Synthesis evidence

Enhancement in electrical conductivity of a porous indium based metal-organic framework upon I2 uptake: Combined experimental and theoretical investigations

Mani P., Mandal N., Roopesh M. et al. · Journal of Materials Chemistry C · 2020 · 4836-4842

5 structured synthesis routes

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

Blocked Missing Si recipeSource: Missing SI

Route 1: Unknown

p002 · Results and discussion

Partial recipeSource: Main

Route 2: Other

p002 · Results and discussion · Fig. S3; Fig. S4

Metal precursorscompound 1; indium already in framework
Linker precursorscompound 1; TDC already in framework
Solventsiodine solution, solvent not explicitly restated in this sentence; likely cyclohexane from preceding route
Additivesiodine, 0.1 M
Atmospherevacuum drying; activation atmosphere not restated
Timeabout 10 days uptake
Oxidant / reductantI2 guest molecule
Work-upSeparated by filtration and dried under vacuum.
ActivationCompound 1 was activated before iodine dispersion; activation conditions not repeated in this paragraph.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1Not specifiedp002 · Results and discussion · Fig. S3; Fig. S4
Additiveiodine solution0.1 Mp002 · Results and discussion · Fig. S3; Fig. S4
Partial recipeSource: Main

Route 3: Other

p002 · Results and discussion · Fig. 1b; Fig. S1

Metal precursorscompound 1; indium already in framework
Linker precursorscompound 1; TDC already in framework
Solventscyclohexane
Additivesiodine guest, 0.1 M in cyclohexane
Atmospherevacuum during activation and drying; uptake atmosphere not specified
Temperature80 activation
Time5 activation; uptake sampled over time intervals
Oxidant / reductantI2 guest molecule
Work-upAt each interval crystals separated by filtration, washed with cyclohexane and dried under vacuum.
Activationcompound 1 activated at 80 deg C for 5 h under vacuum
Scalability contextReported on 100 mg activated MOF.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1 (activated)100 mgp002 · Results and discussion · Fig. 1b; Fig. S1
Additiveiodine0.1 M in cyclohexanep002 · Results and discussion · Fig. 1b; Fig. S1
SolventcyclohexaneNot specifiedp002 · Results and discussion · Fig. 1b; Fig. S1
Partial recipeSource: SI

Route 4: Other

p004 · Figure S1 caption and text · Fig. S1

Metal precursorscompound 1; indium already in framework
Linker precursorscompound 1; TDC already in framework
Solventsnone stated for vapour exposure
Additivesiodine vapours
Atmosphereclosed glass flask with iodine vapours
Timeabout 168 h for 7 day uptake point; graph extends to about 260 h
Oxidant / reductantI2 vapour guest molecule
Work-upIncremental weight measured at each time interval; no washing/drying workup described in SI passage.
Scalability contextReported on about 100 mg compound 1.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1about 100 mgp004 · Figure S1 caption and text · Fig. S1
Additiveiodine vaporsNot specifiedp004 · Figure S1 caption and text · Fig. S1
Partial recipeSource: Main

Route 5: Other

p003 · Results and discussion · Fig. 4

Solventscyclohexane
Timerelease monitored over about 15 days
Work-upI2@1 dispersed in cyclohexane; release monitored by UV-visible spectroscopy.
Scalability context10 mg I2@1 in 4 mL cyclohexane for spectroscopy; Fig. 4 caption also mentions 50 mg in 4 mL for photographs.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherI2@1about 10 mgp003 · Results and discussion · Fig. 4
Solventcyclohexane4 mLp003 · Results and discussion · Fig. 4