of TABQ
Solvent	ethanol	not specified · 99% listed in main materials	SI pp.1-2 · 1. Synthesis of TABQ