Synthesis · Cu3(hexaiminotriphenylene)2: An electrically conductive 2D metal-organic framework for chemiresistive sensing

4 structured synthesis routes

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

Vague recipeSource: SI

Route 1: Other

SI p.S5 · Discussion of Cu mixed-valency in Cu3(HITP)2 · Figs. S5-S6

Metal precursorsCuI.

Linker precursorsHATP.6HCl.

SolventsMeCN.

AdditivesEt3N.

AtmosphereAir.

Temperature23

Oxidant / reductantAerobic oxidation; Cu(I) precursor prevents Cu(II) serving as oxidant.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	Not specified	SI p.S5 · Discussion of Cu mixed-valency in Cu3(HITP)2 · Figs. S5-S6
Linker	HATP.6HCl	Not specified	SI p.S5 · Discussion of Cu mixed-valency in Cu3(HITP)2 · Figs. S5-S6
Base	Et3N	Not specified	SI p.S5 · Discussion of Cu mixed-valency in Cu3(HITP)2 · Figs. S5-S6
Solvent	MeCN	Not specified	SI p.S5 · Discussion of Cu mixed-valency in Cu3(HITP)2 · Figs. S5-S6

Partial recipeSource: Both

Route 2: Drop Cast

main p.2, article p.4350 · Results · Fig. 3; Fig. S7

Metal precursorsFreshly prepared Cu3(HITP)2 powder.

SolventsAcetone.

AtmosphereAmbient conditions not further specified.

Substrate orientationITO-coated glass slide.

Work-upDrop-cast from acetone suspension onto ITO glass; mechanically robust against ultrasonic washing according to main text.

Scalability contextSimple drop casting presented as potentially valuable for device manufacturing.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HITP)2	Not specified	main p.2, article p.4350 · Results · Fig. 3; Fig. S7
Solvent	acetone	Not specified	main p.2, article p.4350 · Results · Fig. 3; Fig. S7

Complete recipeSource: SI

Route 3: Drop Cast

SI p.S3 · Procedure for Gas Detection Measurements · Fig. S8

Metal precursorsFreshly prepared Cu3(HITP)2 powder.

SolventsAcetone.

AtmosphereAmbient deposition atmosphere not specified; sensing performed in controlled gas chamber.

Substrate orientationInterdigitated gold electrodes (CC1.W1 from BVT Technologies).

Work-upDrop-cast suspension; deposited amount monitored by resistance until 10-100 kOhm starting values were targeted.

Scalability contextDevice fabrication uses simple solution drop casting.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	freshly prepared Cu3(HITP)2	~1 mg/mL	SI p.S3 · Procedure for Gas Detection Measurements · Fig. S8
Solvent	acetone	Not specified	SI p.S3 · Procedure for Gas Detection Measurements · Fig. S8

Complete recipeSource: Both

Route 4: Other

SI p.S3 · Synthesis of Cu3(HITP)2

Metal precursorsCuSO4.5H2O (7.0 mg, 2.8e-2 mmol, 1.5 equiv)

Linker precursorsHATP.6HCl (10. mg, 1.9e-2 mmol, 1.0 equiv)

SolventsDistilled water (3 mL for linker solution; 2 mL for metal/base solution); acetone wash (15 mL).

AdditivesConcentrated aqueous ammonia (14 M; 100 uL).

AtmosphereUnder air; ambient atmosphere.

Temperature23

Time3 h standing reaction; 72 h water stirring/washing; 24 h acetone stirring.

Oxidant / reductantAir and redox-active HITP ligand environment; no separate oxidant/reductant specified.

Work-upImmediate dark precipitate; centrifuged and decanted; stirred with water at 23 deg C for three days with water exchanged twice daily; stirred with acetone for one day; isolated by centrifugation.

ActivationDried under vacuum (<=20 mTorr) at 23 deg C.

Scalability contextMilligram-scale recipe gives 7.2 mg product in 95% yield.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HATP.6HCl	10. mg, 1.9e-2 mmol, 1.0 equiv	SI p.S3 · Synthesis of Cu3(HITP)2
Metal Source	CuSO4.5H2O	7.0 mg, 2.8e-2 mmol, 1.5 equiv	SI p.S3 · Synthesis of Cu3(HITP)2
Base	concentrated aqueous ammonia	100 uL · 14 M	SI p.S3 · Synthesis of Cu3(HITP)2
Solvent	distilled water	3 mL + 2 mL; 15 mL water wash	SI p.S3 · Synthesis of Cu3(HITP)2
Solvent	acetone	15 mL	SI p.S3 · Synthesis of Cu3(HITP)2