Complete recipeSource: Both
Route 1: Solvothermal
S3 · Synthesis of Ni3HBC
Metal precursorsNi(OAc)2.4H2O stock solution: 65.8 mg, 264 umol in 1.5 mL DMF; 150 uL added.
Linker precursorsHBC: 7.0 mg, 8.8 umol, 1 eq.
Solvents447 uL DMF + 433 uL deionized water for HBC solution; metal stock in DMF; DCM and n-hexane used for solvent exchange.
AtmosphereExternal air admitted by loosening the vial cap; final contact curing for transport pellet was under Ar but not part of synthesis.
Temperature85
Time16
Oxidant / reductantOxygen from external air allowed to enter via loosened vial cap.
Work-upSonicate resulting solution 10 min; collect product by centrifugation; wash three times with DMF; soak powder in DCM 30 min with solvent replaced twice at 10 min intervals; repeat same procedure with n-hexane.
ActivationDry under vacuum for 6 h, then heat at 100 deg C under vacuum for an additional 6 h to remove residual solvents; sorption samples were further degassed at 100 deg C for 12 h.
Scalability contextSmall-vial solvothermal synthesis: HBC 7.0 mg in a 2 mL vial; no yield or scale-up data reported.
Show 7 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HBC | 7.0 mg, 8.8 umol, 1 eq | S3 · Synthesis of Ni3HBC |
| Metal Source | Ni(OAc)2.4H2O | 65.8 mg, 264 umol stock; 150 uL stock solution added · 65.8 mg in 1.5 mL DMF | S3 · Synthesis of Ni3HBC |
| Solvent | N,N-dimethylformamide (DMF) | 447 uL in HBC solution plus stock-solution solvent | S3 · Synthesis of Ni3HBC |
| Solvent | deionized water | 433 uL · 18.2 Mohm resistivity | S3 · Synthesis of Ni3HBC |
| Oxidant | oxygen from external air | not quantified | S3 · Synthesis of Ni3HBC |
| Solvent | dichloromethane (DCM) | solvent exchange, 30 min total with two replacements | S3 · Synthesis of Ni3HBC |
| Solvent | n-hexane | solvent exchange, same procedure as DCM | S3 · Synthesis of Ni3HBC |