Synthesis · Structures and electrical conductivities of a series of coordination polymers based on tetrathiafulvalene

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

2 · 2.2 Synthesis of [Co(H2TTFTB)(H2O)4DMF] (1)

Metal precursorsCo(OTf)2 (40 mg, 0.11 mmol)

Linker precursorsH4TTFTB (20 mg, 0.03 mmol), prepared by previously reported method [32]

SolventsDMF, EtOH and H2O (v/v/v 2/2/1); solvent volumes not reported

Atmospherenot reported

Temperature60

Time72

Work-upMixture sonicated and heated; filtrate evaporated in a beaker under ambient conditions for about one week to afford block-shaped red crystals

Activationnot reported

Scalability contextYield 30% based on H4TTFTB; no scale-up data reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OTf)2	40 mg, 0.11 mmol	2 · 2.2 Synthesis of [Co(H2TTFTB)(H2O)4DMF] (1)
Linker	H4TTFTB	20 mg, 0.03 mmol	2 · 2.2 Synthesis of [Co(H2TTFTB)(H2O)4DMF] (1)
Solvent	DMF, EtOH and H2O	v/v/v 2/2/1; volumes not reported	2 · 2.2 Synthesis of [Co(H2TTFTB)(H2O)4DMF] (1)

Partial recipeSource: Main

Route 2: Solvothermal

2 · 2.3 Synthesis of [Co6(HTTFTB)4(H2O)] (2)

Metal precursorsCoCl2.6H2O (35 mg, 0.15 mmol)

Linker precursorsH4TTFTB (10 mg, 0.015 mmol)

SolventsDMF and EtOH (v/v 3/2); solvent volumes not reported

AdditivesCH3COOH (590 uL)

Atmospherenot reported

Temperature120

Time72

Work-upMixture sonicated, sealed in a 25 mL Teflon-lined stainless-steel vessel, heated, cooled at 5 deg C/h to room temperature, and filtered to obtain dark needle-shaped crystals

Activationnot reported

Scalability contextYield 40% based on H4TTFTB; no scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CoCl2.6H2O	35 mg, 0.15 mmol	2 · 2.3 Synthesis of [Co6(HTTFTB)4(H2O)] (2)
Linker	H4TTFTB	10 mg, 0.015 mmol	2 · 2.3 Synthesis of [Co6(HTTFTB)4(H2O)] (2)
Solvent	DMF and EtOH	v/v 3/2; volumes not reported	2 · 2.3 Synthesis of [Co6(HTTFTB)4(H2O)] (2)
Acid	CH3COOH	590 uL	2 · 2.3 Synthesis of [Co6(HTTFTB)4(H2O)] (2)

Partial recipeSource: Main

Route 3: Solvothermal

2 · 2.4 Synthesis of [Mn4(TTFTB)4(H2O)7DMF] (3)

Metal precursorsMn(NO3)2.6H2O (40 mg, 0.16 mmol)

Linker precursorsH4TTFTB (20 mg, 0.03 mmol)

SolventsDMF, EtOH and H2O (v/v/v 2/2/1); solvent volumes not reported

Atmospherenot reported

Temperature60

Time72

Work-upMixture sonicated and heated; dark needle-shaped crystals obtained by filtration

Activationnot reported

Scalability contextYield 40% based on H4TTFTB; no scale-up data reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Mn(NO3)2.6H2O	40 mg, 0.16 mmol	2 · 2.4 Synthesis of [Mn4(TTFTB)4(H2O)7DMF] (3)
Linker	H4TTFTB	20 mg, 0.03 mmol	2 · 2.4 Synthesis of [Mn4(TTFTB)4(H2O)7DMF] (3)
Solvent	DMF, EtOH and H2O	v/v/v 2/2/1; volumes not reported	2 · 2.4 Synthesis of [Mn4(TTFTB)4(H2O)7DMF] (3)