cMOF Evidence Base

Synthesis evidence

Reaction-Type-Dependent Behavior of Redox-Hopping in MOFs─Does Charge Transport Have a Preferred Direction?

Yan M., Bowman Z., Knepp Z.J. et al. · Journal of Physical Chemistry Letters · 2024 · 11919-11926

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Electrochemical

p003 · Electrophoretic deposition of Ru-NU-1000

Metal precursorsRu-NU-1000 particles, 15 mg
Linker precursorsRu-NU-1000 framework particles
Solventstoluene, 25 mL; Alconox solution and DI water for cleaning
Additivesnone reported
Atmospherenot reported
Temperatureroom temperature implied; not explicitly reported
Time0.25 h + 0.25 h slide sonication; 3 h electrophoretic deposition
Substrate orientationTwo FTO slides 1 cm apart, conductive sides facing each other and submerged
Oxidant / reductant135 V constant potential applied between FTO slides
Work-upFTO slides sonicated in Alconox and DI water for 15 min each, washed, dried by airflow; Ru-NU-1000 suspension ultrasonicated and stirred at 320 rpm during deposition.
Activationnot reported after deposition
Scalability context6-dram vial EPD; no scale-up study reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherRu-NU-100015 mgp003 · Electrophoretic deposition of Ru-NU-1000
Solventtoluene25 mLp003 · Electrophoretic deposition of Ru-NU-1000
OtherFTO slidestwo slides · 1 cm spacedp003 · Electrophoretic deposition of Ru-NU-1000
AdditiveAlconox solutioncleaning solutionp003 · Electrophoretic deposition of Ru-NU-1000
SolventDI watercleaning solventp003 · Electrophoretic deposition of Ru-NU-1000
Complete recipeSource: SI

Route 2: Solvothermal

p001 · Synthesis of NU-1000

Metal precursorsZrOCl2.8H2O, 98 mg
Linker precursors1,3,6,8-tetrakis(p-benzoate)pyrene (H4TBAPy), 40 mg
SolventsDMF: 8 mL initially; 12 mL DMF during HCl treatment; acetone wash
Additivesbenzoic acid 2 g; trifluoroacetic acid 40 uL; 0.33 mL 12 M HCl
Atmospherenot reported
Temperature100; vacuum drying at 80
Time1 h preheat; 18 h after linker/TFA addition; 18 h HCl/DMF treatment; overnight drying
Work-upCentrifuge yellow precipitate; wash with fresh DMF three times with 1 h soaks; after HCl treatment wash with DMF and acetone, first two washes 1 h and third overnight; collect by centrifuge.
ActivationDried in vacuum oven at 80 C overnight.
Scalability contextUses 6-dram vial batch; no scale-up study reported.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrOCl2.8H2O98 mgp001 · Synthesis of NU-1000
Linker1,3,6,8-tetrakis(p-benzoate)pyrene (H4TBAPy)40 mgp001 · Synthesis of NU-1000
SolventN,N-dimethylformamide (DMF)8 mL initially; 12 mL for acid treatmentp001 · Synthesis of NU-1000
Additivebenzoic acid2 gp001 · Synthesis of NU-1000
Acidtrifluoroacetic acid (TFA)40 uLp001 · Synthesis of NU-1000
AcidHCl0.33 mL · 12 Mp001 · Synthesis of NU-1000
Solventacetone12 mL washesp001 · Synthesis of NU-1000
Complete recipeSource: SI

Route 3: Other

p001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2

Metal precursorsRu(bpy)2Cl2.2H2O, 291.38 mg
Linker precursors4-carboxy-2,2'-bipyridine (bpy-COOH), 112 mg; bpy ligands already present in Ru precursor
Solvents5 mL methanol + 5 mL water; DI water; saturated NH4PF6 aqueous solution
Additivesfew drops concentrated HCl; NH4PF6 for counterion exchange
Atmospherenot reported
Temperaturereflux; drying temperature not reported
Timereflux overnight; NH4PF6 exchange stirred overnight; vacuum drying overnight
Oxidant / reductantnone reported
Work-upFilter, rotary evaporate nearly dry, redissolve with acidic DI water, rotary evaporate to dry, ultrasonicate in saturated NH4PF6, stir overnight, filter, wash with cold DI water.
ActivationDried in vacuum oven overnight.
Scalability contextNo scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceRu(bpy)2Cl2.2H2O291.38 mgp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
Linker4-carboxy-2,2'-bypiridine (bpy-COOH)112 mgp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
Solventmethanol5 mLp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
Solventwater5 mLp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
Acidconcentrated HClfew dropsp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
AdditiveNH4PF6 aqueous solution~3.5 mL · saturatedp001 · Synthesis of [RuII(bpy)2(bpy-COOH)](PF6)2
Complete recipeSource: Both

Route 4: Other

p002 · Solvent-assistant ligand incorporation (SALI) of NU-1000

Metal precursors[RuII(bpy)2(bpy-COOH)](PF6)2, 108 mg
Linker precursorsNU-1000 powder, 30 mg; bpy-COOH ligand anchors Ru complex to NU-1000 nodes
SolventsDMF, 1.2 mL; acetone and diethyl ether washes
Additivesnone reported
Atmospherenot reported
Temperature100; vacuum drying at 80
Time7 days SALI; overnight drying
Oxidant / reductantnone reported
Work-upShake once per day; after cooling, wash with fresh DMF until supernatant colourless with 1 h soaks; wash with acetone three times and diethyl ether twice; collect by centrifuge.
ActivationDried in vacuum oven at 80 C overnight.
Scalability context1-dram vial, 30 mg NU-1000 batch; no scale-up study reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNU-100030 mgp002 · Solvent-assistant ligand incorporation (SALI) of NU-1000
Metal Source[RuII(bpy)2(bpy-COOH)](PF6)2108 mgp002 · Solvent-assistant ligand incorporation (SALI) of NU-1000
SolventDMF1.2 mLp002 · Solvent-assistant ligand incorporation (SALI) of NU-1000
Solventacetone3 washesp002 · Solvent-assistant ligand incorporation (SALI) of NU-1000
Solventdiethyl ether2 washesp002 · Solvent-assistant ligand incorporation (SALI) of NU-1000