Synthesis evidence

Metal-halide porous framework superlattices

Zhang W., Jiang H., Liu Y. et al. · Nature · 2025 · 418-424

25 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

424 · Methods: Synthesis of CdI2@MOF superlattice

Metal precursorsCdI2 10-15 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:2 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time240-360
Work-upwashed with DMF ten times to remove isolated CdI2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 2: Other

424 · Methods: Synthesis of CdI2@MOF superlattice

Metal precursorsCdI2 10-15 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:2 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time240-360
Work-upwashed with DMF ten times to remove isolated CdI2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 3: Other

424 · Methods: Synthesis of NiBr2@MOF superlattices

Metal precursorsNiBr2 10 mg
Linker precursorsactivated MOF crystal template
Solventsdiglyme 3 ml
Atmospheredegassed by 3 freeze-pump-thaw cycles; flame-sealed
Temperature120
Time720
Work-upwashed with DMF ten times to remove isolated NiBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 4: Other

424 · Methods: Synthesis of NiBr2@MOF superlattices

Metal precursorsNiBr2 10 mg
Linker precursorsactivated MOF crystal template
Solventsdiglyme 3 ml
Atmospheredegassed by 3 freeze-pump-thaw cycles; flame-sealed
Temperature120
Time720
Work-upwashed with DMF ten times to remove isolated NiBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: SI

Route 5: Solvothermal

S7-S8 · Synthesis of NU-1000

Metal precursorsZrOCl2.8H2O 388 mg, 1.20 mmol
Linker precursorsH4TBAPy 160 mg, 0.24 mmol
SolventsDEF 32 mL
Additivesbenzoic acid 10.8 g, trifluoroacetic acid modulator
Atmospheresealed bottle/air not specified
Temperature100
Time1 h pre-incubation plus 48 h after linker addition
Work-upsolvent-exchanged to absolute ethanol three times over three days
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrOCl2.8H2O388 mg, 1.20 mmolS7-S8 · Synthesis of NU-1000
LinkerH4TBAPy160 mg, 0.24 mmolS7-S8 · Synthesis of NU-1000
SolventN,N-diethylformamide (DEF)32 mLS7-S8 · Synthesis of NU-1000
Additivebenzoic acid10.8 g, 88.43 mmolS7-S8 · Synthesis of NU-1000
Additivetrifluoroacetic acidsmall amountS7-S8 · Synthesis of NU-1000
Complete recipeSource: SI

Route 6: Solvothermal

S8 · Synthesis of NU-600

Metal precursorsZrCl4 10 mg
Linker precursorsH4TCPB-Br2 8 mg
SolventsDEF 2 mL
Additivesacetic acid 0.8 mL
Atmospheresealed vial
Temperature120
Time24
Work-upwashed with DMF and acetone; dried in air
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 7: Other

424 · Methods: Synthesis of PbBr2@MOF superlattices

Metal precursorsPbBr2 15-25 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 8: Other

424 · Methods: Synthesis of PbBr2@MOF superlattices

Metal precursorsPbBr2 15-25 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 9: Other

424 · Methods: Synthesis of PbBr2@MOF superlattices

Metal precursorsPbBr2 15-25 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 10: Other

424 · Methods: Synthesis of PbBr2@MOF superlattices

Metal precursorsPbBr2 15-25 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 1:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbBr2 residue
Activationactivated MOF crystals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Both

Route 11: Other

424 · Methods: Synthesis of PbI2@MOF superlattices

Metal precursorsPbI2 10-20 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 2:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbI2 residue
ActivationMOF crystals washed with DMF and methanol, soaked 6 h between cleaning intervals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI210-20 mM424 · Methods: Synthesis of PbI2@MOF superlattices
SolventDMF/methanol4 mL · 2:1 v/v424 · Methods: Synthesis of PbI2@MOF superlattices
Otheractivated MOF crystals5 mg424 · Methods: Synthesis of PbI2@MOF superlattices
Complete recipeSource: Both

Route 12: Other

424 · Methods: Synthesis of PbI2@MOF superlattices

Metal precursorsPbI2 10-20 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 2:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbI2 residue
ActivationMOF crystals washed with DMF and methanol, soaked 6 h between cleaning intervals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI210-20 mM424 · Methods: Synthesis of PbI2@MOF superlattices
SolventDMF/methanol4 mL · 2:1 v/v424 · Methods: Synthesis of PbI2@MOF superlattices
Otheractivated MOF crystals5 mg424 · Methods: Synthesis of PbI2@MOF superlattices
Complete recipeSource: Both

Route 13: Other

424 · Methods: Synthesis of PbI2@MOF superlattices

Metal precursorsPbI2 10-20 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 2:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbI2 residue
ActivationMOF crystals washed with DMF and methanol, soaked 6 h between cleaning intervals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI210-20 mM424 · Methods: Synthesis of PbI2@MOF superlattices
SolventDMF/methanol4 mL · 2:1 v/v424 · Methods: Synthesis of PbI2@MOF superlattices
Otheractivated MOF crystals5 mg424 · Methods: Synthesis of PbI2@MOF superlattices
Complete recipeSource: Both

Route 14: Other

424 · Methods: Synthesis of PbI2@MOF superlattices

Metal precursorsPbI2 10-20 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 2:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbI2 residue
ActivationMOF crystals washed with DMF and methanol, soaked 6 h between cleaning intervals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI210-20 mM424 · Methods: Synthesis of PbI2@MOF superlattices
SolventDMF/methanol4 mL · 2:1 v/v424 · Methods: Synthesis of PbI2@MOF superlattices
Otheractivated MOF crystals5 mg424 · Methods: Synthesis of PbI2@MOF superlattices
Complete recipeSource: Both

Route 15: Other

424 · Methods: Synthesis of PbI2@MOF superlattices

Metal precursorsPbI2 10-20 mM solution
Linker precursorsactivated MOF crystal template
SolventsDMF/methanol 2:1 v/v, 4 mL
Atmospherestable undisturbed vial
Temperature25 (not explicitly stated; room temperature implied)
Time600-720
Work-upwashed with DMF ten times to remove isolated PbI2 residue
ActivationMOF crystals washed with DMF and methanol, soaked 6 h between cleaning intervals
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI210-20 mM424 · Methods: Synthesis of PbI2@MOF superlattices
SolventDMF/methanol4 mL · 2:1 v/v424 · Methods: Synthesis of PbI2@MOF superlattices
Otheractivated MOF crystals5 mg424 · Methods: Synthesis of PbI2@MOF superlattices
Complete recipeSource: SI

Route 16: Solvothermal

S8 · Synthesis of PCN-606

Metal precursorsZrCl4 20 mg
Linker precursorsH4TPCB 10 mg
SolventsDMF 3 mL
Additivesbenzoic acid 500 mg
Atmospheresealed vial
Temperature120
Time48
Work-upwashed with DMF and acetone; dried in air
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: SI

Route 17: Solvothermal

S8 · Synthesis of PCN-609

Metal precursorsZrCl4 20 mg
Linker precursorsH4CBTB 10 mg
SolventsDMF 3 mL
Additivesbenzoic acid 430 mg
Atmospheresealed vial
Temperature120
Time48
Work-upwashed with DMF and acetone; dried in air
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: SI

Route 18: Solvothermal

S8 · Synthesis of PCN-700

Metal precursorsZrCl4 9 mg
Linker precursorsH2Me2-BPDC 9 mg
SolventsDMF 1.5 mL
Additivestrifluoroacetic acid 0.08 mL
Atmospheresealed vial
Temperature120
Time24
Work-upwashed with DMF and acetone; dried in air
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl49 mgS8 · Synthesis of PCN-700
LinkerH2Me2-BPDC9 mgS8 · Synthesis of PCN-700
SolventDMF1.5 mLS8 · Synthesis of PCN-700
Additivetrifluoroacetic acid0.08 mLS8 · Synthesis of PCN-700
Complete recipeSource: Main

Route 19: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS- or R-alpha-methylbenzylamine 1 mL
Linker precursorsPbI2@MOF crystals 50 mg
SolventsDMF 1 mL
Additivesamine guest
Atmosphereambient/air not specified
Temperature25
Timevarious durations; MBA reaches PL maximum near 8 days in Fig. 4b
Work-upcentrifuge 8000 rpm 5 min; redisperse/centrifuge in DMF three times; wash ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: SI

Route 20: Other

S8 · Synthesis of rodlike PbI2 crystal

Metal precursorsPbI2 powder 20 mg
SolventsDMF 1 mL; methanol 0.5 mL
Atmosphereambient/air not specified
Time0.333
Work-upPbI2 solution added dropwise into methanol for 20 min; crystals characterized by SC-XRD
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 21: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS- or R-alpha-methylbenzylamine 1 mL
Linker precursorsPbI2@MOF crystals 50 mg
SolventsDMF 1 mL
Additivesamine guest
Atmosphereambient/air not specified
Temperature25
Timevarious durations; MBA reaches PL maximum near 8 days in Fig. 4b
Work-upcentrifuge 8000 rpm 5 min; redisperse/centrifuge in DMF three times; wash ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 22: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS- or R-alpha-methylbenzylamine 1 mL
Linker precursorsPbI2@MOF crystals 50 mg
SolventsDMF 1 mL
Additivesamine guest
Atmosphereambient/air not specified
Temperature25
Timevarious durations; MBA reaches PL maximum near 8 days in Fig. 4b
Work-upcentrifuge 8000 rpm 5 min; redisperse/centrifuge in DMF three times; wash ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 23: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS- or R-alpha-methylbenzylamine 1 mL
Linker precursorsPbI2@MOF crystals 50 mg
SolventsDMF 1 mL
Additivesamine guest
Atmosphereambient/air not specified
Temperature25
Timevarious durations; MBA reaches PL maximum near 8 days in Fig. 4b
Work-upcentrifuge 8000 rpm 5 min; redisperse/centrifuge in DMF three times; wash ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 24: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS- or R-alpha-methylbenzylamine 1 mL
Linker precursorsPbI2@MOF crystals 50 mg
SolventsDMF 1 mL
Additivesamine guest
Atmosphereambient/air not specified
Temperature25
Timevarious durations; MBA reaches PL maximum near 8 days in Fig. 4b
Work-upcentrifuge 8000 rpm 5 min; redisperse/centrifuge in DMF three times; wash ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes
Complete recipeSource: Main

Route 25: Other

424 · Methods: Synthesis of amine-modified PbI2@MOF superlattices

Metal precursorsS-NEA 1 mL
Linker precursorsPbI2@PCN-606 crystals 50 mg
SolventsDMF 1 mL
Additiveschiral amine guest
Atmosphereambient/air not specified
Temperature25
Time240
Work-upcentrifuge 8000 rpm 5 min; wash DMF three times and ethanol three times
Scalability contextbulk single crystals, milligram-scale in vials/tubes