cMOF Evidence Base

Synthesis evidence

Reversible iodine absorption of nonporous coordination polymer Cu(TCNQ)

Miyao K., Funabiki A., Takahashi K. et al. · New Journal of Chemistry · 2014 · 739-743

13 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

p002-p003 / article pages 740-741 · Results; Experimental · Fig. 3; Fig. 6

Metal precursorsCu(TCNQ)I4 generated from phase I Cu(TCNQ)
Linker precursorsTCNQ in Cu(TCNQ)I4
Solventsnone
Atmospherevacuum
Temperature200
Time1.5
Oxidant / reductantiodine desorption by annealing
Work-upannealing under vacuum
Activation200 C for 1.5 h under vacuum
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu(TCNQ)I4not specifiedp002-p003 / article pages 740-741 · Results; Experimental · Fig. 3; Fig. 6
Partial recipeSource: Main

Route 2: Other

p002 / article page 740 · Results; Experimental · Fig. 3

Metal precursorsCu(TCNQ)I4 generated from phase II Cu(TCNQ)
Linker precursorsTCNQ in Cu(TCNQ)I4
Solventsnone
Atmospherevacuum
Temperature200
Time1.5
Oxidant / reductantiodine desorption by annealing
Work-upannealing under vacuum
Activation200 C for 1.5 h under vacuum
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu(TCNQ)I4not specifiedp002 / article page 740 · Results; Experimental · Fig. 3
Partial recipeSource: Both

Route 3: Other

p003 / article page 741 · Results · Fig. S6

Metal precursorsCu(TCNQ)In n = 2.1 liquid-phase mixture
Linker precursorsTCNQ in Cu(TCNQ)In
Solventsnone specified during milling
Atmospherenot specified
Timenot specified
Oxidant / reductantmechanochemical redistribution of iodine
Work-upball-milling
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu(TCNQ)In (n = 2.1)not specifiedp003 / article page 741 · Results · Fig. S6
Vague recipeSource: Main

Route 4: Other

p003 / article page 741 · Results

Metal precursorsCuI
Linker precursorsTCNQ
Solventsnot specified; implied grinding solid-state reaction
Atmospherenot specified
Oxidant / reductantI2
Work-upnot specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuInot specifiedp003 / article page 741 · Results
LinkerTCNQnot specifiedp003 / article page 741 · Results
OxidantI2not specifiedp003 / article page 741 · Results
Vague recipeSource: Main

Route 5: Unknown

p004 / article page 742 · Experimental

Metal precursorsnot reported; prepared according to literature ref. 7
Linker precursorsnot reported; prepared according to literature ref. 7
Solventsnot reported
Atmospherenot reported
Work-upnot reported
Vague recipeSource: Main

Route 6: Unknown

p004 / article page 742 · Experimental

Metal precursorsnot reported; prepared according to literature ref. 7
Linker precursorsnot reported; prepared according to literature ref. 7
Solventsnot reported
Atmospherenot reported
Work-upnot reported
Partial recipeSource: Main

Route 7: Other

p002 / article page 740 · Results · Fig. 2

Metal precursorsCu(TCNQ)I4 from phase I or phase II Cu(TCNQ)
Linker precursorsTCNQ in Cu(TCNQ)I4
Solventshexane
Atmospherenot specified
Time960
Oxidant / reductantiodine desorption
Work-upnot specified
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ)I4not specifiedp002 / article page 740 · Results · Fig. 2
Solventhexanenot specifiedp002 / article page 740 · Results · Fig. 2
Partial recipeSource: Main

Route 8: Other

p003 / article page 741 · Iodine absorption by liquid-phase reaction

Metal precursorsCu(TCNQ) phase II
Linker precursorsTCNQ already in Cu(TCNQ)
Solventshexane solution of iodine
Atmospherenot explicitly stated
Temperature12 inferred from liquid-phase recipe
Timeabout 1440
Oxidant / reductantiodine
Work-upnot specified for phase II partial product
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ) phase IInot specifiedp003 / article page 741 · Iodine absorption by liquid-phase reaction
Solventhexanenot specified for phase IIp003 / article page 741 · Iodine absorption by liquid-phase reaction
Oxidantiodinenot specified for phase IIp003 / article page 741 · Iodine absorption by liquid-phase reaction
Complete recipeSource: Main

Route 9: Other

p004 / article page 742 · Experimental

Metal precursorsCu(TCNQ) phase I
Linker precursorsTCNQ already in Cu(TCNQ)
Solventshexane, 300 mL
Atmospherenot explicitly stated; reactions under air gave heterogeneous hygroscopic mixtures
Temperature12
Time168-336
Oxidant / reductantiodine in hexane
Work-upcollected by filtration, washed with hexane, vacuum dried for 10 min
Scalability context97 mg Cu(TCNQ), 830 mg iodine in 300 mL hexane.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ)97 mg, 3.6 x 10-4 molp004 / article page 742 · Experimental
Solventhexane300 mLp004 / article page 742 · Experimental
Oxidantiodine830 mg, 3.3 x 10-3 molp004 / article page 742 · Experimental
Partial recipeSource: Main

Route 10: Other

p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3b

Metal precursorsCu(TCNQ) phase II
Linker precursorsTCNQ already in Cu(TCNQ)
Solventssolventless
Additivesfew drops of water can accelerate reaction
Atmospherenot specified; reactions under air produced heterogeneous hygroscopic mixtures
Time0.5-1.5
Oxidant / reductantI2
Work-upnone specified for solid-state grinding product
Scalability contextTotal mixture about 0.2 g; ball milling at 750 rpm.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ) phase IIpart of about 0.2 g mixture · molar ratio Cu(TCNQ):I2 = 1:2p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3b
OxidantI2part of about 0.2 g mixture · molar ratio Cu(TCNQ):I2 = 1:2p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3b
Additivewatera few drops, optional acceleratorp001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3b
Partial recipeSource: Main

Route 11: Other

p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3a

Metal precursorsCu(TCNQ) phase I
Linker precursorsTCNQ already in Cu(TCNQ)
Solventssolventless
Additivesfew drops of water can accelerate reaction
Atmospherenot specified; reactions under air produced heterogeneous hygroscopic mixtures
Time0.5-1.5
Oxidant / reductantI2
Work-upnone specified for solid-state grinding product
Scalability contextTotal mixture about 0.2 g; ball milling at 750 rpm.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ) phase Ipart of about 0.2 g mixture · molar ratio Cu(TCNQ):I2 = 1:2p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3a
OxidantI2part of about 0.2 g mixture · molar ratio Cu(TCNQ):I2 = 1:2p001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3a
Additivewatera few drops, optional acceleratorp001 and p004 / article pages 739 and 742 · Results; Experimental · Fig. 3a
Partial recipeSource: Both

Route 12: Other

p002 · Supporting Information · Fig. S3

Metal precursorsCu(TCNQ) phase II
Linker precursorsTCNQ already in Cu(TCNQ)
Solventssolventless
Atmospherenot specified
Timenot specified for stepwise experiment
Oxidant / reductantstepwise addition of iodine
Work-upnot specified
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ) phase IInot specifiedp002 · Supporting Information · Fig. S3
OxidantI2stepwise addition to n = 1, 2, 3, and 4p002 · Supporting Information · Fig. S3
Partial recipeSource: Main

Route 13: Other

p002-p003 / article pages 740-741 · Results · Fig. 5

Metal precursorsCu(TCNQ) phase I
Linker precursorsTCNQ already in Cu(TCNQ)
Solventssolventless
Atmospherenot specified
Timenot specified for stepwise experiment
Oxidant / reductantstepwise addition of iodine
Work-upnot specified
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu(TCNQ) phase Inot specifiedp002-p003 / article pages 740-741 · Results · Fig. 5
OxidantI2stepwise addition to n = 1, 2, and 4p002-p003 / article pages 740-741 · Results · Fig. 5