Synthesis · Efficient and Selective Uptake of TcO4- by a Cationic Metal-Organic Framework Material with Open Ag+ Sites

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

3 · Synthesis of SCU-100 and SCU-100-Re

Metal precursorsSCU-100 crystals; NaReO4

Linker precursorstipm already present in SCU-100

Solventsaqueous NaReO4 solution

Atmosphereambient; not otherwise specified

Temperatureroom temperature

Time12

Work-upcrystals filtered and washed with deionized water

Activationnone reported

Scalability context10 mg SCU-100 in 10 mL NaReO4 solution.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SCU-100 crystals	10 mg	3 · Synthesis of SCU-100 and SCU-100-Re
Other	NaReO4 solution	10 mL · 10 mM	3 · Synthesis of SCU-100 and SCU-100-Re

Complete recipeSource: Both

Route 2: Solvothermal

3 · Synthesis of SCU-100 and SCU-100-Re

Metal precursorsAgNO3 (0.017 g, 0.10 mmol)

Linker precursorstipm (0.029 g, 0.05 mmol)

SolventsCH3CN (0.5 mL) and deionised water (2 mL), v/v 1/4

Atmospheresealed autoclave; atmosphere not specified

Temperature90

Time96

Work-upcooled to room temperature at 1.25 C h-1; product washed with ethanol and dried in air at room temperature

Activationnone reported

Scalability context10 mL autoclave batch; no scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	AgNO3	0.017 g, 0.10 mmol	3 · Synthesis of SCU-100 and SCU-100-Re
Linker	tipm	0.029 g, 0.05 mmol	3 · Synthesis of SCU-100 and SCU-100-Re
Solvent	CH3CN	0.5 mL	3 · Synthesis of SCU-100 and SCU-100-Re
Solvent	deionized water	2 mL	3 · Synthesis of SCU-100 and SCU-100-Re

Complete recipeSource: SI

Route 3: Other

S3 · Synthesis of Tetrakis(4-bromophenyl)methane

Linker precursorstetraphenylmethane (2.25 g, 7.02 mmol)

Solventsethanol (200 mL) cooled to -78 C

Additivessaturated aqueous NaHSO3 wash

Atmospherenot specified

Temperature-78 workup; 50 drying

Time5

Oxidant / reductantbromine (4.0 mL, 77.8 mmol)

Work-uppoured into cold ethanol; precipitated solid filtered, washed with saturated aqueous NaHSO3 solution (80 mL x3), dried at 50 C under vacuum

Activationvacuum drying at 50 C

Scalability contextReported 4.45 g product, 99.6% yield.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Oxidant	Bromine	4.0 mL, 77.8 mmol	S3 · Synthesis of Tetrakis(4-bromophenyl)methane
Linker	tetraphenylmethane	2.25 g, 7.02 mmol	S3 · Synthesis of Tetrakis(4-bromophenyl)methane
Solvent	ethanol	200 mL	S3 · Synthesis of Tetrakis(4-bromophenyl)methane
Reductant	saturated aqueous NaHSO3 solution	80 mL x3 · saturated	S3 · Synthesis of Tetrakis(4-bromophenyl)methane

Complete recipeSource: SI

Route 4: Other

S3 · Synthesis of the ligand tipm

Metal precursorsCuI catalyst (0.08 g, 0.4 mmol)

Linker precursorstetrakis(4-bromophenyl)methane (0.64 g, 1 mmol); imidazole (0.70 g, 10 mmol)

Solventswater workup; MeOH recrystallisation

AdditivesK2CO3 (0.83 g, 6 mmol); EDTA (0.12 g, 0.4 mmol); NH3·H2O (25-28%, 0.5 mL)

Atmospherenot specified

Time0.025 h microwave irradiation plus 5 h stirring after workup

Work-upmixture poured into water; EDTA and NH3·H2O added; stirred 5 h; filtered, washed with water, recrystallised from MeOH, dried under vacuum

Activationvacuum drying

Scalability contextReported 0.32 g product, 50% yield.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	tetrakis(4-bromophenyl)methane	0.64 g, 1 mmol	S3 · Synthesis of the ligand tipm
Linker	imidazole	0.70 g, 10 mmol	S3 · Synthesis of the ligand tipm
Base	K2CO3	0.83 g, 6 mmol	S3 · Synthesis of the ligand tipm
Additive	CuI	0.08 g, 0.4 mmol	S3 · Synthesis of the ligand tipm
Additive	EDTA	0.12 g, 0.4 mmol	S3 · Synthesis of the ligand tipm
Base	NH3·H2O	0.5 mL · 25-28%	S3 · Synthesis of the ligand tipm