cMOF Evidence Base

Synthesis evidence

Functionality in metal-organic framework minerals: Proton conductivity, stability and potential for polymorphism

Huskic I., Novendra N., Lim D.-W. et al. · Chemical Science · 2019 · 4923-4929

8 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

4925 · Deuterated ST1 and ZH · SI Fig. S12-S13

Metal precursorsNaMgFe(C2O4)3.9H2O (ST1)
Linker precursorsOxalate already present in ST1
SolventsD2O
Atmospheredry N2
Temperature70
Work-upFully dehydrated parent phase under vacuum at 70 deg C, dissolved in D2O and recrystallized under dry N2.
ActivationFull dehydration under vacuum at 70 deg C before D2O recrystallisation.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNaMgFe(C2O4)3.9H2O (ST1)Not specified4925 · Deuterated ST1 and ZH · SI Fig. S12-S13
SolventD2ONot specified4925 · Deuterated ST1 and ZH · SI Fig. S12-S13
Partial recipeSource: Both

Route 2: Other

4925 · Deuterated ST1 and ZH · SI Fig. S12-S13

Metal precursorsNaMgAl(C2O4)3.9H2O/ZH parent phase as written in main text
Linker precursorsOxalate already present in parent
SolventsD2O
Atmospheredry N2
Temperature70
Work-upFully dehydrated parent phase under vacuum at 70 deg C, dissolved in D2O and recrystallized under dry N2.
ActivationFull dehydration under vacuum at 70 deg C before D2O recrystallisation.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNaMgAl(C2O4)3.9H2ONot specified4925 · Deuterated ST1 and ZH · SI Fig. S12-S13
SolventD2ONot specified4925 · Deuterated ST1 and ZH · SI Fig. S12-S13
Partial recipeSource: Main

Route 3: Other

4924 · Synthesis of ST1 and ST2

Metal precursorsFeO(OH) generated from FeCl3.6H2O and NaHCO3; MgCl2.6H2O; NaOH
Linker precursorsOxalic acid
SolventsWater
AdditivesNaHCO3; NaOH
Atmosphereambient/not specified
Temperature4
Work-upFiltered solution was refrigerated at 4 deg C for crystallisation and slow evaporation; ST1/ST2 crystals separated by hand based on morphology.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3.6H2ONot specified4924 · Synthesis of ST1 and ST2
BaseNaHCO3Not specified4924 · Synthesis of ST1 and ST2
Linkeroxalic acidNot specified4924 · Synthesis of ST1 and ST2
BaseNaOHNot specified4924 · Synthesis of ST1 and ST2
Metal SourceMgCl2.6H2ONot specified4924 · Synthesis of ST1 and ST2
Partial recipeSource: Main

Route 4: Other

4924 · Dehydration of ST1 and ST2 single crystals

Metal precursorsST1 single crystals
Linker precursorsOxalate already present in ST1
Atmospherevacuum
Temperature50
Time12
Work-upGentle heating under vacuum.
ActivationDehydration itself; no separate activation reported.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherST1 single crystalsNot specified4924 · Dehydration of ST1 and ST2 single crystals
Partial recipeSource: Main

Route 5: Other

4924 · Synthesis of ST1 and ST2

Metal precursorsFeO(OH) generated from FeCl3.6H2O and NaHCO3; MgCl2.6H2O; NaOH
Linker precursorsOxalic acid
SolventsWater
AdditivesNaHCO3; NaOH
Atmosphereambient/not specified
Temperature4
Work-upFiltered solution was refrigerated at 4 deg C; faster evaporation, including rotary evaporation, gave ST2 as the major product.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3.6H2ONot specified4924 · Synthesis of ST1 and ST2
BaseNaHCO3Not specified4924 · Synthesis of ST1 and ST2
Linkeroxalic acidNot specified4924 · Synthesis of ST1 and ST2
BaseNaOHNot specified4924 · Synthesis of ST1 and ST2
Metal SourceMgCl2.6H2ONot specified4924 · Synthesis of ST1 and ST2
Partial recipeSource: Main

Route 6: Other

4924 · Dehydration of ST1 and ST2 single crystals

Metal precursorsST2 single crystals
Linker precursorsOxalate already present in ST2
Atmospherevacuum
Temperature50
Time12
Work-upGentle heating under vacuum.
ActivationDehydration itself; no separate activation reported.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherST2 single crystalsNot specified4924 · Dehydration of ST1 and ST2 single crystals
Partial recipeSource: Main

Route 7: Other

4924 · Synthesis of ZH

Metal precursorsNaMgAl(C2O4)3.9H2O and NaMgFe(C2O4)3.9H2O
Linker precursorsOxalate already present in precursors
SolventsWater
Atmosphereambient/not specified
Time0.5
Work-upMilled in 10 mL Teflon jars with one 10 mm zirconia ball at 25 Hz.
Scalability contextBulk sample generated by mechanochemical liquid-assisted milling.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNaMgAl(C2O4)3.9H2Oequimolar amount4924 · Synthesis of ZH
OtherNaMgFe(C2O4)3.9H2Oequimolar amount4924 · Synthesis of ZH
SolventH2O40 mL as extracted text; rendered page shows 40 uL4924 · Synthesis of ZH
Partial recipeSource: Main

Route 8: Other

4924 · Synthesis of ZH

Metal precursorsAluminium metal; MgCl2.6H2O; NaMgFe(C2O4)3.9H2O; NaMgAl(C2O4)3.9H2O
Linker precursorsOxalic acid
SolventsWater
AdditivesNaOH
Atmosphereambient/not specified
Temperature4
Timeseveral days
Work-upNaMgAl(C2O4)3.9H2O prepared by dissolution/sonication, NaOH and MgCl2.6H2O addition, filtration and evaporation. Equivalent Al and Fe oxalates were dissolved in a small amount of water; yellow-green ZH needles isolated after several days at 4 deg C.
Scalability contextBulk ZH was additionally prepared by liquid-assisted milling.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcealuminum metalNot specified4924 · Synthesis of ZH
Linkeroxalic acidNot specified4924 · Synthesis of ZH
BaseNaOHNot specified4924 · Synthesis of ZH
Metal SourceMgCl2.6H2ONot specified4924 · Synthesis of ZH
OtherNaMgFe(C2O4)3.9H2Oequivalent amount4924 · Synthesis of ZH
OtherNaMgAl(C2O4)3.9H2Oequivalent amount4924 · Synthesis of ZH