Synthesis · Novel Topology in Semiconducting Tetrathiafulvalene Lanthanide Metal-Organic Frameworks

3 structured synthesis routes

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

Complete recipeSource: SI

S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)

Metal precursorsLu(NO3)3.xH2O, 7.5 mg, approximately 0.0168 mmol

Linker precursorsH4TTFTB, 11.5 mg, 0.0168 mmol

Solvents0.7 mL 1:1 H2O/EtOH for metal salt; 0.7 mL 3:1 DMF/EtOH for linker

AtmosphereCapped 2 mL vial; atmosphere not otherwise specified

Temperature50

Time72

Work-upWashed with 3 x 5 mL DMF and 3 x 5 mL EtOH, then collected by centrifugation.

ActivationFor N2 adsorption comparison, heated to 220 C under dynamic vacuum until outgas rate <2 mTorr/min.

Scalability contextSmall 2 mL vial synthesis; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Lu(NO3)3.xH2O	7.5 mg, ~0.0168 mmol	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Linker	H4TTFTB	11.5 mg, 0.0168 mmol	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Solvent	H2O/EtOH	0.7 mL, 1:1	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Solvent	DMF/EtOH	0.7 mL, 3:1	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)

Complete recipeSource: SI

S2 · Synthesis of Tm6(TTFTB)5

Metal precursorsTm(NO3)3.5H2O, 7.5 mg, 0.0168 mmol

Linker precursorsH4TTFTB, 11.5 mg, 0.0168 mmol

Solvents0.47 mL 1:1 H2O/EtOH for metal salt; 0.93 mL 3:1 DMF/EtOH for linker

AtmosphereCapped 2 mL vial; atmosphere not otherwise specified

Temperatureroom temperature

Time672

Work-upNo washing/workup reported for Tm crystal isolation; crystals described as product of slow room-temperature reaction.

Scalability contextTwenty-eight-day room-temperature crystallisation; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Tm(NO3)3.5H2O	7.5 mg, 0.0168 mmol	S2 · Synthesis of Tm6(TTFTB)5
Linker	H4TTFTB	11.5 mg, 0.0168 mmol	S2 · Synthesis of Tm6(TTFTB)5
Solvent	H2O/EtOH	0.47 mL, 1:1	S2 · Synthesis of Tm6(TTFTB)5
Solvent	DMF/EtOH	0.93 mL, 3:1	S2 · Synthesis of Tm6(TTFTB)5

Complete recipeSource: SI

S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)

Metal precursorsYb(NO3)3.5H2O, 7.5 mg, 0.0168 mmol

Linker precursorsH4TTFTB, 11.5 mg, 0.0168 mmol

Solvents0.7 mL 1:1 H2O/EtOH for metal salt; 0.7 mL 3:1 DMF/EtOH for linker

AtmosphereCapped 2 mL vial; atmosphere not otherwise specified

Temperature50

Time72

Work-upWashed with 3 x 5 mL DMF and 3 x 5 mL EtOH, then collected by centrifugation.

ActivationFor N2 adsorption, heated to 220 C under dynamic vacuum until outgas rate <2 mTorr/min.

Scalability contextSmall 2 mL vial synthesis; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Yb(NO3)3.5H2O	7.5 mg, 0.0168 mmol	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Linker	H4TTFTB	11.5 mg, 0.0168 mmol	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Solvent	H2O/EtOH	0.7 mL, 1:1	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)
Solvent	DMF/EtOH	0.7 mL, 3:1	S2 · Synthesis of Ln6(TTFTB)5 (Ln = Yb and Lu)