cMOF Evidence Base

Synthesis evidence

Cofacial Assembly of Metallomacrocycles as an Approach to Controlling Lattice Architecture in Low-Dimensional Molecular Solids. Chemical, Structural, Oxidation-State, Transport, and Optical Properties of the Coordination Polymer [Fe(phthalocyaninato)(μ-pyrazine)]n and the Consequences of Halogen Doping

Diel B.N., Inabe T., Jaggi N.K. et al. · Journal of the American Chemical Society · 1984 · 3207-3214

10 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

3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I

Metal precursors[Fe(Pc)(pyz)]n polymer
Linker precursorsmu-pyrazine in polymer
Solventsbenzene, ca. 0.1 mL portions
Temperatureroom temperature
Timetotal grinding time ca. 10-15 min
Oxidant / reductantiodine, 6.4 mg
Work-upwet with benzene, grind until benzene evaporated; repeat twice more to yield finely divided black solid
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other[Fe(Pc)(pyz)]n130 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
OxidantI26.4 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Solventbenzeneca. 0.1 mL, repeated3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Partial recipeSource: Main

Route 2: Other

3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I

Metal precursors[Fe(Pc)(pyz)]n polymer
Linker precursorsmu-pyrazine in polymer
Solventsbenzene, ca. 0.1 mL portions
Temperatureroom temperature
Timetotal grinding time ca. 10-15 min
Oxidant / reductantiodine, 12.7 mg
Work-upwet with benzene, grind until benzene evaporated; repeat twice more to yield finely divided black solid
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other[Fe(Pc)(pyz)]n130 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
OxidantI212.7 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Solventbenzeneca. 0.1 mL, repeated3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Partial recipeSource: Main

Route 3: Other

3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I

Metal precursors[Fe(Pc)(pyz)]n polymer
Linker precursorsmu-pyrazine in polymer
Solventsbenzene, ca. 0.1 mL portions
Temperatureroom temperature
Timetotal grinding time ca. 10-15 min
Oxidant / reductantiodine, 50.8 mg
Work-upwet with benzene, grind until benzene evaporated; repeat twice more to yield finely divided black solid
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other[Fe(Pc)(pyz)]n260 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
OxidantI250.8 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Solventbenzeneca. 0.1 mL, repeated3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Partial recipeSource: Main

Route 4: Other

3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I

Metal precursors[Fe(Pc)(pyz)]n polymer
Linker precursorsmu-pyrazine in polymer
Solventsbenzene, ca. 0.1 mL portions
Temperatureroom temperature
Timetotal grinding time ca. 10-15 min; analysis after 1 week
Oxidant / reductantiodine, 101.5 mg
Work-upwet with benzene, grind until benzene evaporated; repeat twice more to yield finely divided black solid
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other[Fe(Pc)(pyz)]n130 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
OxidantI2101.5 mg3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Solventbenzeneca. 0.1 mL, repeated3208 · Iodine Doping, Starting with [Fe(Pc)(pyz)]n · Table I
Partial recipeSource: Main

Route 5: Other

3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II

Metal precursorsFe(Pc)(pyz)2
Linker precursorspyrazine
SolventsCHCl3, 10 mL
Temperatureroom temperature
Time24
Oxidant / reductantiodine, 25.4 mg
Work-upstir 24 h; centrifuge; remove supernatant containing iodine from black precipitate
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)(pyz)2146 mg (0.2 mmol)3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
OxidantI225.4 mg3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
SolventCHCl310 mL3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
Partial recipeSource: Main

Route 6: Other

3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II

Metal precursorsFe(Pc)(pyz)2
Linker precursorspyrazine
SolventsCHCl3, 10 mL
Temperatureroom temperature
Time24
Oxidant / reductantiodine, 113.5 mg
Work-upstir 24 h; centrifuge; remove supernatant containing iodine from black precipitate
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)(pyz)2292 mg3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
OxidantI2113.5 mg3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
SolventCHCl310 mL3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
Partial recipeSource: Main

Route 7: Other

3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II

Metal precursorsFe(Pc)(pyz)2
Linker precursorspyrazine
SolventsCHCl3, 10 mL
Temperatureroom temperature
Time24
Oxidant / reductantiodine, 203 mg
Work-upstir 24 h; centrifuge; remove supernatant containing iodine from black precipitate
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)(pyz)2292 mg3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
OxidantI2203 mg3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
SolventCHCl310 mL3208 · Iodine Doping, Starting with Fe(Pc)(pyz)2 · Table II
Partial recipeSource: Main

Route 8: Other

3209 · Polymer Synthesis and Structure · eq 1

Metal precursorsFe(Pc)
Linker precursorspyrazine
Solventspyrazine, neat
Temperatureheated; exact temperature not reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)Not specified3209 · Polymer Synthesis and Structure · eq 1
LinkerpyrazineNot specified3209 · Polymer Synthesis and Structure · eq 1
Partial recipeSource: Main

Route 9: Other

3209 · Polymer Synthesis and Structure · eq 2

Metal precursorsFe(Pc)(pyz)2
Linker precursorspyrazine already coordinated; pyrazine eliminated
SolventsCHCl3
Temperatureroom temperature
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)(pyz)2Not specified3209 · Polymer Synthesis and Structure · eq 2
SolventCHCl3Not specified3209 · Polymer Synthesis and Structure · eq 2
Partial recipeSource: Main

Route 10: Other

3209 · Polymer Synthesis and Structure · eq 3

Metal precursorsFe(Pc)
Linker precursorspyrazine
SolventsC6H5Cl or benzene
Temperatureheated; exact temperature not reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(Pc)Not specified3209 · Polymer Synthesis and Structure · eq 3
LinkerpyrazineNot specified3209 · Polymer Synthesis and Structure · eq 3
SolventC6H5Cl or benzeneNot specified3209 · Polymer Synthesis and Structure · eq 3