Synthesis · Spin crossover in Fe(triazole)-Pt nanoparticle self-assembly structured at the sub-5 nm scale

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

p005, journal p. 8184 · Experimental methods - Chemical syntheses

Metal precursorsFe(oTs)2.6H2O

Linker precursorsL ligand

SolventsTHF

AdditivesoTs = paratoluene sulfonate counterion

Temperatureroom temperature

Time2

Work-upVigorous stirring, then partial evaporation to light-yellow gel with 50 mass percent solvent remaining; further evaporation gives powder state.

ActivationNo activation; avoid THF evaporation for gel-state characterisation.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	L ligand in THF	10 mL · 6 x 10^-3 mol L^-1	p005, journal p. 8184 · Experimental methods - Chemical syntheses
Metal Source	Fe(oTs)2.6H2O in THF	10 mL · 2 x 10^-3 mol L^-1	p005, journal p. 8184 · Experimental methods - Chemical syntheses
Solvent	THF	Not specified	p005, journal p. 8184 · Experimental methods - Chemical syntheses

Complete recipeSource: Main

Route 2: Other

p005, journal p. 8184 · Experimental methods - Chemical syntheses

Linker precursors4-amino-4H-1,2,4-triazole; 3-acetylthiophene

Solventsethanol

Temperaturereflux

Timeovernight

Work-upPartial evaporation to give a white solid.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4-Amino-4H-1,2,4 triazole	2 g, 0.023 M	p005, journal p. 8184 · Experimental methods - Chemical syntheses
Linker	3-acetylthiophene	2.9 g, 0.023 M	p005, journal p. 8184 · Experimental methods - Chemical syntheses
Solvent	ethanol	50 mL	p005, journal p. 8184 · Experimental methods - Chemical syntheses

Complete recipeSource: Main

Route 3: Other

p006, journal p. 8185 · Experimental methods - Self-assembly

Metal precursorsnative PtNP mixture; Fe(oTs)2.6H2O

Linker precursorsL ligand

SolventsTHF

AdditivesoTs = tosylate counterion

Atmospherevigorous mixing; no explicit atmosphere stated for self-assembly step

Temperatureroom temperature

Time2

Work-upDrops deposited on characterisation substrates; remaining solution partially evaporated to gel with 50 mass percent solvent remaining; further evaporation to dark-brown powder.

ActivationNo activation; THF retention required for gel state.

Scalability contextExperiments repeated several times; conditions were optimised over a larger parameter study.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	L ligand in THF	1 mL · 6 x 10^-3 mol L^-1	p006, journal p. 8185 · Experimental methods - Self-assembly
Metal Source	Fe(oTs)2.6H2O in THF	1 mL · 2 x 10^-3 mol L^-1	p006, journal p. 8185 · Experimental methods - Self-assembly
Other	native NP mixture	4 mL	p006, journal p. 8185 · Experimental methods - Self-assembly
Solvent	THF	Not specified	p006, journal p. 8185 · Experimental methods - Self-assembly

Complete recipeSource: Main

Route 4: Other

p006, journal p. 8185 · Experimental methods - Platinum nanoparticles

Metal precursorsPt2(dba)3

Solventsfreshly distilled and deoxygenated THF; pentane wash

Atmosphereargon; 1 bar CO

Temperatureroom temperature

Time0.5

Oxidant / reductantCO atmosphere

Work-upEvaporated, washed with pentane 3 x 20 mL to eliminate dba, redissolved in 20 mL THF.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Pt2(dba)3	90 mg; 0.165 mmol of Pt	p006, journal p. 8185 · Experimental methods - Platinum nanoparticles
Solvent	freshly distilled and deoxygenated THF	20 mL	p006, journal p. 8185 · Experimental methods - Platinum nanoparticles
Reductant	CO	1 bar	p006, journal p. 8185 · Experimental methods - Platinum nanoparticles
Solvent	pentane	3 x 20 mL	p006, journal p. 8185 · Experimental methods - Platinum nanoparticles

Complete recipeSource: Main

Route 5: Drop Cast

p006-p007, journal pp. 8185-8186 · Experimental methods - Charge transport measurements

Solventscolloidal self-assembly solution

Temperatureroom temperature

Time0.0056

Substrate orientationinterdigitated comb electrodes

Work-upDroplet dried using absorbing paper after 20 seconds.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	PtNPs-FeL3 colloidal solution	10 uL	p006-p007, journal pp. 8185-8186 · Experimental methods - Charge transport measurements