cMOF Evidence Base

Synthesis evidence

Cooperative Proton and Li-ion Conduction in a 2D-Layered MOF via Mechanical Insertion of Lithium Halides

Sarango-Ramirez M.K., Donoshita M., Yoshida Y. et al. · Angewandte Chemie - International Edition · 2023 · e202301284

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

S1 · Sample preparation

Metal precursorsTi(OiPr)4 (600 uL, 2 mmol)
Linker precursorsH4dobdc (1.5852 g, 8 mmol)
Solvents16 mL 2-propanol for Ti precursor; 16 mL acetonitrile for H4dobdc suspension; ethanol wash
Atmospheresealed 100 mL autoclave; dynamic vacuum during drying
Temperature119.85 (393 K)
Time24 h oven heating after 1 h stirring
Work-upcollected by filtration; washed with acetonitrile/2-propanol 1:1 v/v until no UV fluorescence; washed with ethanol for two days
Activationdried under dynamic vacuum at 373 K for 4 h
Scalability contextSI calls the synthesis a scaled-up previously reported procedure.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTi(OiPr)4600 uL, 2 mmolS1 · Sample preparation
LinkerH4dobdc1.5852 g, 8 mmolS1 · Sample preparation
Solvent2-propanol16 mLS1 · Sample preparation
Solventacetonitrile16 mLS1 · Sample preparation
Solventethanolwash for two daysS1 · Sample preparation
Complete recipeSource: Both

Route 2: Other

S1-S2 · Sample preparation

Metal precursorspre-synthesised Ti-dobdc
Linker precursorspre-synthesised Ti-dobdc framework
AdditivesLiBr 0.0388 g
Atmospherehumidity control chamber at 95% RH
Time24 h at RH 95% after mixing/grinding
Work-upmechanically mixed and ground
Activationnot specified for synthesis; all samples activated at 373 K under vacuum (10^-2 Pa) for 4 h before H2O sorption
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi-dobdc0.3006 gS1-S2 · Sample preparation
AdditiveLiBr0.0388 g · MOF:LiBr = 1:1S1-S2 · Sample preparation
Partial recipeSource: Main

Route 3: Other

2 · Results · Figure S1

Metal precursorspre-synthesised Ti-dobdc
Linker precursorspre-synthesised Ti-dobdc framework
AdditivesLiBr, MOF:LiBr molar ratio 1:3
Atmospherehumidity control chamber at 95% RH
Time24 h at RH 95% after mechanical mixing (main-text general condition)
Work-upmechanically mixed; specific mass not reported for this ratio
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi-dobdcNot specified2 · Results · Figure S1
AdditiveLiBrMOF:LiBr = 1:32 · Results · Figure S1
Partial recipeSource: Main

Route 4: Other

2 · Results · Figure S1

Metal precursorspre-synthesised Ti-dobdc
Linker precursorspre-synthesised Ti-dobdc framework
AdditivesLiBr, MOF:LiBr molar ratio 1:5
Atmospherehumidity control chamber at 95% RH
Time24 h at RH 95% after mechanical mixing (main-text general condition)
Work-upmechanically mixed; specific mass not reported for this ratio
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi-dobdcNot specified2 · Results · Figure S1
AdditiveLiBrMOF:LiBr = 1:52 · Results · Figure S1
Complete recipeSource: Both

Route 5: Other

S1 · Sample preparation

Metal precursorspre-synthesised Ti-dobdc
Linker precursorspre-synthesised Ti-dobdc framework
AdditivesLiCl 0.0185 g
Atmospherehumidity control chamber at 95% RH
Time24 h at RH 95% after mixing/grinding
Work-upmechanically mixed and ground
Activationnot specified for synthesis; all samples activated at 373 K under vacuum (10^-2 Pa) for 4 h before H2O sorption
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi-dobdc0.3001 gS1 · Sample preparation
AdditiveLiCl0.0185 g · MOF:LiCl = 1:1S1 · Sample preparation
Complete recipeSource: Both

Route 6: Other

S2 · Sample preparation

Metal precursorspre-synthesised Ti-dobdc
Linker precursorspre-synthesised Ti-dobdc framework
AdditivesLiI 0.0598 g
Atmospherehumidity control chamber at 95% RH
Time24 h at RH 95% after mixing/grinding
Work-upmechanically mixed and ground
Activationnot specified for synthesis; all samples activated at 373 K under vacuum (10^-2 Pa) for 4 h before H2O sorption
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTi-dobdc0.3008 gS2 · Sample preparation
AdditiveLiI0.0598 g · MOF:LiI = 1:1S2 · Sample preparation