Synthesis evidence

Superexchange Charge Transport in Loaded Metal Organic Frameworks

Neumann T., Liu J., Wachter T. et al. · ACS Nano · 2016 · 7085-7093

6 structured synthesis routes

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

Vague recipeSource: SI

Route 1: Other

S11 · 2.6 Results for an alternative SAM template

Metal precursorspreformed/grown HKUST-1 SURMOF on alternative SAM template
Linker precursors16-mercaptohexadecanoic acid SAM; TCNQ guest
Substrate orientationalternative COOH-terminated SAM; different SURMOF orientation by XRD
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Other16-mecaptohexadecanoic acidNot specifiedS11 · 2.6 Results for an alternative SAM template
AdditiveTCNQNot specifiedS11 · 2.6 Results for an alternative SAM template
Complete recipeSource: SI

Route 2: Other

S2 · 1.2 Preparation of the SAMs template · Figure S1

Linker precursors9-carboxy-10-(mercaptomethyl)triptycene thiol (CMMT)
Solventsethanol
Atmospheredark; room-temperature immersion; dried under N2 stream
Temperatureroom temperature
Time72
Substrate orientationpolycrystalline 5 nm Ti / 100 nm Au on Si(100), predominantly Au(111) grains
Work-uprinsed with ethanol and dried under N2 stream
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker9-carboxy-10-(mercaptomethyl)triptycene thiol (CMMT)20 uMS2 · 1.2 Preparation of the SAMs template · Figure S1
SolventethanolNot specifiedS2 · 1.2 Preparation of the SAMs template · Figure S1
Other5 nm Ti / 100 nm Au on silicon (100) waferNot specifiedS2 · 1.2 Preparation of the SAMs template · Figure S1
Complete recipeSource: SI

Route 3: Other

S3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ

Metal precursorspreformed HKUST-1 SURMOF
Linker precursorsF4-TCNQ guest
Solventsethanol
Atmosphereactivation in air; drying under nitrogen flow
Temperature60 C activation; room-temperature loading
Time0.333 h activation; 72 h loading
Substrate orientationCMMT SAM-modified Au/Si with HKUST-1 SURMOF
Work-uprinsed abundantly with ethanol and dried under nitrogen flow
Activationheated at 60 C for 20 minutes in air
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherpristine HKUST-1 SURMOFNot specifiedS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ
Additive2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquino-dimethane (F4-TCNQ)2 mMS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ
SolventethanolNot specifiedS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ
Complete recipeSource: SI

Route 4: Other

S2-S3 · 1.3 Preparation of SURMOFs

Metal precursorscopper acetate monohydrate
Linker precursors1,3,5-benzenetricarboxylic acid (BTC)
Solventsethanol
Substrate orientationCMMT SAM-modified Au substrate
Work-upafter spraying of metal and linker solutions, 25 s waiting time for crystallisation; target abundantly rinsed with ethanol; cycles repeated to set thickness
Scalability contextThickness controlled by number of spray cycles.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate monohydrate1 mM ethanolic solutionS2-S3 · 1.3 Preparation of SURMOFs
Linker1,3,5-benzenetricarboxylic acid (BTC)0.1 mM ethanolic solutionS2-S3 · 1.3 Preparation of SURMOFs
SolventethanolNot specifiedS2-S3 · 1.3 Preparation of SURMOFs
OtherCMMT SAM modified Au substrateNot specifiedS2-S3 · 1.3 Preparation of SURMOFs
Partial recipeSource: SI

Route 5: Other

S11 · 2.5 Results for an alternative solvent

Metal precursorspreformed HKUST-1 SURMOF
Linker precursorsTCNQ or F4-TCNQ guest
Solventsdichloromethane (DCM)
Temperatureroom temperature
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherpreformed HKUST-1 SURMOFNot specifiedS11 · 2.5 Results for an alternative solvent
AdditiveTCNQ or F4-TCNQNot specifiedS11 · 2.5 Results for an alternative solvent
Solventdichloromethane (DCM)Not specifiedS11 · 2.5 Results for an alternative solvent
Complete recipeSource: SI

Route 6: Other

S3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ

Metal precursorspreformed HKUST-1 SURMOF
Linker precursorsTCNQ guest
Solventsethanol
Atmosphereactivation in air; drying under nitrogen flow
Temperature60 C activation; room-temperature loading
Time0.333 h activation; 72 h loading
Substrate orientationCMMT SAM-modified Au/Si with HKUST-1 SURMOF
Work-uprinsed abundantly with ethanol and dried under nitrogen flow
Activationheated at 60 C for 20 minutes in air
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherpristine HKUST-1 SURMOFNot specifiedS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ
Additive7,7,8,8-tetracyanoquinodimethane (TCNQ)2 mMS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ
SolventethanolNot specifiedS3 · 1.4 Loading of SURMOFs with TCNQ and F4-TCNQ