cMOF Evidence Base

Synthesis evidence

Mechanistic Insight into the Formation and Deposition of Conductive, Layered Metal-Organic Framework Nanocrystals

Ambrogi E.K., Damacet P., Stolz R.M. et al. · ACS Nano · 2025 · 1383-1395

25 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

S41-S42 · In-situ growth experiments · Table S15; Table S16

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantair bubbled at 1 mL/min
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS41-S42 · In-situ growth experiments · Table S15; Table S16
Complete recipeSource: SI

Route 2: Other

S41-S42 · In-situ growth experiments · Table S15; Table S16

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantair bubbled at 2 mL/min
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS41-S42 · In-situ growth experiments · Table S15; Table S16
Complete recipeSource: SI

Route 3: Other

S41-S42 · In-situ growth experiments · Table S15; Table S16

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantair bubbled at 4 mL/min
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS41-S42 · In-situ growth experiments · Table S15; Table S16
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS41-S42 · In-situ growth experiments · Table S15; Table S16
Complete recipeSource: Main

Route 4: Other

p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereair bubbled through solution
Temperature22-25
Time14 h spectra; remaining mixture 18 h for powder
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantair/O2
Work-upremaining mixture collected by vacuum filtration; washed with water and ethanol
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Complete recipeSource: Main

Route 5: Other

p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmospherenitrogen removed; cell left open to air, port in
Temperature22-25
Time14 h spectra; remaining mixture 18 h for powder
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantpassive air/O2 diffusion through smaller aperture
Work-upremaining mixture collected by vacuum filtration; washed with water and ethanol
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Complete recipeSource: Main

Route 6: Other

p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmospherenitrogen removed; cell left open to air, port out
Temperature22-25
Time14 h spectra; remaining mixture 18 h for powder
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantpassive air/O2 diffusion
Work-upremaining mixture collected by vacuum filtration; washed with water and ethanol
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Complete recipeSource: Main

Route 7: Other

p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmospherecell open to air
Temperature22-25
Time14 h spectra; remaining mixture 18 h for powder
Substrate orientationdiamond ATR crystal surface
Oxidant / reductant50 uL 6% H2O2
Work-upremaining mixture collected by vacuum filtration; washed with water and ethanol
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
OxidantH2O250 uL · 6%p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Complete recipeSource: SI

Route 8: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 10eq
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 9: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 10eq delayed
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 10: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 10eq gradual 2h
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 11: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 10eq gradual 4h
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 12: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 1eq
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 13: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 3eq
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 14: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 3eq delayed
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 15: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 5eq
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: SI

Route 16: Other

S36-S39 · In-situ growth experiments · Table S11-S14

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
Atmosphereroom-temperature ATR cell
Temperature22-25
Time14 h spectra; sample isolated after overnight/18 h where stated
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantH2O2 7 5eq
Work-upMOF samples from companion reaction collected for PXRD and SEM
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellS36-S39 · In-situ growth experiments · Table S11-S14
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volS36-S39 · In-situ growth experiments · Table S11-S14
Complete recipeSource: Main

Route 17: Other

p010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solvents20:3 degassed water/DMF
AtmosphereN2 gas flowing slowly over solution
Temperature22-25
Time14 h spectra; remaining mixture 18 h for powder
Substrate orientationdiamond ATR crystal surface
Oxidant / reductantnone
Work-upremaining mixture collected by vacuum filtration; washed with water and ethanol
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP solution500 uL of 11.1 mM solution · 7.4 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Metal SourceNi(OAc)2.4H2O solution250 uL of solution from 55.3 mg in 5 mL · 14.8 mM final in cellp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Solventdegassed water/DMF750 uL in reaction cell · 20:3 vol/volp010 / journal page 1392 · In Situ Monitoring by ATR-FTIR · Figure 2; Table S8
Complete recipeSource: Both

Route 18: Solvothermal

S12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3

Metal precursorsNi(OAc)2(H2O)4
Linker precursorsHHTP
Solvents20:3 DI H2O/DMF
Atmosphereair bubbled through solution
Temperature85
Time18
Oxidant / reductant1 mL 6% H2O2 added after HHTP and Ni(OAc)2
Work-upcollected via centrifuging in SI TEM/SEM captions; washed/dried as bulk product
Activationstored under vacuum
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
OxidantH2O21 mL · 6%S12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Complete recipeSource: SI

Route 19: Hydrothermal

S7 · Figure S6 caption · Figure S6

Metal precursorsNi(OAc)2
Linker precursorsHHTP
Solventswater
Atmosphereair bubbled through vial
Temperature85
Time18
Oxidant / reductantdissolved oxygen/air
Work-upvacuum filtration
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP-tc / HHTP0.111 mmolS7 · Figure S6 caption · Figure S6
Metal SourceNi(OAc)20.222 mmolS7 · Figure S6 caption · Figure S6
SolventwaterNot specifiedS7 · Figure S6 caption · Figure S6
Complete recipeSource: SI

Route 20: Solvothermal

S21-S22 · Impact of Temperature · Figure S28; Table S7

Metal precursorsNi(OAc)2
Linker precursorsHHTP
Solvents3:20 DMF:H2O
Atmosphereair bubbled
Temperature22
Time18
Oxidant / reductantdissolved oxygen/air
Work-upvacuum filtration
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolS21-S22 · Impact of Temperature · Figure S28; Table S7
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolS21-S22 · Impact of Temperature · Figure S28; Table S7
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volS21-S22 · Impact of Temperature · Figure S28; Table S7
Complete recipeSource: SI

Route 21: Solvothermal

S21-S22 · Impact of Temperature · Figure S28; Table S7

Metal precursorsNi(OAc)2
Linker precursorsHHTP
Solvents3:20 DMF:H2O
Atmosphereair bubbled
Temperature40
Time18
Oxidant / reductantdissolved oxygen/air
Work-upvacuum filtration
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolS21-S22 · Impact of Temperature · Figure S28; Table S7
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolS21-S22 · Impact of Temperature · Figure S28; Table S7
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volS21-S22 · Impact of Temperature · Figure S28; Table S7
Complete recipeSource: Both

Route 22: Solvothermal

p010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3

Metal precursorsNi(OAc)2(H2O)4
Linker precursorsHHTP
Solvents20:3 DI H2O/DMF
Atmosphereair bubbled through solution
Temperature85
Time18
Oxidant / reductantdissolved oxygen/air
Work-upvacuum filtration; rinsed 5 times each with 10 mL water then 10 mL acetone; dried and stored under vacuum
Activationstored under vacuum
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Complete recipeSource: Both

Route 23: Solvothermal

S12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3

Metal precursorsNi(OAc)2(H2O)4
Linker precursorsHHTP
Solvents20:3 DI H2O/DMF
AtmosphereN2 bubbled through solution
Temperature85
Time18
Oxidant / reductant1 mL 6% H2O2 added after HHTP and Ni(OAc)2
Work-upcollected via centrifuging in SI TEM/SEM captions; washed/dried as bulk product
Activationstored under vacuum
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volS12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
OxidantH2O21 mL · 6%S12-S14 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Complete recipeSource: Both

Route 24: Solvothermal

p010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3

Metal precursorsNi(OAc)2(H2O)4
Linker precursorsHHTP
Solvents20:3 DI H2O/DMF
AtmosphereN2 bubbled through solution
Temperature85
Time18
Oxidant / reductantnominally no added oxidant; degassed solvent
Work-upvacuum filtration; rinsed with water and acetone; dried/stored under vacuum
Activationstored under vacuum
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP36 mg · 0.111 mmolp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Metal SourceNi(OAc)2(H2O)4 / Ni(OAc)2.4H2O55 mg or 55.3 mg · 0.222 mmolp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
SolventDI H2O/DMF10 mL plus metal solution volume as prepared · 20:3 vol/volp010 / journal page 1392 · Bulk Synthesis of Ni3(HHTP)2 · Figure 1; Table S3
Complete recipeSource: SI

Route 25: Other

S3-S4 · Synthesis of reduced HHTP

Linker precursorsHMTP precursor
Solventsdichloromethane; brine; degassed water; ethyl acetate; dilute HCl wash
Additivesboron tribromide
Atmospherenitrogen, vacuum storage
Temperatureroom temperature
Timeovernight
Oxidant / reductantBBr3 reductive/dealkylation reagent; HHTP protected from oxygen
Work-upvacuum filtration under nitrogen pillow; washed with degassed water and dilute HCl; dried high vacuum
Activationstored under vacuum
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerhexamethoxytriphenylene (HMTP)2.0 g · 4.9 mmolS3-S4 · Synthesis of reduced HHTP
Reductantboron tribromide3.25 mL · 34.3 mmol, 7 equivalentsS3-S4 · Synthesis of reduced HHTP
Solventdichloromethane100 mLS3-S4 · Synthesis of reduced HHTP