Synthesis evidence

Ni(II)-Based Coordination Polymer with Pi-Conjugated Organic Linker as Catalyst for Oxygen Evolution Reaction Activity

Kumar T., Karmakar A., Halder A. et al. · Energy and Fuels · 2022 · 2722-2730

2 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

2723 · 2.2 Synthesis of [Ni(MCA)(bipy)(H2O)2]n CP 1 · Scheme 1

Metal precursorsNi(NO3)2.6H2O (20 mg, 0.07 mmol)
Linker precursorsmesaconic acid (9 mg, 0.07 mmol); 4,4'-bipyridine (11 mg, 0.07 mmol)
Solventsdeionized water/DMF (1:2), total 3 mL
Atmospherenot reported
Temperature80
Time72
Work-upCooled to room temperature, filtered, and washed with deionized water/DMF (1:2).
Activationnot reported
Scalability context15 mL capped glass vial; yield 60%.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O20 mg, 0.07 mmol2723 · 2.2 Synthesis of [Ni(MCA)(bipy)(H2O)2]n CP 1 · Scheme 1
Linkermesaconic acid9 mg, 0.07 mmol2723 · 2.2 Synthesis of [Ni(MCA)(bipy)(H2O)2]n CP 1 · Scheme 1
Linker4,4'-bipyridine11 mg, 0.07 mmol2723 · 2.2 Synthesis of [Ni(MCA)(bipy)(H2O)2]n CP 1 · Scheme 1
Solventdeionized water/DMF (1:2)3 mL2723 · 2.2 Synthesis of [Ni(MCA)(bipy)(H2O)2]n CP 1 · Scheme 1
Complete recipeSource: Main

Route 2: Hydrothermal

2723 · 2.3 Synthesis of CP 2

Metal precursorsNi(ClO4)2.6H2O (55 mg, 0.15 mmol)
Linker precursors4,4'-bipyridine (94 mg, 0.60 mmol)
Solventsdeionized water, 5 mL
Atmospherenot reported
Temperature130
Time48
Work-upCooled to room temperature; blue crystals filtered and washed with deionized water.
Activationnot reported
Scalability context25 mL Teflon-lined stainless-steel autoclave; yield 50%; recipe follows previous report.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(ClO4)2.6H2O55 mg, 0.15 mmol2723 · 2.3 Synthesis of CP 2
Linker4,4'-bipyridine94 mg, 0.60 mmol2723 · 2.3 Synthesis of CP 2
Solventdeionized water5 mL2723 · 2.3 Synthesis of CP 2