Synthesis evidence

Chemiresistive Detection of Gaseous Hydrocarbons and Interrogation of Charge Transport in Cu[Ni(2,3-pyrazinedithiolate) 2 ] by Gas Adsorption

Aubrey M.L., Kapelewski M.T., Melville J.F. et al. · Journal of the American Chemical Society · 2019 · 5005-5013

1 structured synthesis route

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

Complete recipeSource: Main

Route 1: Other

main p.5006 · Modified Synthesis of Cu[Ni(pdt)2]

Metal precursorsNa2[Ni(pdt)2] (0.630 g, 1.62 mmol); CuI (0.309 g, 1.62 mmol)
Linker precursorspdt2- already incorporated in Na2[Ni(pdt)2], prepared according to literature procedure.
SolventsAcetonitrile, 270 mL for Na2[Ni(pdt)2] solution and 75 mL for CuI solution.
AtmosphereDry N2 sparge for both flasks, then positive N2 during CuI addition; filtration in air.
TemperatureRoom temperature for precipitation; 90 C activation
Time0.5 h N2 sparge for each solution; overnight activation
Work-upCuI solution slowly added by syringe to Na2[Ni(pdt)2] solution causing rapid precipitation; solid filtered on 0.22 um nylon filter paper in air.
ActivationActivated overnight at 90 C under high vacuum on a Micromeritics ASAP 2420 with turbo pump.
Scalability contextReported isolated yield was 0.453 g, 69%, as a dark red microcrystalline powder.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNa2[Ni(pdt)2]0.630 g, 1.62 mmolmain p.5006 · Modified Synthesis of Cu[Ni(pdt)2]
Metal SourceCuI0.309 g, 1.62 mmolmain p.5006 · Modified Synthesis of Cu[Ni(pdt)2]
Solventacetonitrile270 mL plus 75 mLmain p.5006 · Modified Synthesis of Cu[Ni(pdt)2]
Otherdry N2sparged 30 min per flask; positive atmosphere during additionmain p.5006 · Modified Synthesis of Cu[Ni(pdt)2]