cMOF Evidence Base

Synthesis evidence

Redox-Active Mixed-Linker Metal–Organic Frameworks with Switchable Semiconductive Characteristics for Tailorable Chemiresistive Sensing

Zhou X.-C., Liu C., Su J. et al. · Angewandte Chemie - International Edition · 2023 · e202211850

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

4 · Experimental Procedures

Metal precursorsMn(NO3)2.4H2O (0.0059 g, 0.024 mmol)
Linker precursors[TTF] (0.0011 g, 0.0015 mmol); [NiS4] (0.0032 g, 0.0045 mmol)
Solvents1.25 mL H2O/EtOH (1/1 v/v); 0.13 mL DMF/EtOH (3/1 v/v)
Atmospherenot specified
Temperature80
Time24; cooled at 5 C h-1
Work-upblack needle crystals collected by filtration and washed with DMF and ethanol three times
Activationnone reported for synthesis; degassing conditions reported separately for sorption
Scalability context15 mL pressure tubing small-batch solvothermal crystallisation.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(NO3)2.4H2O0.0059 g, 0.024 mmol4 · Experimental Procedures
Linker[TTF]0.0011 g, 0.0015 mmol4 · Experimental Procedures
Linker[NiS4]0.0032 g, 0.0045 mmol4 · Experimental Procedures
SolventH2O/EtOH1.25 mL, v/v = 1/14 · Experimental Procedures
SolventDMF/EtOH0.13 mL, v/v = 3/14 · Experimental Procedures
Complete recipeSource: SI

Route 2: Solvothermal

4 · Experimental Procedures

Metal precursorsMn(NO3)2.4H2O (0.0059 g, 0.024 mmol)
Linker precursors[TTF] (0.0021 g, 0.003 mmol); [NiS4] (0.0022 g, 0.003 mmol)
Solvents1.25 mL H2O/EtOH (1/1 v/v); 0.13 mL DMF/EtOH (3/1 v/v)
Atmospherenot specified
Temperature80
Time24; cooled at 5 C h-1
Work-upblack needle crystals collected by filtration and washed with DMF and ethanol three times
Activationnone reported for synthesis; SQUEEZE used only for crystallographic solvent treatment
Scalability context15 mL pressure tubing small-batch solvothermal crystallisation.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(NO3)2.4H2O0.0059 g, 0.024 mmol4 · Experimental Procedures
Linker[TTF]0.0021 g, 0.003 mmol4 · Experimental Procedures
Linker[NiS4]0.0022 g, 0.003 mmol4 · Experimental Procedures
SolventH2O/EtOH1.25 mL, v/v = 1/14 · Experimental Procedures
SolventDMF/EtOH0.13 mL, v/v = 3/14 · Experimental Procedures
Complete recipeSource: SI

Route 3: Solvothermal

4 · Experimental Procedures

Metal precursorsMn(NO3)2.4H2O (0.0059 g, 0.024 mmol)
Linker precursors[TTF] (0.0031 g, 0.0045 mmol); [NiS4] (0.0011 g, 0.0015 mmol)
Solvents1.25 mL H2O/EtOH (1/1 v/v) for Mn source; 0.13 mL DMF/EtOH (3/1 v/v) for linkers
Atmospherenot specified
Temperature80
Time24; cooled at 5 C h-1
Work-upblack needle crystals collected by filtration and washed with DMF and ethanol three times
Activationnone reported for synthesis; degassing conditions reported separately for sorption
Scalability context15 mL pressure tubing small-batch solvothermal crystallisation.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(NO3)2.4H2O0.0059 g, 0.024 mmol4 · Experimental Procedures
Linker[TTF]0.0031 g, 0.0045 mmol4 · Experimental Procedures
Linker[NiS4]0.0011 g, 0.0015 mmol4 · Experimental Procedures
SolventH2O/EtOH1.25 mL, v/v = 1/14 · Experimental Procedures
SolventDMF/EtOH0.13 mL, v/v = 3/14 · Experimental Procedures
Complete recipeSource: Both

Route 4: Solvothermal

4 · Experimental Procedures

Metal precursorsMn(NO3)2.4H2O (0.0059 g, 0.024 mmol)
Linker precursors[TTF] (0.0031 g, 0.006 mmol), [NiS4] (0.0011 g, 0.006 mmol), or [TTF]/[NiS4] mixture with molar ratio 0.3, 1, or 3
Solvents1.25 mL H2O/EtOH (1/1 v/v); 0.13 mL DMF/EtOH (3/1 v/v)
Atmospherenot specified
Temperature60 then 80
Time1 h at 60 C, then 24 h at 80 C; cooled at 5 C h-1
Work-upblack needle crystals collected by filtration and washed with DMF and ethanol three times
Activationnone reported before device drop-casting; dispersed in EtOH for devices
Scalability contextLower reaction temperature gave microcrystalline samples with particle widths about 1 um suitable for thin-film devices.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(NO3)2.4H2O0.0059 g, 0.024 mmol4 · Experimental Procedures
Linker[TTF]0.0031 g, 0.006 mmol or mixture component4 · Experimental Procedures
Linker[NiS4]0.0011 g, 0.006 mmol or mixture component4 · Experimental Procedures
SolventH2O/EtOH1.25 mL, v/v = 1/14 · Experimental Procedures
SolventDMF/EtOH0.13 mL, v/v = 3/14 · Experimental Procedures