cMOF Evidence Base

Synthesis evidence

Bi-porous metal-organic framework with hydrophilic and hydrophobic channels: Selective gas sorption and reversible iodine uptake studies

Chaudhari A.K., Mukherjee S., Nagarkar S.S. et al. · CrystEngComm · 2013 · 9465-9471

3 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

p007 · Gas adsorption details · Fig. S6

SolventsMethanol for guest replacement; vacuum activation
Atmospherevacuum; N2 purge during cooling before gas adsorption
Temperature120
Time24 h room-temperature evacuation plus 48 h at 120 C in main text; SI also reports overnight heating and 2 h pre-measurement degassing
Work-upGuest replacement by exchange with methanol, then evacuation at room temperature for one day.
ActivationFurther heated at 120 C for two days under vacuum; before adsorption, degassed again at 120 C for 2 h using BelPrepvacII.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
SolventmethanolNot specifiedp007 · Gas adsorption details · Fig. S6
Otheras-synthesised compound 1Not specifiedp007 · Gas adsorption details · Fig. S6
Complete recipeSource: Both

Route 2: Other

p004 / 9468 · Results and discussion · Fig. 5

Solventscyclohexane iodine solution; fresh cyclohexane wash
Additivesiodine, 0.01 M in cyclohexane
Atmosphereclosed glass vial; air drying at room temperature
Temperatureroom temperature
Time1
Oxidant / reductantI2 guest/oxidant
Work-upFiltered from pale-yellow supernatant, washed several times with fresh cyclohexane, air-dried at room temperature.
ActivationStarting sample was activated compound 1'.
Scalability contextBatch uptake used 50 mg activated MOF and 3 mL iodine solution.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated compound 1'50 mgp004 / 9468 · Results and discussion · Fig. 5
Oxidantiodine in cyclohexane3 mL · 0.01 Mp004 / 9468 · Results and discussion · Fig. 5
Solventfresh cyclohexane washNot specifiedp004 / 9468 · Results and discussion · Fig. 5
Complete recipeSource: Main

Route 3: Solvothermal

p005-p006 / 9469-9470 · Synthesis of {[(Me2NH2)2].[Cd3(5-tbip)4].2DMF}n (1)

Metal precursorsCd(NO3)2.4H2O, 0.125 mmol (0.039 g)
Linker precursors5tbip ligand, 0.125 mmol (0.028 g)
SolventsDMF (N,N-dimethylformamide), 2 mL
Atmospheresealed glass vial; atmosphere not otherwise specified
Temperature90
Time48; then cooled to room temperature for 24 h
Work-upUpon cooling to room temperature, crystals appeared; isolated product reported in about 86% yield.
Scalability contextSmall sealed-vial solvothermal synthesis; yield reported, no scale-up discussion.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O0.125 mmol (0.039 g)p005-p006 / 9469-9470 · Synthesis of {[(Me2NH2)2].[Cd3(5-tbip)4].2DMF}n (1)
Linker5tbip ligand0.125 mmol (0.028 g)p005-p006 / 9469-9470 · Synthesis of {[(Me2NH2)2].[Cd3(5-tbip)4].2DMF}n (1)
SolventDMF (N,N-dimethyl formamide)2 mLp005-p006 / 9469-9470 · Synthesis of {[(Me2NH2)2].[Cd3(5-tbip)4].2DMF}n (1)