Synthesis · Millimeter-scale semiconductive metal-organic framework single crystal for X-ray imaging

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

main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure 5E; Figure S21

Work-upSix uniform 2 mm SCU-15 single crystals selected and fabricated into a 2 x 3 pixelated Ag-contacted array detector

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SCU-15 single crystals	six crystals, uniform size of 2 mm	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure 5E; Figure S21
Other	Ag detector electrodes	Not specified	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure 5E; Figure S21

Complete recipeSource: Main

Route 2: Other

main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S12

Work-upPure SCU-15 fine powder pelleted at 10 MPa in a 3 mm diameter mould, then contacted with Ag electrodes

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SCU-15 fine powder	Not specified	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S12
Other	Ag electrodes/contacts	Not specified	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S12

Complete recipeSource: Main

Route 3: Other

main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S10

Substrate orientation(011) crystal plane connected to the anode

Work-up3 mm SCU-15 single crystal contacted with Ag electrodes as Ag/SCU-15 single crystal/Ag detector

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ag electrodes/contacts	Not specified	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S10
Other	SCU-15 3 mm single crystal	one 3 mm single crystal	main p.9 · Fabrication of SCU-15-SC, SCU-15 PP, and SCU-15 array detector devices · Figure S10

Complete recipeSource: Main

Route 4: Solvothermal

main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3

Metal precursorsUO2(NO3)2.6H2O (25.1 mg, 0.05 mmol)

Linker precursors4-mercaptobenzoic acid (4-MBA; 23.1 mg, 0.15 mmol)

SolventsDeionized water (1.5 mL) and N,N-dimethylformamide (DMF; 0.5 mL)

AdditivesTrifluoroacetic acid (TFA; 50 uL)

AtmosphereNot specified for synthesis; dried in air after workup

Temperature120

Time12

Oxidant / reductantIn situ oxidation of 4-MBA thiol groups to disulfide bonds during solvothermal reaction; no separate oxidant specified

Work-upCooled naturally to room temperature; light-yellow crystals rinsed with DMF and MeOH and dried in air

ActivationNo activation reported

Scalability contextCrystal size tunable from about 50 um to 3 mm by controlling heating rate. Main text reports up to 3 mm at 9 deg C/min ([AB] = 10 min) and about 50 um at 0.125 deg C/min ([AB] = 8 h).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	UO2(NO3)2.6H2O	25.1 mg, 0.05 mmol	main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3
Linker	4-MBA (4-mercaptobenzoic acid)	23.1 mg, 0.15 mmol	main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3
Solvent	deionized water	1.5 mL	main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3
Solvent	N,N-dimethylformamide (DMF)	0.5 mL	main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3
Acid	trifluoroacetic acid (TFA)	50 uL	main p.8-p.9 · Synthesis of SCU-15 · Figure S1; Figure S3