cMOF Evidence Base

Synthesis evidence

Electrochemical oxygen reduction catalysed by Ni3 (hexaiminotriphenylene)2

Miner E.M., Fukushima T., Sheberla D. et al. · Nature Communications · 2016 · 10942

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

main p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode

Metal precursorsnickel(II) chloride hexahydrate (4.6 mg)
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloric acid (HATP.6HCl) salt (10.4 mg)
SolventsMilli-Q water; methanol for workup
Additivesconcentrated aqueous ammonium hydroxide (0.4 ml, 25% aqueous solution)
Atmospherenot specified; capped glass vial
Temperature65
Time15 h growth; water and methanol workup at 65 C; final vacuum dry
Substrate orientationTwo alumina micropolished glassy carbon electrodes placed with polished faces parallel to bottom of reaction vial; only polished face exposed by NMR tube cap.
Work-upHeat electrode in 20 ml Milli-Q water at 65 C for 4 h, rinse, heat again in water at 65 C for 15 h; rinse with CH3OH; heat in fresh CH3OH at 65 C for 5 h; heat in fresh CH3OH at 65 C for 15 h.
ActivationDried under dynamic vacuum and stored under dynamic vacuum.
Scalability contextRecipe modifies two 5 mm glassy carbon electrodes in a 20 ml vial and also produces black powder/film on vial walls.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloric acid (HATP.6HCl) salt10.4 mgmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
Metal Sourcenickel(II) chloride hexahydrate4.6 mgmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
SolventMilli-Q water6 ml for HATP solution; 4 ml for NiCl2 solution; 20 ml for water workupmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
Baseconcentrated aqueous ammonium hydroxide0.4 ml · 25% aqueous solutionmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
SolventCH3OHfresh CH3OH for two heated workup stepsmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
Partial recipeSource: Main

Route 2: Solvothermal

main p.2 · Synthesis and quantification of Ni3(HITP)2 · Supplementary Fig. 4

Metal precursorsnot separately specified for ITO; inferred same NiCl2.6H2O conditions as glassy carbon film
Linker precursorsnot separately specified for ITO; inferred same HATP.6HCl conditions as glassy carbon film
Solventswater/methanol workup not separately specified for ITO
Additivesaqueous ammonium hydroxide not separately specified for ITO
Atmospherenot specified
Temperature65 (inferred from electrode-film route)
Time15 h growth inferred; exact ITO recipe not separately reported
Substrate orientationITO slide/electrode; exact placement not specified
Work-upNot separately specified for ITO in the available text.
ActivationNot separately specified for ITO.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel(II) chloride hexahydratenot separately specified for ITOmain p.2 · Synthesis and quantification of Ni3(HITP)2 · Supplementary Fig. 4
LinkerHATP.6HClnot separately specified for ITOmain p.2 · Synthesis and quantification of Ni3(HITP)2 · Supplementary Fig. 4
Baseaqueous ammonium hydroxidenot separately specified for ITOmain p.2 · Synthesis and quantification of Ni3(HITP)2 · Supplementary Fig. 4
Complete recipeSource: Main

Route 3: Solvothermal

main p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode

Metal precursorsnickel(II) chloride hexahydrate (4.6 mg)
Linker precursorsHATP.6HCl (10.4 mg)
SolventsMilli-Q water; methanol for workup
Additivesconcentrated aqueous ammonium hydroxide (0.4 ml, 25% aqueous solution)
Atmospherenot specified; capped glass vial
Temperature65
Time15 h growth; multiple 4-15 h wash/heating steps; final 15 h vacuum dry
Substrate orientationPowder recovered from remaining reaction mixture after electrode-film synthesis.
Work-upCentrifuge; sonicate solid in 15 ml water for 5 min; heat capped vial with stirring at 65 C for 4 h; repeat with final heating duration 15 h; centrifuge; sonicate in 15 ml CH3OH for 5 min; heat in CH3OH at 65 C for 5 h; repeat CH3OH wash; centrifuge; remove supernatant.
ActivationBlack solid dried under vacuum for 15 h.
Scalability contextPowder is obtained as a secondary solid from the same vial-scale film reaction.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHATP.6HCl10.4 mgmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
Metal Sourcenickel(II) chloride hexahydrate4.6 mgmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
Baseaqueous ammonium hydroxide0.4 ml · 25%main p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
SolventMilli-Q water15 ml portions for powder washingmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode
SolventCH3OH15 ml portions for powder washingmain p.5 · Synthesis of the Ni3(HITP)2 film on glassy carbon electrode