Synthesis evidence

Metal-Organic Framework Photoconductivity via Time-Resolved Terahertz Spectroscopy

Pattengale B., Neu J., Ostresh S. et al. · Journal of the American Chemical Society · 2019 · 9793-9797

4 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

S2 · Synthesis and Characterization of Zn2TTFTB

Metal precursors159.5 mg Zn(NO3)2.6H2O
Linker precursors100 mg H4TTFTB
SolventsDimethylformamide and ethanol
AtmosphereEvacuated and N2-filled three times on a Schlenk line
Temperature75
Time48
Work-upDark precipitate collected by vacuum filtration and washed three times with dimethylformamide followed by ethanol.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH4TTFTB100 mgS2 · Synthesis and Characterization of Zn2TTFTB
Solventdimethylformamide12 mL in ligand solution; 8 mL in metal solutionS2 · Synthesis and Characterization of Zn2TTFTB
Solventethanol4 mL added to ligand solution; 8 mL in metal solutionS2 · Synthesis and Characterization of Zn2TTFTB
Metal SourceZn(NO3)2.6H2O159.5 mgS2 · Synthesis and Characterization of Zn2TTFTB
Partial recipeSource: Both

Route 2: Other

p002 / 9794 · main text · Figures S4-S5

Work-upAs-prepared tape cell pressed with 11 kbar hydraulic pressure.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherAs-prepared Zn2TTFTB tape cellNot specifiedp002 / 9794 · main text · Figures S4-S5
Vague recipeSource: Both

Route 3: Other

S8 · Supplementary Figures · Figure S6

AdditivesPTFE matrix
Work-upZn2TTFTB/PTFE pellet pressed at 11 kbar.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn2TTFTBNot specifiedS8 · Supplementary Figures · Figure S6
AdditivePTFENot specifiedS8 · Supplementary Figures · Figure S6
Complete recipeSource: SI

Route 4: Other

S2 · Tape Cell Preparation

SolventsIsopropanol used to wipe outside of cell
AdditivesAcrylic tape and paper business card
AtmosphereAmbient sample preparation
Work-upMOF powder packed into 7 mm punched hole, lightly scraped, repeated three times, sealed with second acrylic tape layer, trimmed and wiped clean.
Scalability contextDesigned to study delicate powder samples without pressing pellets or sintering.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherAs-synthesised Zn2TTFTB powderAdded to fill 7 mm punched holeS2 · Tape Cell Preparation
Otherpaper business card0.35 +/- 0.01 mm thickness; 7 mm punched holeS2 · Tape Cell Preparation
OtherIntertape Polymer Group model 291 acrylic tape2.5 mil = 63.5 um thickness; two piecesS2 · Tape Cell Preparation
SolventisopropanolUsed to wipe clean outside of cellS2 · Tape Cell Preparation