Synthesis · Colossal Increase in Electric Current and High Rectification Ratio in a Photoconducting, Self-Cleaning, and Luminescent Schottky Barrier NMOF Diode

6 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure S21

Metal precursorsAl rectifier metal contact; ITO substrate

Linker precursorsH2OPE-C12 material

Solventsethanol medium for dispersion; soap solution, acetone, ethanol and distilled water for ITO cleaning

Additivesnone reported

Atmospherenot reported; thermal evaporation for Al contact

Temperatureroom temperature for coating; Al deposited by thermal evaporation

Timespin coating for 2 min

Substrate orientationITO-coated glass; Al top contact through shadow mask

Oxidant / reductantnone

Work-upsame spin-coating and Al evaporation procedure as NMOF-1 SBD device

Activationnot reported

Scalability contexteffective diode area 7.065 x 10^-6 m2 maintained by shadow mask

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2OPE-C12	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure S21
Solvent	ethanol	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure S21
Other	ITO coated glass substrate	Not specified	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure S21
Other	Aluminium rectifier metal contact	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure S21

Partial recipeSource: SI

Route 2: Other

9 · Synthetic Procedure; Synthesis of Ligand · Scheme S1

Metal precursorsnone

Linker precursors4-iodobenzoic acid derivative and dialkoxy-substituted hydroquinone intermediates shown in Scheme S1

Solventsmethanol; acetonitrile; THF; THF-MeOH (from Scheme S1)

AdditivesAcCl; Pd(PPh3)2Cl2; Pd(PPh3)4; NEt3; Cu2I2; K2CO3; ICl; KOH

Atmospherenot reported

Temperature25, 60 and 70 C steps shown in Scheme S1

Time6, 12, 36 and 48 h steps shown in Scheme S1

Oxidant / reductantnot specified

Work-upnot reported in this SI; authors cite reported Sonogashira-Hagihara procedure

Activationnot reported

Scalability contextnot reported

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2OPE-C12 ligand precursor route in Scheme S1	Not specified	9 · Synthetic Procedure; Synthesis of Ligand · Scheme S1
Solvent	Methanol; MeCN; THF; THF-MeOH	Not specified	9 · Synthetic Procedure; Synthesis of Ligand · Scheme S1
Additive	Pd(PPh3)4; Pd(PPh3)2Cl2; NEt3; Cu2I2; K2CO3; ICl; KOH; AcCl	Not specified	9 · Synthetic Procedure; Synthesis of Ligand · Scheme S1

Complete recipeSource: Both

Route 3: Other

9-10 · Synthetic Procedure; Synthesis of NMOF-1 · Scheme S2

Metal precursorsZn(OAc)2.2H2O (11 mg, 0.07 mmol)

Linker precursorsH2OPE-C12 (30 mg, 0.035 mmol)

Solvents1:1 DMF/H2O mixture (10 mL)

Additivestriethylamine (100 uL)

Atmospherenot reported; room-temperature open solution implied

Temperatureroom temperature

Time6 h total after triethylamine addition; mixture stirred 15 min before base addition

Oxidant / reductantnone reported

Work-upreaction stopped; precipitate centrifuged and washed well with THF and water

Activationnone for synthesis; adsorption samples activated separately at 170 C under 1 x 10^-1 Pa vacuum for about 12 h

Scalability contextsolution-processable dispersion enabled coating on large glass areas, but scale-up not quantified

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2OPE-C12	30 mg, 0.035 mmol	9-10 · Synthetic Procedure; Synthesis of NMOF-1 · Scheme S2
Metal Source	Zn(OAc)2.2H2O	11 mg, 0.07 mmol	9-10 · Synthetic Procedure; Synthesis of NMOF-1 · Scheme S2
Solvent	1:1 DMF/H2O	10 mL	9-10 · Synthetic Procedure; Synthesis of NMOF-1 · Scheme S2
Base	triethylamine	100 uL	9-10 · Synthetic Procedure; Synthesis of NMOF-1 · Scheme S2

Partial recipeSource: Main

Route 4: Drop Cast

2 · Results and Discussion · Figures 1g and 2a

Metal precursorsNMOF-1 dispersion/solution

Linker precursorsnot applicable

Solventsnot specified for drop-casting; THF dispersion discussed elsewhere

Additivesnone reported

Atmosphereambient implied

Temperatureroom temperature implied

Timenot reported

Substrate orientationglass substrate

Oxidant / reductantnone

Work-upformed thin film on glass substrate

Activationnot reported

Scalability contextauthors state coating could be applied to large areas of glass by simple drop-casting

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NMOF-1 dispersion/solution	not reported	2 · Results and Discussion · Figures 1g and 2a
Other	glass substrate	Not specified	2 · Results and Discussion · Figures 1g and 2a

Partial recipeSource: SI

Route 5: Other

5 · Conductivity Measurements of NMOF-1 and H2OPE-C12 · Scheme S4

Metal precursorsNMOF-1 material

Linker precursorsnot applicable

Solventsnot specified for conductivity film

Additivesnone reported

Atmosphereopen atmosphere for measurement

Temperatureroom temperature

Timespin coating for 2 min

Substrate orientationglass substrate; two parallel ohmic electrodes

Oxidant / reductantnone

Work-upspin-coated at 1200 rpm for 2 min and dried; electrodes connected for two-probe measurement

Activationnot reported

Scalability contextnot reported

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NMOF-1 material	not reported	5 · Conductivity Measurements of NMOF-1 and H2OPE-C12 · Scheme S4
Other	glass substrate	Not specified	5 · Conductivity Measurements of NMOF-1 and H2OPE-C12 · Scheme S4

Partial recipeSource: SI

Route 6: Other

6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure 2d

Metal precursorsNMOF-1 material; Al rectifier metal contact; ITO substrate

Linker precursorsnot applicable

Solventsethanol medium for dispersion; soap solution, acetone, ethanol and distilled water for ITO cleaning

Additivesnone reported

Atmospherenot reported; thermal evaporation for Al contact

Temperatureroom temperature for coating; Al deposited by thermal evaporation

Timespin coating for 2 min

Substrate orientationITO-coated glass; Al top contact through shadow mask

Oxidant / reductantnone

Work-upITO cleaned sequentially in ultrasonic bath; material ultrasonicated in ethanol; spin coated at 1200 rpm for 2 min and dried; Al deposited by thermal evaporation

Activationnot reported

Scalability contexteffective diode area 7.065 x 10^-6 m2 maintained by shadow mask

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NMOF-1	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure 2d
Solvent	ethanol	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure 2d
Other	ITO coated glass substrate	Not specified	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure 2d
Other	Aluminium rectifier metal contact	not reported	6 · Fabrication of ITO/NMOF-1/Al and ITO/H2OPE-C12/AlSchottky diode · Figure 2d