Synthesis · Mn2(2,5-disulfhydrylbenzene-1,4-dicarboxylate): A microporous metal-organic framework with infinite (-Mn-S-)∞ chains and high intrinsic charge mobility

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

main pp.8185-8186 · Main text, synthesis

Metal precursorsanhydrous MnCl2

Linker precursorsH4DSBDC

Solventsdry degassed DMF/methanol, 10:1 by volume

Atmospherenitrogen

Temperature120

Time24

Work-upGenerated yellow crystals and unidentified orange powder; no detailed isolation in main text.

Scalability contextInitial conditions gave mixed yellow crystals and orange powder.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	anhydrous MnCl2	Not specified	main pp.8185-8186 · Main text, synthesis
Linker	H4DSBDC	Not specified	main pp.8185-8186 · Main text, synthesis
Solvent	N,N-dimethylformamide (DMF)	DMF/methanol 10:1 by volume	main pp.8185-8186 · Main text, synthesis
Solvent	methanol	DMF/methanol 10:1 by volume	main pp.8185-8186 · Main text, synthesis

Complete recipeSource: Both

Route 2: Solvothermal

SI p.S5 · Bulk synthesis

Metal precursorsanhydrous MnCl2 (337 mg, 2.62 mmol)

Linker precursorsH4DSBDC (120 mg, 0.53 mmol)

Solventsdry and deaerated DMF (14 mL) and methanol (7 mL), 2:1

Atmospherenitrogen during bulk synthesis; glovebox collection after methanol exchange; dynamic vacuum for activation

Temperature125 for synthesis; 150 for activation

Time24 for synthesis; 48 h Soxhlet exchange; 32 h activation

Work-upVacuum filtration, washed with 10 mL methanol, Soxhlet reflux with dry deaerated methanol for 2 days, collected in glovebox.

ActivationCompletely desolvated under dynamic vacuum (<10 umHg) at 150 deg C for 32 h to yield activated 1; main text reports 150 deg C under 3 mTorr for 2 days.

Scalability contextBulk synthesis gave 71 mg activated 1 (0.21 mmol, 40%) yellow powder.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Anhydrous MnCl2	337 mg, 2.62 mmol	SI p.S5 · Bulk synthesis
Linker	H4DSBDC	120 mg, 0.53 mmol	SI p.S5 · Bulk synthesis
Solvent	dry and deaerated DMF	14 mL	SI p.S5 · Bulk synthesis
Solvent	methanol	7 mL plus 10 mL wash and Soxhlet solvent	SI p.S5 · Bulk synthesis

Complete recipeSource: SI

Route 3: Solvothermal

SI p.S5 · Crystal growth

Metal precursorsMnCl2.4H2O (52 mg, 0.26 mmol)

Linker precursorsH4DSBDC (12 mg, 0.05 mmol)

Solventsdry and deaerated DMF (2 mL)

AtmosphereEvacuated sealed Pyrex tube after freeze-pump-thaw cycles

Temperature120

Time48

Work-upYellow crystals and orange powder formed; yellow single crystal selected for X-ray crystallography.

Scalability contextCrystal-growth recipe intentionally produced diffraction-quality crystals, not bulk pure phase.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	MnCl2.4H2O	52 mg, 0.26 mmol	SI p.S5 · Crystal growth
Linker	H4DSBDC	12 mg, 0.05 mmol	SI p.S5 · Crystal growth
Solvent	dry and deaerated DMF	2 mL	SI p.S5 · Crystal growth