cMOF Evidence Base

Synthesis evidence

Solid-state structural transformation doubly triggered by reaction temperature and time in 3D metal-organic frameworks: Great enhancement of stability and gas adsorption

Shen P., He W.-W., Du D.-Y. et al. · Chemical Science · 2014 · 1368-1374

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

p002-p003 · S3. Electrical conductivity values

Metal precursorsactivated IFMC-69
Solventsanhydrous methanol; dichloromethane; hexane
AdditivesI2
Atmosphereoil-pump evacuation; other atmosphere not specified
Temperature45
Time24 h I2 soak; 2 h evacuation
Oxidant / reductantiodine guest/oxidising molecule
Work-upMethanol wash/soak, dichloromethane wash/soak, solvent decanting, iodine loading in hexane, evacuation.
ActivationEvacuated with an oil pump at 45 C for 2 h before and after iodine loading.
Scalability context0.9 g activated IFMC-69 prepared; half loaded to give 0.49 g activated I2@IFMC-69.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherIFMC-690.9 g activated IFMC-69; half usedp002-p003 · S3. Electrical conductivity values
AdditiveI20.05 mol/L in hexanep002-p003 · S3. Electrical conductivity values
SolventhexaneNot specifiedp002-p003 · S3. Electrical conductivity values
Solventanhydrous methanol3 x 50 mLp002-p003 · S3. Electrical conductivity values
Solventdichloromethane3 x 50 mLp002-p003 · S3. Electrical conductivity values
Complete recipeSource: Main

Route 2: Solvothermal

p006 / 1373 · Experimental, Synthesis of IFMC-68

Metal precursorsZn(NO3)2.6H2O (0.150 g, 0.504 mmol)
Linker precursorsH4L (0.050 g, 0.081 mmol)
SolventsDMA (5 mL)
Atmospheresealed Teflon-lined steel container; atmosphere not specified
Temperature85
Time72
Work-upColourless crystals collected, washed with Et2O, and dried at room temperature.
Scalability context0.050 g linker scale; yield 79% based on H4L.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.150 g, 0.504 mmolp006 / 1373 · Experimental, Synthesis of IFMC-68
LinkerH4L0.050 g, 0.081 mmolp006 / 1373 · Experimental, Synthesis of IFMC-68
SolventDMA5 mLp006 / 1373 · Experimental, Synthesis of IFMC-68
Complete recipeSource: Main

Route 3: Solvothermal

p006 / 1373 · Experimental, Synthesis of IFMC-69

Metal precursorsZn(NO3)2.6H2O (0.150 g, 0.504 mmol)
Linker precursorsH4L (0.050 g, 0.081 mmol)
SolventsDMA (5 mL)
Atmospheresealed Teflon-lined steel container; atmosphere not specified
Temperature140
Time72
Work-upColourless crystals collected, washed with Et2O, and dried at room temperature.
Scalability context0.050 g linker scale; yield 63% based on H4L.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.150 g, 0.504 mmolp006 / 1373 · Experimental, Synthesis of IFMC-69
LinkerH4L0.050 g, 0.081 mmolp006 / 1373 · Experimental, Synthesis of IFMC-69
SolventDMA5 mLp006 / 1373 · Experimental, Synthesis of IFMC-69
Complete recipeSource: SI

Route 4: Other

p002 · S1. Materials and instrumentations for measurements

Metal precursorsas-synthesised IFMC-69
Solventsmethanol; dichloromethane
Atmospheredynamic vacuum; outgas function
Temperatureroom temperature
Time24 h methanol, additional 24 h methanol, additional methanol exchange, dichloromethane similarly, overnight vacuum, 12 h outgas
Work-upDecant solvent exchanges; remove dichloromethane by decanting.
ActivationDynamic vacuum at room temperature overnight, then 12 h outgas at room temperature.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
SolventmethanolNot specifiedp002 · S1. Materials and instrumentations for measurements
SolventdichloromethaneNot specifiedp002 · S1. Materials and instrumentations for measurements
Complete recipeSource: Main

Route 5: Other

p006 / 1373 · Experimental, The process of SCSC transformation

Metal precursorsIFMC-68 crystals (50 mg)
Linker precursorsframework linker already present in IFMC-68
SolventsDMA (5 mL)
Atmospheresealed Teflon liner; atmosphere not specified
Temperature140
Time72
Work-upColourless block single crystals of IFMC-69 collected.
Scalability context50 mg IFMC-68 transformation scale.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherIFMC-6850 mgp006 / 1373 · Experimental, The process of SCSC transformation
SolventDMA5 mLp006 / 1373 · Experimental, The process of SCSC transformation
Complete recipeSource: Main

Route 6: Other

p005-p006 / 1372-1373 · Results and discussion / Experimental · Fig. 4

Metal precursorsIFMC-68 crystals (50 mg)
Linker precursorsframework linker already present in IFMC-68
Solventsnone
Atmospheresealed Teflon liner without solvent; atmosphere not specified
Temperature140
Time24
Work-upColourless block single crystals of IFMC-69 collected.
Scalability context50 mg IFMC-68 transformation scale.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherIFMC-6850 mgp005-p006 / 1372-1373 · Results and discussion / Experimental · Fig. 4