cMOF Evidence Base

Synthesis evidence

MOF matrix isolation: Cooperative conformational mobility enables reliable single crystal transformations

Peralta R.A., Huxley M.T., Young R.J. et al. · Faraday Discussions · 2021 · 84-99

14 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1 crystals
Linker precursorspre-formed MnMOF-1
SolventsDMF wash; acetone exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upDMF replaced by exchange solvent five times; 10 min soak between exchanges
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventacetone5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventDMF5 x 3 mL washp012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 2: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1 crystals
Linker precursorspre-formed MnMOF-1
SolventsDMF wash; MeCN exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upDMF replaced by exchange solvent five times; 10 min soak between exchanges
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventMeCN5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventDMF5 x 3 mL washp012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 3: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1 crystals
Linker precursorspre-formed MnMOF-1
SolventsDMF wash; EtOH exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upDMF replaced by exchange solvent five times; 10 min soak between exchanges
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventEtOH5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventDMF5 x 3 mL washp012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 4: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1 crystals
Linker precursorspre-formed MnMOF-1
SolventsDMF wash; MeOH exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upDMF replaced by exchange solvent five times; 10 min soak between exchanges
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventMeOH5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventDMF5 x 3 mL washp012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 5: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1-ace crystals
Linker precursorspre-formed MnMOF-1
Solventsacetone intermediate; dichloromethane exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upacetone-solvated crystals washed with fresh dichloromethane at 10 min intervals, five times
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1-ace single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventdichloromethane5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventacetoneintermediate solvatep012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 6: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1-ace crystals
Linker precursorspre-formed MnMOF-1
Solventsacetone intermediate; diethyl ether exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upacetone-solvated crystals washed with fresh diethyl ether at 10 min intervals, five times
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1-ace single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventdiethyl ether5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventacetoneintermediate solvatep012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 7: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1-ace crystals
Linker precursorspre-formed MnMOF-1
Solventsacetone intermediate; p-xylene exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upacetone-solvated crystals washed with fresh p-xylene at 10 min intervals, five times
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1-ace single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventp-xylene5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventacetoneintermediate solvatep012 / journal page 95 · Solvent exchange of MnMOF-1
Complete recipeSource: Both

Route 8: Other

p012 / journal page 95 · Solvent exchange of MnMOF-1

Metal precursorsMnMOF-1-ace crystals
Linker precursorspre-formed MnMOF-1
Solventsacetone intermediate; THF exchange solvent
Atmospheresolvents dried and degassed with Ar prior to use
Temperatureroom temperature
Time0.833
Work-upacetone-solvated crystals washed with fresh THF at 10 min intervals, five times
Activationsolvent-exchanged crystals retained in mother liquor
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1-ace single crystalsNot specifiedp012 / journal page 95 · Solvent exchange of MnMOF-1
SolventTHF5 x 3 mLp012 / journal page 95 · Solvent exchange of MnMOF-1
Solventacetoneintermediate solvatep012 / journal page 95 · Solvent exchange of MnMOF-1
Partial recipeSource: Both

Route 9: Other

p012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2

Metal precursors[Rh(CO)2Cl]2; pre-formed MnMOF-1 solvatomorph
Linker precursorspre-formed MnMOF-1
Solventsacetone
AtmosphereAr
Temperatureroom temperature
Timeovernight
Oxidant / reductant[Rh(CO)2Cl]2
Work-upyellow solution replaced with fresh acetone (5 x 3 mL) under Ar
Activationnone reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 crystals30 mgp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Other[Rh(CO)2Cl]2excessp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Solventacetone3 mL; fresh wash 5 x 3 mLp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Partial recipeSource: Both

Route 10: Other

p012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2

Metal precursors[Rh(CO)2Cl]2; pre-formed MnMOF-1 solvatomorph
Linker precursorspre-formed MnMOF-1
Solventsdichloromethane
AtmosphereAr
Temperatureroom temperature
Timeovernight
Oxidant / reductant[Rh(CO)2Cl]2
Work-upyellow solution replaced with fresh dichloromethane (5 x 3 mL) under Ar
Activationnone reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 crystals30 mgp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Other[Rh(CO)2Cl]2excessp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Solventdichloromethane3 mL; fresh wash 5 x 3 mLp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Partial recipeSource: Both

Route 11: Other

p012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2

Metal precursors[Rh(CO)2Cl]2; pre-formed MnMOF-1 solvatomorph
Linker precursorspre-formed MnMOF-1
Solventsdiethyl ether
AtmosphereAr
Temperatureroom temperature
Timeovernight
Oxidant / reductant[Rh(CO)2Cl]2
Work-upyellow solution replaced with fresh diethyl ether (5 x 3 mL) under Ar
Activationnone reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 crystals30 mgp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Other[Rh(CO)2Cl]2excessp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Solventdiethyl ether3 mL; fresh wash 5 x 3 mLp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Partial recipeSource: Both

Route 12: Other

p012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2

Metal precursors[Rh(CO)2Cl]2; pre-formed MnMOF-1 solvatomorph
Linker precursorspre-formed MnMOF-1
Solventsp-xylene
AtmosphereAr
Temperatureroom temperature
Timeovernight
Oxidant / reductant[Rh(CO)2Cl]2
Work-upyellow solution replaced with fresh p-xylene (5 x 3 mL) under Ar
Activationnone reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 crystals30 mgp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Other[Rh(CO)2Cl]2excessp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Solventp-xylene3 mL; fresh wash 5 x 3 mLp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Partial recipeSource: Both

Route 13: Other

p012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2

Metal precursors[Rh(CO)2Cl]2; pre-formed MnMOF-1 solvatomorph
Linker precursorspre-formed MnMOF-1
SolventsTHF
AtmosphereAr
Temperatureroom temperature
Timeovernight
Oxidant / reductant[Rh(CO)2Cl]2
Work-upyellow solution replaced with fresh THF (5 x 3 mL) under Ar
Activationnone reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMnMOF-1 crystals30 mgp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Other[Rh(CO)2Cl]2excessp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
SolventTHF3 mL; fresh wash 5 x 3 mLp012-p013 / journal pages 95-96 · Post-synthetic metalation of MnMOF-1 with [Rh(CO)2Cl]2
Vague recipeSource: Main

Route 14: Unknown

p012 / journal page 95 · General experimental

Metal precursorsnot reported in assigned document
Linker precursorsbis-(4-carboxyphenyl-3,5-dimethylpyrazolyl)
SolventsDMF solvate; full parent synthesis not reported here
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Linkerbis-(4-carboxyphenyl-3,5-dimethylpyrazolyl)Not specifiedp012 / journal page 95 · General experimental