cMOF Evidence Base

Synthesis evidence

Synthesis of ordered carbonaceous frameworks from organic crystals

Nishihara H., Hirota T., Matsuura K. et al. · Nature Communications · 2017 · 109

8 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

7 · Methods; Materials

Metal precursorsNone
Linker precursorsH4-CPDPy
AtmosphereN2 flow
Temperature599.85
Time1
ActivationHeat treatment of H4-CPDPy at 873 K for 1 h; 5 K min-1 ramp.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherH4-CPDPyNot specified7 · Methods; Materials
Vague recipeSource: Main

Route 2: Unknown

7 · Methods; Materials

Metal precursorsNone; free-base porphyrin control.
Linker precursorsNot detailed; H4-CPDPy synthesized according to literature reference 25.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
LinkerH4-CPDPy precursor not specifiedNot specified7 · Methods; Materials
Partial recipeSource: Main

Route 3: Other

7-8 · Methods; Materials

Metal precursorsNi2-CPDPy
Linker precursorsNi2-CPDPy diacetylene-containing cyclic porphyrin dimer
AtmosphereN2 flow
Temperature319.85
Time0
Work-upHeating stopped immediately when the temperature reached 593 K.
ActivationThermal polymerisation at 593 K; 5 K min-1 ramp.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi2-CPDPyNot specified7-8 · Methods; Materials
Partial recipeSource: Main

Route 4: Other

7-8 · Methods; Materials

Metal precursorsNi2-CPDPy
Linker precursorsNi2-CPDPy diacetylene-containing cyclic porphyrin dimer
AtmosphereN2 flow
Temperature599.85
Time1
ActivationCarbonisation at 873 K for 1 h; 5 K min-1 ramp.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi2-CPDPyNot specified7-8 · Methods; Materials
Partial recipeSource: SI

Route 5: Drop Cast

27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods

SolventsWater
AdditivesNafion solution, 5%
Temperatureroom temperature
Substrate orientationGlassy carbon plate, 2 cm2
Work-upSonicated to form catalyst ink; ink dropped on glassy carbon.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi2-CPDPy973(1)55 ug cm-2 loaded catalyst27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods
AdditiveNafion solution0.13 ug cm-2 Nafion · 5%27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods
SolventwaterNot specified27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods
Partial recipeSource: Main

Route 6: Other

7-8 · Methods; Materials

Metal precursorsNi2-CPDPy
Linker precursorsNi2-CPDPy diacetylene-containing cyclic porphyrin dimer
AtmosphereN2 flow
Temperature699.85
Time1
ActivationCarbonisation at 973 K for 1 h; 5 K min-1 ramp.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi2-CPDPyNot specified7-8 · Methods; Materials
Vague recipeSource: Main

Route 7: Unknown

7-8 · Methods; Author contributions

Metal precursorsNot detailed; synthesized according to literature reference 22.
Linker precursorsNot detailed; cyclic porphyrin dimer CPDPy ligand system.
Work-upGuest-free crystals used as precursor; preparation details not given in this paper.
Scalability contextAuthors note methods were improved to provide sufficient amounts, but recipe is external.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi precursor not specified in this paperNot specified7-8 · Methods; Author contributions
LinkerCPDPy cyclic porphyrin dimer precursor not specifiedNot specified7-8 · Methods; Author contributions
Partial recipeSource: Both

Route 8: Other

27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods

Metal precursors5,10,15,20-tetraphenyl-21H,23H-porphine nickel(II) (Ni-TPP)
Linker precursorsTetraphenylporphyrin
AtmosphereN2 flow
Temperature699.85
Time1
ActivationSame carbonisation procedure as Ni2-CPDPy973(1).
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal Source5,10,15,20-tetraphenyl-21H,23H-porphine nickel(II)Not specified27 · Evaluation of selective CO2 reduction into CO · Supplementary Methods