Complete recipeSource: Main
Route 1: Hydrothermal
6 · Methods; Preparation of {[Cu2(6-Hmna)(6-mn)].NH4}n (1) · Fig. 1
Metal precursorsCu(NO3)2.6H2O (46.1 mg, 0.20 mmol)
Linker precursors6,6'-dithiodinicotinic acid (H2dtdn, 30.8 mg, 0.10 mmol)
SolventsDMF/H2O (5:1 v/v)
Additivespyrazine (13.3 mg, 0.20 mmol)
AtmosphereNot specified; hydrothermal conditions.
Temperature140
Time72 h reaction followed by 72 h slow cooling
Oxidant / reductantIn situ S-S bond cleavage; nitrate reduction proposed to generate NH4+ in presence of DMF and pyrazine.
Work-upBrown rod-shaped crystals isolated on a filter, washed with water, then DMF, and dried at room temperature.
ActivationNo activation for synthesis; separate TGA sample had surface water removed in a desiccator with activated molecular sieves.
Scalability contextYield 51.0% (15.9 mg, 0.035 mmol based on copper salt); authors describe the procedure as straightforward and simple.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Cu(NO3)2.6H2O | 46.1 mg, 0.20 mmol | 6 · Methods; Preparation of {[Cu2(6-Hmna)(6-mn)].NH4}n (1) · Fig. 1 |
| Linker | 6,6'-dithiodinicotinic acid (H2dtdn) | 30.8 mg, 0.10 mmol | 6 · Methods; Preparation of {[Cu2(6-Hmna)(6-mn)].NH4}n (1) · Fig. 1 |
| Additive | pyrazine | 13.3 mg, 0.20 mmol | 6 · Methods; Preparation of {[Cu2(6-Hmna)(6-mn)].NH4}n (1) · Fig. 1 |
| Solvent | DMF/H2O | 5:1 v/v solution | 6 · Methods; Preparation of {[Cu2(6-Hmna)(6-mn)].NH4}n (1) · Fig. 1 |