Synthesis evidence

A semiconducting layered metal-organic framework magnet

Yang C., Dong R., Wang M. et al. · Nature Communications · 2019 · 3260

2 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p007 · Typical synthesis of K3Fe2[PcFe-O8]

Metal precursorsiron(II) acetate, 9.4 mg, 0.054 mmol
Linker precursorsPcFe-OH8, 20 mg, 0.029 mmol
SolventsN-methyl-2-pyrrolidone/H2O, 3 mL/1 mL v/v
Additivespotassium acetate (KOAc), 26 mg, 0.26 mmol
AtmosphereDegassed by freeze-pump-thaw three times; sealed under high vacuum; general reactions under vacuum/Schlenk line or nitrogen.
Temperature150
Time72
Work-upCooled to room temperature, filtrated, soaked in degassed H2O for 1 day, washed by acetone and filtration.
ActivationDried under vacuum at 40 C; for BET, powder was treated in a supercritical CO2 dryer for 5 days and activated at 80 C overnight.
Scalability contextSmall 25 mL tube solvothermal/vacuum-sealed route; reported yield 88.4%.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerPcFe-OH820 mg, 0.029 mmolp007 · Typical synthesis of K3Fe2[PcFe-O8]
Metal Sourceiron (II) acetate9.4 mg, 0.054 mmolp007 · Typical synthesis of K3Fe2[PcFe-O8]
AdditiveKOAc26 mg, 0.26 mmolp007 · Typical synthesis of K3Fe2[PcFe-O8]
SolventN-methyl-2-pyrrolidone (NMP)3 mLp007 · Typical synthesis of K3Fe2[PcFe-O8]
SolventH2O1 mL in reaction; degassed H2O soak for 1 day during workupp007 · Typical synthesis of K3Fe2[PcFe-O8]
Solventacetonewashing solventp007 · Typical synthesis of K3Fe2[PcFe-O8]
Vague recipeSource: SI

Route 2: Solvothermal

p014 · Supplementary Figure 7 · Supplementary Figure 7

Metal precursorsnot specified; stated to follow the same method as K3Fe2[PcFe-O8]
Linker precursorsPcFe-OH8-derived framework, by analogy to K3Fe2[PcFe-O8]
Solventsnot specified; same method as K3Fe2[PcFe-O8] implies NMP/H2O
AdditivesLi+ counterion source not named in official SI text
Atmospherenot specified; same method as K3Fe2[PcFe-O8]
ActivationSupercritical CO2 drying before N2 sorption; detailed activation for Li analogue not separately specified.