Synthesis evidence

Crystal Structure and Electrochemical and Charge Transfer Properties in Redox-Active Coordination Polymers Based on a Truncated Tetrathiafulvalene Linker

Yang Z.-M., Li Y.-Y., Zhou X.-C. et al. · Crystal Growth and Design · 2022 · 4941-4947

2 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p002 / journal page 4942 · Experimental Section

Metal precursorsCd(NO3)2.6H2O (0.017 g, about 0.05 mmol)
Linker precursorsm-H4TTFTB (0.013 g, 0.019 mmol)
Solvents0.63 mL DMF and 0.21 mL CH2CH3OH for linker solution; 0.6 mL DMF and 0.6 mL H2O for Cd salt solution
Additivesnone reported
Atmospherenot specified
Temperature75
Time48
Oxidant / reductantnone reported
Work-upAllowed to cool to room temperature; red rod-like crystals filtered and washed with DMF three times.
Activationnone reported
Scalability contextSmall single-crystal solvothermal batch; isolated mass 0.010 g, 58% yield based on m-H4TTFTB.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.6H2O0.017 g, about 0.05 mmolp002 / journal page 4942 · Experimental Section
Linkerm-H4TTFTB0.013 g, 0.019 mmolp002 / journal page 4942 · Experimental Section
SolventDMF0.63 mL in linker solution; 0.6 mL in Cd solutionp002 / journal page 4942 · Experimental Section
SolventCH2CH3OH0.21 mLp002 / journal page 4942 · Experimental Section
SolventH2O0.6 mLp002 / journal page 4942 · Experimental Section
Complete recipeSource: Both

Route 2: Solvothermal

p002 / journal page 4942 · Experimental Section

Metal precursorsZn(NO3)2.6H2O (0.0074 g, about 0.025 mmol)
Linker precursorsm-H4TTFTB (0.005 g, 0.007 mmol)
Solvents1.2 mL DMF/H2O (v/v 1/1) for Zn salt; 1 mL DMF/CH2CH3OH (v/v 3/1) for linker
Additivesnone reported
Atmospheresealed in 15 mL pressure tubing; gas atmosphere not specified
Temperature75
Time24
Oxidant / reductantnone reported
Work-upCooled to room temperature; red rod-like crystals filtered and washed with DMF three times.
Activationnone reported
Scalability contextSmall single-crystal solvothermal batch; isolated mass 0.004 g, 62% yield based on m-H4TTFTB.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.0074 g, about 0.025 mmolp002 / journal page 4942 · Experimental Section
Linkerm-H4TTFTB0.005 g, 0.007 mmolp002 / journal page 4942 · Experimental Section
SolventDMF/H2O1.2 mL · v/v = 1/1p002 / journal page 4942 · Experimental Section
SolventDMF/CH2CH3OH1 mL · v/v = 3/1p002 / journal page 4942 · Experimental Section