Synthesis evidence

Confinement of single polysilane chains in coordination nanospaces

Kitao T., Bracco S., Comotti A. et al. · Journal of the American Chemical Society · 2015 · 5231-5238

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

p002 · Experimental Section - Introduction of PMPrS into 1

Metal precursorspreformed Al PCP host 1a
Linker precursorspreformed 2,6-naphthalenedicarboxylate PCP framework
Solventshexane
AdditivesPMPrS guest polymer
Atmospherereduced pressure/evacuation during drying and solvent removal
Temperature150 activation; 120 loading/solvent removal
Time5 activation; 12 loading/solvent removal
Work-upHost powder immersed in PMPrS hexane solution at room temperature; hexane completely removed by evacuation at 120 C for 12 h to obtain powdery composite.
ActivationCompound 1 (150 mg) dried by evacuation at 150 C for 5 h before immersion.
Scalability contextGeneral procedure used 150 mg host and 64 mg PMPrS in 1 mL hexane, yielding 211 mg composite.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1a host powder150 mgp002 · Experimental Section - Introduction of PMPrS into 1
AdditivePMPrS64 mgp002 · Experimental Section - Introduction of PMPrS into 1
Solventhexane1 mLp002 · Experimental Section - Introduction of PMPrS into 1
Complete recipeSource: Main

Route 2: Other

p002 · Experimental Section - Introduction of PMPrS into 1

Metal precursorspreformed Al PCP host 1b
Linker precursorspreformed 4,4'-biphenyldicarboxylate PCP framework
Solventshexane
AdditivesPMPrS guest polymer
Atmospherereduced pressure/evacuation during drying and solvent removal
Temperature150 activation; 120 loading/solvent removal
Time5 activation; 12 loading/solvent removal
Work-upHost powder immersed in PMPrS hexane solution at room temperature; hexane completely removed by evacuation at 120 C for 12 h to obtain powdery composite.
ActivationCompound 1 (150 mg) dried by evacuation at 150 C for 5 h before immersion.
Scalability contextGeneral procedure used 150 mg host and 64 mg PMPrS in 1 mL hexane, yielding 211 mg composite.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1b host powder150 mgp002 · Experimental Section - Introduction of PMPrS into 1
AdditivePMPrS64 mgp002 · Experimental Section - Introduction of PMPrS into 1
Solventhexane1 mLp002 · Experimental Section - Introduction of PMPrS into 1
Vague recipeSource: Main

Route 3: Unknown

p002 · Experimental Section - Materials and Measurement

Linker precursors2,6-naphthalenedicarboxylate ligand implied by material formula
ActivationFor adsorption measurements, treated under reduced pressure (<10^-2 Pa) at 373 K for 5 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Linker2,6-naphthalenedicarboxylateNot specifiedp002 · Experimental Section - Materials and Measurement
Vague recipeSource: Main

Route 4: Unknown

p002 · Experimental Section - Materials and Measurement

Linker precursors4,4'-biphenyldicarboxylate ligand implied by material formula
ActivationFor adsorption measurements, treated under reduced pressure (<10^-2 Pa) at 373 K for 5 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Linker4,4'-biphenyldicarboxylateNot specifiedp002 · Experimental Section - Materials and Measurement
Complete recipeSource: Main

Route 5: Other

p002 · Experimental Section - Synthesis of PMPrS

Linker precursorsdichloromethylpropylsilane
Solventstoluene; 2-propanol and methanol for fractional precipitation
Additiveschlorotrimethylsilane terminator
Temperature120
Time2
Oxidant / reductantsodium metal reductant for Wurtz-type condensation
Work-upIsolated by fractional precipitation with successive additions of 2-propanol (5 mL) and methanol (5 mL); insoluble fraction dried in vacuum; yield 19%.
Scalability contextReported product after fractional precipitation had Mn = 3600 and Mw/Mn = 1.64.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Otherdichloromethylpropylsilane20 mmolp002 · Experimental Section - Synthesis of PMPrS
ReductantsodiumNot specifiedp002 · Experimental Section - Synthesis of PMPrS
Solventtoluene14 mLp002 · Experimental Section - Synthesis of PMPrS
Additivechlorotrimethylsilane10 mmolp002 · Experimental Section - Synthesis of PMPrS
Solvent2-propanol5 mLp002 · Experimental Section - Synthesis of PMPrS
Solventmethanol5 mLp002 · Experimental Section - Synthesis of PMPrS