Synthesis evidence

A Dual-Ligand Porous Coordination Polymer Chemiresistor with Modulated Conductivity and Porosity

Yao M.-S., Zheng J.-J., Wu A.-Q. et al. · Angewandte Chemie - International Edition · 2020 · 172-176

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: Other

1 · Fabrication of Cu3(HHTP)(THQ) nanowires

Metal precursorsCopper acetate (Cu(OAc)2.H2O), 11.450 mM, 22 mg in aqueous solution A
Linker precursorsHHTP, 1.085 mM, 3.5 mg; THQ, 2.610 mM, 4.5 mg in aqueous solution B
SolventsWater; acetone used in final washing
AdditivesEthylenediamine (en), 17.250 mM, 11.5 uL, used as Cu2+ chelating/base/template additive
AtmosphereSealed 10 mL test tube; no inert atmosphere specified
Temperature65 for 24 h, then 60 for 12 h; vacuum drying at 65 overnight
Time24 h primary reaction; 12 h secondary 60 deg C treatment; overnight drying
Work-upAfter 15 min ultrasonication/mixing, transferred to sealed test tube; 7.5 mL upper solution removed and replaced with 3.75 mL fresh solution A and 3.75 mL water; product washed five times with water by dispersion/centrifugation at 3500 rpm for 10 min; uniform nanowires collected by repeated dispersion/centrifugation in water at 2000 rpm for 3 min; filtered and washed with H2O (50 mL x 2) and acetone (25 mL x 2).
ActivationMaintained obtained solution at 60 deg C for 12 h; dried under vacuum at 65 deg C overnight.
Scalability contextBatch recipe uses 10 mL total initial solution in a 10 mL sealed test tube; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate (Cu(OAc)2.H2O)22 mg · 11.450 mM in 5 mL aqueous solution A1 · Fabrication of Cu3(HHTP)(THQ) nanowires
Baseethylenediamine (en)11.5 uL · 17.250 mM in 5 mL aqueous solution A1 · Fabrication of Cu3(HHTP)(THQ) nanowires
LinkerHHTP (2,3,6,7,10,11-hexahydrotriphenylene)3.5 mg · 1.085 mM in 5 mL aqueous solution B1 · Fabrication of Cu3(HHTP)(THQ) nanowires
LinkerTHQ (tetrahydroxy-1,4-quinone)4.5 mg · 2.610 mM in 5 mL aqueous solution B1 · Fabrication of Cu3(HHTP)(THQ) nanowires
Solventwater5 mL solution A + 5 mL solution B; later 3.75 mL added1 · Fabrication of Cu3(HHTP)(THQ) nanowires
Solventacetone25 mL x 2 wash1 · Fabrication of Cu3(HHTP)(THQ) nanowires
Partial recipeSource: Both

Route 2: Drop Cast

174 · Results and discussion · Figure 4

SolventsEthanol suspension of Cu3(HHTP)(THQ) nanowires
AtmosphereActivated under flowing dry air at room temperature
Temperatureroom temperature activation
Substrate orientationGlass substrate with precoated Au electrodes
Work-upCu3(HHTP)(THQ) nanowires ultrasonically dispersed in ethanol and drop-coated onto glass/Au electrodes.
ActivationFlowing dry air at room temperature
Scalability contextFilm thickness and nanowire loading are not reported.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)(THQ) nanowiresnot reported174 · Results and discussion · Figure 4
Solventethanolnot reported174 · Results and discussion · Figure 4