Synthesis · A comparative study of honeycomb-like 2D π-conjugated metal-organic framework chemiresistors: conductivity and channels

6 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

p008; article page 13242 · Preparation of Cu-HHTP NRs

Metal precursorscopper acetate (40 mg)

Linker precursorsHHTP (2,3,6,7,10,11-hexahydrotriphenylene, 32.5 mg)

Solvents14 mL water and 14 mL DMF

Atmospheresealed glass bottle; atmosphere not specified

Temperature65

Time24

Work-upcool to room temperature; collect bottom product; wash five times with fresh water and five times with methanol by ultrasonic dispersion and centrifugation at 13500 rpm for 10 min; methanol washing dispersion 1 h per cycle

Activationdried under vacuum at 80 deg C for 12 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	copper acetate	40 mg	p008; article page 13242 · Preparation of Cu-HHTP NRs
Linker	HHTP (2,3,6,7,10,11-hexahydrotriphenylene)	32.5 mg	p008; article page 13242 · Preparation of Cu-HHTP NRs
Solvent	water	14 mL	p008; article page 13242 · Preparation of Cu-HHTP NRs
Solvent	DMF	14 mL	p008; article page 13242 · Preparation of Cu-HHTP NRs

Complete recipeSource: Main

Route 2: Solvothermal

p008; article page 13242 · Preparation of Cu-HHTP NSs

Metal precursorscopper acetate (40 mg)

Linker precursorsHHTP (2,3,6,7,10,11-hexahydrotriphenylene, 32.5 mg)

Solvents28 mL EtOH

Atmospheresealed glass bottle; atmosphere not specified

Temperature65

Time24

Work-upcool to room temperature; collect products; wash five times with fresh water and five times with methanol by dispersion and centrifugation at 13500 rpm for 10 min

Activationdried under vacuum at 80 deg C for 12 h

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	copper acetate	40 mg	p008; article page 13242 · Preparation of Cu-HHTP NSs
Linker	HHTP (2,3,6,7,10,11-hexahydrotriphenylene)	32.5 mg	p008; article page 13242 · Preparation of Cu-HHTP NSs
Solvent	EtOH	28 mL	p008; article page 13242 · Preparation of Cu-HHTP NSs

Complete recipeSource: Main

Route 3: Solvothermal

p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires

Metal precursorscopper acetate (22 mg)

Linker precursorsHHTP (3.5 mg) and THQ (4.5 mg)

Solventswater

Additivesethylenediamine (en, 11.5 uL)

Atmospheresealed test tube; atmosphere not specified

Temperature65

Time24

Work-upultrasonically mix aqueous solutions for 15 min; transfer to 10 mL sealed test tube; remove 7.5 mL upper solution and replace with 3.75 mL fresh solution A and 3.75 mL water; after heating, collect black products from reactor bottom; wash five times with fresh water by dispersion and centrifugation at 3500 rpm for 10 min; collect uniform nanowires from upper solution by repeated dispersion and centrifugation with fresh water at 2000 rpm for 3 min; maintain solution at 60 deg C for 12 h; filter; wash with H2O (50 mL x 2) and acetone (25 mL x 2)

Activationdried under vacuum at 65 deg C overnight

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	copper acetate	22 mg	p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires
Additive	ethylenediamine (en)	11.5 uL	p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires
Linker	HHTP (2,3,6,7,10,11-hexahydrotriphenylene)	3.5 mg	p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires
Linker	THQ (tetrahydroxy-1,4-quinone)	4.5 mg	p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires
Solvent	water	initial 10 mL aqueous solutions plus replacement water	p008; article page 13242 · Fabrication of Cu-HHTP-THQ nanowires

Complete recipeSource: Main

Route 4: Other

p008; article page 13242 · Preparation of Cu-HITP powders

Metal precursorsCuSO4.5H2O (22.7 mg, 0.028 mM)

Linker precursorsHATP.6HCl (10 mg, 0.019 mM)

SolventsDI water, 2 mL for metal/base solution and 2 mL for ligand solution

AdditivesNH3.H2O (0.075 mL)

Atmosphereroom-temperature stirring; atmosphere not specified

Temperatureroom temperature

Time3

Oxidant / reductantair/oxidation state not controlled in procedure; authors note porosity depends on ligand status and degree of oxidization

Work-upcollect products and wash five times with methanol

Activationdried under vacuum at 65 deg C overnight

Scalability contextPorosity varied batch-to-batch even using the same synthetic procedure.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuSO4.5H2O	22.7 mg (0.028 mM)	p008; article page 13242 · Preparation of Cu-HITP powders
Base	NH3.H2O	0.075 mL	p008; article page 13242 · Preparation of Cu-HITP powders
Linker	HATP.6HCl	10 mg (0.019 mM)	p008; article page 13242 · Preparation of Cu-HITP powders
Solvent	DI water	4 mL total	p008; article page 13242 · Preparation of Cu-HITP powders

Complete recipeSource: Main

Route 5: Solvothermal

p008-p009; article pages 13242-13243 · Preparation of Cu-THQ

Metal precursorsCu(NO3)2.3H2O (53.2 mg)

Linker precursorsTHQ (30 mg)

Solventssolution A: water 7.5 mL, methanol 2.5 mL; solution B: water 7.5 mL, methanol 2.5 mL

Additivesethylenediamine (en, 11.5 uL)

Atmospheresealed glass bottle; atmosphere not specified

Temperature80

Time14

Work-upultrasonically mix solutions for 15 min; transfer to 50 mL sealed glass bottle; cool to room temperature; collect black products from bottom; wash three times with water by dispersion and centrifugation at 3500 rpm for 10 min; collect upper Cu-THQ solution repeatedly by dispersion and centrifugation with fresh water at 3500 rpm for 3 min; maintain obtained solution at 60 deg C for 12 h; filter; wash with H2O (50 mL x 2) and acetone (25 mL x 2)

Activationdried under vacuum at 65 deg C overnight

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	53.2 mg	p008-p009; article pages 13242-13243 · Preparation of Cu-THQ
Additive	ethylenediamine (en)	11.5 uL	p008-p009; article pages 13242-13243 · Preparation of Cu-THQ
Linker	THQ	30 mg	p008-p009; article pages 13242-13243 · Preparation of Cu-THQ
Solvent	water	15 mL total in solutions A and B	p008-p009; article pages 13242-13243 · Preparation of Cu-THQ
Solvent	methanol	5 mL total in solutions A and B	p008-p009; article pages 13242-13243 · Preparation of Cu-THQ

Complete recipeSource: Main

Route 6: Drop Cast

p005 and p009; article pages 13239 and 13243 · Results and discussion; Gas sensor characterization · Fig. 5

Solventsmethanol suspension of cMOF powders

Atmosphereflowing dry air during activation/aging

Temperature65 activation; about 25 measurement baseline

Time3 activation/aging

Substrate orientationAl2O3 substrate with precoated Ag-Pd interdigital electrodes

Work-upultrasonically disperse cMOF in methanol; drop-coat suspension onto electrode substrate

Activationactivated and aged under 5 V and flowing dry air at 65 deg C for 3 h, then cooled to about 25 deg C

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Solvent	methanol	not reported	p005 and p009; article pages 13239 and 13243 · Results and discussion; Gas sensor characterization · Fig. 5
Other	cMOF powder	not reported	p005 and p009; article pages 13239 and 13243 · Results and discussion; Gas sensor characterization · Fig. 5
Other	Al2O3 substrate with Ag-Pd interdigital electrodes	not reported	p005 and p009; article pages 13239 and 13243 · Results and discussion; Gas sensor characterization · Fig. 5