Synthesis · Insight into charge transportation in cadmium based semiconducting organic-inorganic hybrid materials and their application in the fabrication of photosensitive Schottky devices

6 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication

Metal precursorscomplex 1

SolventsN,N-dimethylformamide (DMF)

Atmosphereambient fabrication; main-text measurements in nitrogen-filled glove box

Temperature80 deg C drying after room-temperature spin coating

Time600 rpm for 5 min; 900 rpm for 5 min; dried several minutes

Substrate orientationITO-coated glass substrate; aluminium top electrode; shadow-mask active area 7.065 x 10^-2 cm^-2

Work-upFresh DMF dispersion (25 mg mL^-1) was spin-coated on ITO-coated glass, dried in a vacuum oven at 80 deg C, and capped with aluminium by vacuum coating.

Activationvacuum-oven drying at 80 deg C for several minutes to remove solvent

Scalability contextLaboratory spin-coated thin-film device; no scale-up discussed.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	complex 1	25 mg/ml dispersion · 25 mg/ml in DMF	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Solvent	N,N-dimethyl formamide (DMF)	not reported	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Other	ITO coated glass substrate	not reported	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Other	aluminium electrode	deposited by Vacuum Coating Unit	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication

Complete recipeSource: Both

Route 2: Other

SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication

Metal precursorscomplex 2

SolventsN,N-dimethylformamide (DMF)

Atmosphereambient fabrication; main-text measurements in nitrogen-filled glove box

Temperature80 deg C drying after room-temperature spin coating

Time600 rpm for 5 min; 900 rpm for 5 min; dried several minutes

Substrate orientationITO-coated glass substrate; aluminium top electrode; shadow-mask active area 7.065 x 10^-2 cm^-2

Work-upFresh DMF dispersion (25 mg mL^-1) was spin-coated on ITO-coated glass, dried in a vacuum oven at 80 deg C, and capped with aluminium by vacuum coating.

Activationvacuum-oven drying at 80 deg C for several minutes to remove solvent

Scalability contextLaboratory spin-coated thin-film device; no scale-up discussed.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	complex 2	25 mg/ml dispersion · 25 mg/ml in DMF	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Solvent	N,N-dimethyl formamide (DMF)	not reported	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Other	ITO coated glass substrate	not reported	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication
Other	aluminium electrode	deposited by Vacuum Coating Unit	SI PDF p2 and p11 / rendered p002 and p011 · Device fabrication

Complete recipeSource: Main

Route 3: Other

PDF p2 / article p5722 · Preparation of [(NCS)2Cd(H2L)]n (1)

Metal precursorscadmium(II) acetate dihydrate

Linker precursorsin situ H2L Schiff base ligand

Solventsmethanol: 20 cc ligand solution + 20 cc Cd solution + 10 cc NaSCN solution

Additivessodium thiocyanate

Atmospherenot reported

Temperature65 for ligand reflux; room temperature for metalation/crystallisation

Time2 h ligand reflux; 1 h stirring after NaSCN; 7 days crystallisation

Oxidant / reductantnone reported

Work-upFiltered solution mixture; kept in a beaker for crystallisation at room temperature; single crystals collected after seven days.

Activationnot reported

Scalability contextSolution crystallisation yielding 0.437 g (70%); no scale-up discussed.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2L	prepared from 4 mmol aldehyde and 2 mmol diamine	PDF p2 / article p5722 · Preparation of [(NCS)2Cd(H2L)]n (1)
Metal Source	cadmium(II) acetate dihydrate	2 mmol, 0.534 g · in methanol (20 cc)	PDF p2 / article p5722 · Preparation of [(NCS)2Cd(H2L)]n (1)
Additive	sodium thiocyanate	2 mmol, 0.162 g · in methanol (10 cc)	PDF p2 / article p5722 · Preparation of [(NCS)2Cd(H2L)]n (1)
Solvent	methanol	50 cc total reported	PDF p2 / article p5722 · Preparation of [(NCS)2Cd(H2L)]n (1)

Partial recipeSource: Main

Route 4: Other

PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)

Metal precursorscadmium(II) acetate dihydrate

Linker precursorsin situ H2L Schiff base ligand

Solventsmethanol with a few drops of DMF for crystallisation

Additivespotassium iodide

Atmospherenot reported

Temperature65 for ligand reflux; room temperature for metalation/crystallisation

Timesame as complex 1 for ligand and stirring except crystallisation time not reported for complex 2

Oxidant / reductantnone reported

Work-upFiltered solution mixture; a few drops of DMF were added; kept in a beaker for crystallisation at room temperature.

Activationnot reported

Scalability contextSolution crystallisation yielding 1.093 g (75%); no scale-up discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2L	prepared as for complex 1	PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)
Metal Source	cadmium(II) acetate dihydrate	2 mmol, 0.534 g inferred from similar procedure · in methanol (20 cc) inferred from similar procedure	PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)
Additive	potassium iodide	2 mmol, 0.332 g	PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)
Solvent	methanol	as for complex 1	PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)
Solvent	DMF	a few drops	PDF p2 / article p5722 · Preparation of [Cd(ICdL)2].DMF (2)

Partial recipeSource: Both

Route 5: Other

PDF p6-p7 / article p5726-p5727 · Electrical characterization · Fig. 7

Linker precursorsH2L ligand

Solventsnot separately reported for ligand control; complex-device route used DMF

Atmosphereambient during fabrication; measurement in nitrogen-filled glove box per main text

Temperatureroom temperature fabrication; 80 deg C drying inferred from complex-device route if same procedure used

Timenot separately reported for ligand control

Substrate orientationITO/ligand/Al control device

Work-upLigand device measured as ohmic control; separate fabrication recipe not detailed in SI.

Activationnot reported

Scalability contextSpin-coated thin-film control; no scale-up discussed.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	H2L ligand	not reported for ligand control	PDF p6-p7 / article p5726-p5727 · Electrical characterization · Fig. 7

Partial recipeSource: Main

Route 6: Other

PDF p2 / article p5722 · Preparation

Linker precursors2-hydroxy-3-ethoxybenzaldehyde; 2,2-dimethylpropane-1,3-diamine

Solventsmethanol (20 cc)

Atmospherenot reported

Temperature65

Time2

Work-upLigand solution used in situ for complex synthesis; ligand reported to crystallise from methanol in discussion.

Activationnot reported

Scalability contextSmall solution synthesis on 2 mmol diamine scale; no scale-up discussed.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2-hydroxy-3-ethoxybenzaldehyde	0.664 g, 4 mmol	PDF p2 / article p5722 · Preparation
Linker	2,2-dimethylpropane-1,3-diamine	0.24 cc, 2 mmol	PDF p2 / article p5722 · Preparation
Solvent	methanol	20 cc	PDF p2 / article p5722 · Preparation