Synthesis · Structural Control of Photoconductivity in a Flexible Titanium-Organic Framework

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: Other

6 · S.2.1 · Scheme S1

Work-upExtracted with CH2Cl2 (3 x 100 mL), washed with brine, dried over MgSO4, purified by silica gel chromatography (hexane:EtOAc 8:2) to yield compound I, 1.10 g, 69%.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2,5,8-Tribromobenzo[1,2-b:3,4-b':5,6-b'']trithiophene	1.0 g, 2.07 mmol	6 · S.2.1 · Scheme S1
Linker	tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate	2.81 g, 9.32 mmol	6 · S.2.1 · Scheme S1
Additive	tetrakis(triphenylphosphine)palladium(0)	414 mg, 0.36 mmol	6 · S.2.1 · Scheme S1
Base	K2CO3	5.5 g, 39.80 mmol	6 · S.2.1 · Scheme S1
Solvent	tetrahydrofuran	80 mL	6 · S.2.1 · Scheme S1
Solvent	water	20 mL	6 · S.2.1 · Scheme S1

Complete recipeSource: SI

Route 2: Other

6 · S.2.1 · Scheme S2

Work-upPrecipitate collected by filtration, washed with diethyl ether and methanol several times, and dried in vacuo; H3BTTTB 0.58 g, 90%.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	compound I	0.82 g, 1.06 mmol	6 · S.2.1 · Scheme S2
Solvent	dichloromethane	40.0 mL	6 · S.2.1 · Scheme S2
Acid	trifluoroacetic acid	4.0 mL	6 · S.2.1 · Scheme S2

Complete recipeSource: SI

Route 3: Drop Cast

34 · S.6.4 · Figure S27

Work-upManual contacting was used after e-beam lithography contacts were lost during lift-off.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MUV-35-c single crystals	Not specified	34 · S.6.4 · Figure S27
Other	Si/SiO2 substrate	285 nm SiO2	34 · S.6.4 · Figure S27
Other	silver paint contacts	Not specified	34 · S.6.4 · Figure S27

Complete recipeSource: Both

Route 4: Solvothermal

7 · S.2.2

Work-upYellow crystals recovered by sonication and rinsed with fresh DMF and acetone several times.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H3BTTTB	15 mg, 0.024 mmol	7 · S.2.2
Metal Source	MnCl2·4H2O	4 mg, 0.020 mmol	7 · S.2.2
Metal Source	titanium(IV) isopropoxide (Ti(OiPr)4)	10 μL, 32.5 μmol	7 · S.2.2
Solvent	N,N-dimethylformamide (DMF)	3.0 mL	7 · S.2.2
Acid	acetic acid (AcOH)	0.2 mL	7 · S.2.2