Vague recipeSource: SI
Route 1: Unknown
S2 · Synthesis of NU-1000 installed with NiCB
Synthesis evidence
Increased Electrical Conductivity in a Mesoporous Metal-Organic Framework Featuring Metallacarboranes Guests
Kung C.-W., Otake K., Buru C.T. et al. · Journal of the American Chemical Society · 2018 · 3871-3875
10 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: SI
Route 2: Drop Cast
S4-S5 · Preparation of electrodes
Metal precursorsNiCB@NU-1000 or NU-1000; NiCB for molecular control
Solventsacetone
Atmospheredried in air/room atmosphere
Temperatureroom temperature
Timeovernight drying
Substrate orientationPt IDE with 180 pairs of fingers and 5-um gap
Work-up2 uL suspension drop-cast successively until full coverage; electrodes dried overnight.
Show 2 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NU-1000 or NiCB@NU-1000 | 10 mg/mL in acetone | S4-S5 · Preparation of electrodes |
| Solvent | acetone | Not specified | S4-S5 · Preparation of electrodes |
Complete recipeSource: SI
Route 3: Cvd
S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000
Metal precursorsNiCB@NU-1000, about 10 mg; Mn(CpEt)2 precursor
Linker precursorsPreformed NiCB@NU-1000 framework
Solventswater vapour source for ALD half-cycle
AtmosphereN2 flow, 5 sccm
TemperatureALD chamber 125 C; Mn(CpEt)2 precursor 95 C; water at room temperature
Time30 min pre-hold; 30 cycles Mn(CpEt)2 1-120-120 s; 600 s wait; 30 cycles water 0.015-120-120 s
Oxidant / reductantwater vapour with Mn(CpEt)2 precursor
Work-upDark brown powders obtained after AIM.
Scalability contextAbout 10 mg powder packed in stainless-steel powder holder.
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NiCB@NU-1000 | about 10 mg | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
| Metal Source | Mn(CpEt)2 | Not specified | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
| Oxidant | water vapour | Not specified | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
Complete recipeSource: SI
Route 4: Cvd
S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000
Metal precursorsNU-1000, about 10 mg; Mn(CpEt)2 precursor
Linker precursorsPreformed NU-1000 framework
Solventswater vapour source for ALD half-cycle
AtmosphereN2 flow, 5 sccm
TemperatureALD chamber 125 C; Mn(CpEt)2 precursor 95 C; water at room temperature
Time30 min pre-hold; 30 cycles Mn(CpEt)2 1-120-120 s; 600 s wait; 30 cycles water 0.015-120-120 s
Oxidant / reductantwater vapour with Mn(CpEt)2 precursor
Work-upDark brown powders obtained after AIM.
Scalability contextAbout 10 mg powder packed in stainless-steel powder holder.
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NU-1000 | about 10 mg | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
| Metal Source | Mn(CpEt)2 | Not specified | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
| Oxidant | water vapour | Not specified | S4 · Installation of manganese oxide in NU-1000 and NiCB@NU-1000 |
Complete recipeSource: Both
Route 5: Other
S2 · Synthesis of NU-1000 installed with NiCB
Metal precursorsNU-1000, 80 mg; NiCB, 24 mg
Linker precursorsPreformed NU-1000 framework
SolventsDMF, 16 mL; acetone, 24 mL portions
Atmosphereair/ambient not specified
Temperatureroom temperature during immersion; 80 C drying
Time72 h immersion; acetone wash holds 2 h, overnight, and 2 h; overnight oven drying
Work-upCentrifugation to remove solution; three acetone washing/soaking steps with sonication after adding fresh acetone; collect by centrifugation.
Activationdried in an oven at 80 C overnight
Scalability context80 mg NU-1000 batch; NiCB used at 2 equivalents to Zr6 nodes.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NiCB | 24 mg (0.074 mmol; 2 equivalences to Zr6 nodes) | S2 · Synthesis of NU-1000 installed with NiCB |
| Other | NU-1000 | 80 mg (0.037 mmol) | S2 · Synthesis of NU-1000 installed with NiCB |
| Solvent | DMF | 16 mL | S2 · Synthesis of NU-1000 installed with NiCB |
| Solvent | acetone | 24 mL per wash | S2 · Synthesis of NU-1000 installed with NiCB |
Vague recipeSource: SI
Route 6: Unknown
S2 · Synthesis of NU-1000 installed with NiCB
Complete recipeSource: SI
Route 7: Other
S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction
Metal precursorsSC-NU-1000, about 15 mg crystals; NiCB, 4.5 mg
Linker precursorsPreformed SC-NU-1000
SolventsDMF, 3 mL; acetone, 4.5 mL wash portions; water, 4.5 mL
Atmosphereambient not specified
Temperatureroom temperature
Time168 h NiCB immersion; acetone washing intervals 2 h, overnight, and 2 h
Work-upDMF decanted, NiCB solution added, sample washed three times with acetone by decantation, acetone removed, water added.
Scalability contextSingle-crystal preparation on about 15 mg crystal portion.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NiCB | 4.5 mg | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Other | SC-NU-1000 | ~15 mg crystals | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Solvent | DMF | 3 mL | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Solvent | acetone | 4.5 mL x 3 | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Solvent | water | 4.5 mL | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
Complete recipeSource: SI
Route 8: Other
S5 · Preparation of pellets for conductivity measurements
Metal precursorsNiCB@NU-1000 or NU-1000, about 10 mg
Solventsacetone
Atmosphereair drying step
Temperature80 C final drying
Substrate orientationPellet sandwiched between two conductive FTO substrates for measurement
Work-upImmerse in acetone, remove most acetone by centrifugation, partially dry in air, press in 7 mm die at 0.5 metric ton, dry at 80 C.
Activationdried at 80 C
Scalability contextPellet thickness about 0.7 mm from about 10 mg powder.
Show 2 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | NiCB@NU-1000 or NU-1000 | about 10 mg | S5 · Preparation of pellets for conductivity measurements |
| Solvent | acetone | Not specified | S5 · Preparation of pellets for conductivity measurements |
Complete recipeSource: SI
Route 9: Solvothermal
S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction
Metal precursorsZrCl4, 105 mg
Linker precursorsH4TBAPy, 60 mg
SolventsDEF, 9 mL for ZrCl4/benzoic acid and 6 mL for H4TBAPy
Additivesbenzoic acid, 3 g; TFA, 225 uL; HCl activation
Temperature100 C preheat for 1 h; 120 C solvothermal step
Time1 h preheat; 24 h at 120 C
Work-upCrystals washed with DMF; after HCl activation washed twice with DMF to remove HCl impurities; fresh DMF added.
Activationactivated with HCl, same as prior procedure
Scalability contextPrepared as four portions of about 15 mg crystals for further single-crystal guest installation.
Show 6 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | ZrCl4 | 105 mg | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Linker | H4TBAPy | 60 mg | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Solvent | DEF | 9 mL + 6 mL | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Additive | benzoic acid | 3 g | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Acid | TFA | 225 uL | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
| Acid | HCl | Not specified | S3 · Installation of NiCB in NU-1000 crystals for single-crystal X-ray diffraction |
Vague recipeSource: SI
Route 10: Other
S5 · Preparation of electrodes
Metal precursorsNU-1000, NiCB@NU-1000, Mn-AIM-NU-1000, or Mn-AIM-NiCB@NU-1000
Substrate orientationFTO conductive glass substrates, 8 ohm/sq
Work-upSpin-coated thin films deposited on FTO following a previous study.
Show 1 structured reagent record
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | FTO conductive glass substrates | 8 ohm/sq | S5 · Preparation of electrodes |