Synthesis · Dye-sensitized solar cells with new one-dimensional halide-bridged Cu(I)-Ni(II) heterometal coordination polymers containing hexamethylene dithiocarbamate ligand

12 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

p003 (journal p1615) · 2.2. Synthesis of 1a

Metal precursorsCuBr.S(CH3)2 (0.041 g, 0.2 mmol); Ni(Hm-dtc)2 (0.041 g, 0.10 mmol)

Linker precursorsHm-dtc supplied within preformed Ni(Hm-dtc)2

Solventsacetonitrile (10 mL), acetone (10 mL), CHCl3 (20 mL)

Atmospherenot specified; likely ambient

Temperaturenot specified

Time5 min stirring; crystals obtained in several days

Oxidant / reductantCu(I) source CuBr.S(CH3)2; no separate oxidant/reductant reported

Work-upReaction mixture stirred for 5 min, filtered; crystals grew from filtrate over several days.

Activationnone reported

Scalability contextSmall-scale solution crystallisation; no scalability discussion.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuBr.S(CH3)2	0.041 g; 0.2 mmol	p003 (journal p1615) · 2.2. Synthesis of 1a
Metal Source	Ni(Hm-dtc)2	0.041 g; 0.10 mmol	p003 (journal p1615) · 2.2. Synthesis of 1a
Linker	Hm-dtc in Ni(Hm-dtc)2	contained in 0.041 g Ni(Hm-dtc)2	p003 (journal p1615) · 2.2. Synthesis of 1a
Solvent	acetonitrile	10 mL	p003 (journal p1615) · 2.2. Synthesis of 1a
Solvent	acetone	10 mL	p003 (journal p1615) · 2.2. Synthesis of 1a
Solvent	CHCl3	20 mL	p003 (journal p1615) · 2.2. Synthesis of 1a

Complete recipeSource: SI

Route 2: Other

p002 · Supporting Information · Figure S3

Metal precursorscoordination polymer 1a

Linker precursorsalready present in coordination polymer

Solventsnone reported

AdditivesKBr powder matrix

Atmospherenot specified

Temperatureambient/not specified

Time5 min grinding

Substrate orientation13 mm pellet maker

Work-upGround with KBr powder in a mortar for 5 min, then pressed in a pellet maker of diameter 13 mm.

Activationnone reported

Scalability contextAnalytical pellet preparation only; no scale-up discussion.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 1a	0.5 umol	p002 · Supporting Information · Figure S3
Additive	KBr powder	50 mg	p002 · Supporting Information · Figure S3

Partial recipeSource: Main

Route 3: Other

p003 (journal p1615) · 2.3. Synthesis of 1b

Metal precursorsCuI (0.038 g, 0.2 mmol); Ni(Hm-dtc)2 (0.041 g, 0.10 mmol)

Linker precursorsHm-dtc supplied within preformed Ni(Hm-dtc)2

Solventsacetonitrile (10 mL), acetone (10 mL), CHCl3 (20 mL)

Atmospherenot specified; likely ambient

Temperaturenot specified

Time5 min stirring; crystals obtained in several days

Oxidant / reductantCu(I) source CuI; no separate oxidant/reductant reported

Work-upReaction mixture stirred for 5 min, filtered; crystals grew from filtrate over several days.

Activationnone reported

Scalability contextSmall-scale solution crystallisation; no scalability discussion.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.038 g; 0.2 mmol	p003 (journal p1615) · 2.3. Synthesis of 1b
Metal Source	Ni(Hm-dtc)2	0.041 g; 0.10 mmol	p003 (journal p1615) · 2.3. Synthesis of 1b
Linker	Hm-dtc in Ni(Hm-dtc)2	contained in 0.041 g Ni(Hm-dtc)2	p003 (journal p1615) · 2.3. Synthesis of 1b
Solvent	acetonitrile	10 mL	p003 (journal p1615) · 2.3. Synthesis of 1b
Solvent	acetone	10 mL	p003 (journal p1615) · 2.3. Synthesis of 1b
Solvent	CHCl3	20 mL	p003 (journal p1615) · 2.3. Synthesis of 1b

Complete recipeSource: SI

Route 4: Other

p002 · Supporting Information · Figure S3

Metal precursorscoordination polymer 1b

Linker precursorsalready present in coordination polymer

Solventsnone reported

AdditivesKBr powder matrix

Atmospherenot specified

Temperatureambient/not specified

Time5 min grinding

Substrate orientation13 mm pellet maker

Work-upGround with KBr powder in a mortar for 5 min, then pressed in a pellet maker of diameter 13 mm.

Activationnone reported

Scalability contextAnalytical pellet preparation only; no scale-up discussion.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 1b	0.5 umol	p002 · Supporting Information · Figure S3
Additive	KBr powder	50 mg	p002 · Supporting Information · Figure S3

Complete recipeSource: SI

Route 5: Other

p002 · Supporting Information · Figure S3

Metal precursorscoordination polymer 2a

Linker precursorsalready present in coordination polymer

Solventsnone reported

AdditivesKBr powder matrix

Atmospherenot specified

Temperatureambient/not specified

Time5 min grinding

Substrate orientation13 mm pellet maker

Work-upGround with KBr powder in a mortar for 5 min, then pressed in a pellet maker of diameter 13 mm.

Activationnone reported

Scalability contextAnalytical pellet preparation only; no scale-up discussion.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 2a	0.5 umol	p002 · Supporting Information · Figure S3
Additive	KBr powder	50 mg	p002 · Supporting Information · Figure S3

Complete recipeSource: SI

Route 6: Other

p002 · Supporting Information · Figure S3

Metal precursorscoordination polymer 2b

Linker precursorsalready present in coordination polymer

Solventsnone reported

AdditivesKBr powder matrix

Atmospherenot specified

Temperatureambient/not specified

Time5 min grinding

Substrate orientation13 mm pellet maker

Work-upGround with KBr powder in a mortar for 5 min, then pressed in a pellet maker of diameter 13 mm.

Activationnone reported

Scalability contextAnalytical pellet preparation only; no scale-up discussion.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 2b	0.5 umol	p002 · Supporting Information · Figure S3
Additive	KBr powder	50 mg	p002 · Supporting Information · Figure S3

Partial recipeSource: Main

Route 7: Other

p004 (journal p1616) · 2.5. Fabrication of DSSCs

Metal precursorscoordination polymer 1a; TiO2 paste PECC-K01; PEDOT-TMA counter-electrode material

Linker precursorscoordination polymer ligand already present in sensitizer

Solventsethanol for PEDOT-TMA mixture; polyethylene glycol electrolyte medium

AdditivesLiI (0.5 M), I2 (0.05 M), PEDOT-TMA; TiO2 paste; Kapton tape spacer

Atmospherenot specified

Temperature50 C annealing for photoelectrode and counter-electrode

Time10 min mortar grinding; 0.5 h photoelectrode anneal; 10 s spin coating; 10 min counter-electrode anneal

Substrate orientationITO glass substrate, sheet resistance 10 ohm/sq

Oxidant / reductantLiI/I2 redox electrolyte

Work-upPolymer/TiO2 mixture painted on ITO with 50 um Kapton spacer; annealed; assembled with PEDOT-TMA counter-electrode; electrolyte injected.

Activation50 C annealing of photoelectrode for 0.5 h and counter-electrode for 10 min

Scalability contextManual mortar mixing and painted films; no scale-up discussion.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 1a	0.3 mol	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	TiO2 paste PECC-K01	0.1 mL	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	PEDOT-TMA	mixed with ethanol at volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	ethanol	PEDOT-TMA:ethanol volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	LiI	0.5 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	I2	0.05 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	polyethylene glycol	electrolyte solvent	p004 (journal p1616) · 2.5. Fabrication of DSSCs

Partial recipeSource: Main

Route 8: Other

p004 (journal p1616) · 2.5. Fabrication of DSSCs

Metal precursorscoordination polymer 1b; TiO2 paste PECC-K01; PEDOT-TMA counter-electrode material

Linker precursorscoordination polymer ligand already present in sensitizer

Solventsethanol for PEDOT-TMA mixture; polyethylene glycol electrolyte medium

AdditivesLiI (0.5 M), I2 (0.05 M), PEDOT-TMA; TiO2 paste; Kapton tape spacer

Atmospherenot specified

Temperature50 C annealing for photoelectrode and counter-electrode

Time10 min mortar grinding; 0.5 h photoelectrode anneal; 10 s spin coating; 10 min counter-electrode anneal

Substrate orientationITO glass substrate, sheet resistance 10 ohm/sq

Oxidant / reductantLiI/I2 redox electrolyte

Work-upPolymer/TiO2 mixture painted on ITO with 50 um Kapton spacer; annealed; assembled with PEDOT-TMA counter-electrode; electrolyte injected.

Activation50 C annealing of photoelectrode for 0.5 h and counter-electrode for 10 min

Scalability contextManual mortar mixing and painted films; no scale-up discussion.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 1b	0.3 mol	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	TiO2 paste PECC-K01	0.1 mL	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	PEDOT-TMA	mixed with ethanol at volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	ethanol	PEDOT-TMA:ethanol volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	LiI	0.5 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	I2	0.05 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	polyethylene glycol	electrolyte solvent	p004 (journal p1616) · 2.5. Fabrication of DSSCs

Partial recipeSource: Main

Route 9: Other

p004 (journal p1616) · 2.5. Fabrication of DSSCs

Metal precursorscoordination polymer 2a; TiO2 paste PECC-K01; PEDOT-TMA counter-electrode material

Linker precursorscoordination polymer ligand already present in sensitizer

Solventsethanol for PEDOT-TMA mixture; polyethylene glycol electrolyte medium

AdditivesLiI (0.5 M), I2 (0.05 M), PEDOT-TMA; TiO2 paste; Kapton tape spacer

Atmospherenot specified

Temperature50 C annealing for photoelectrode and counter-electrode

Time10 min mortar grinding; 0.5 h photoelectrode anneal; 10 s spin coating; 10 min counter-electrode anneal

Substrate orientationITO glass substrate, sheet resistance 10 ohm/sq

Oxidant / reductantLiI/I2 redox electrolyte

Work-upPolymer/TiO2 mixture painted on ITO with 50 um Kapton spacer; annealed; assembled with PEDOT-TMA counter-electrode; electrolyte injected.

Activation50 C annealing of photoelectrode for 0.5 h and counter-electrode for 10 min

Scalability contextManual mortar mixing and painted films; no scale-up discussion.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 2a	0.3 mol	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	TiO2 paste PECC-K01	0.1 mL	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	PEDOT-TMA	mixed with ethanol at volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	ethanol	PEDOT-TMA:ethanol volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	LiI	0.5 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	I2	0.05 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	polyethylene glycol	electrolyte solvent	p004 (journal p1616) · 2.5. Fabrication of DSSCs

Partial recipeSource: Main

Route 10: Other

p004 (journal p1616) · 2.5. Fabrication of DSSCs

Metal precursorscoordination polymer 2b; TiO2 paste PECC-K01; PEDOT-TMA counter-electrode material

Linker precursorscoordination polymer ligand already present in sensitizer

Solventsethanol for PEDOT-TMA mixture; polyethylene glycol electrolyte medium

AdditivesLiI (0.5 M), I2 (0.05 M), PEDOT-TMA; TiO2 paste; Kapton tape spacer

Atmospherenot specified

Temperature50 C annealing for photoelectrode and counter-electrode

Time10 min mortar grinding; 0.5 h photoelectrode anneal; 10 s spin coating; 10 min counter-electrode anneal

Substrate orientationITO glass substrate, sheet resistance 10 ohm/sq

Oxidant / reductantLiI/I2 redox electrolyte

Work-upPolymer/TiO2 mixture painted on ITO with 50 um Kapton spacer; annealed; assembled with PEDOT-TMA counter-electrode; electrolyte injected.

Activation50 C annealing of photoelectrode for 0.5 h and counter-electrode for 10 min

Scalability contextManual mortar mixing and painted films; no scale-up discussion.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 2b	0.3 mol	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	TiO2 paste PECC-K01	0.1 mL	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	PEDOT-TMA	mixed with ethanol at volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	ethanol	PEDOT-TMA:ethanol volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	LiI	0.5 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	I2	0.05 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	polyethylene glycol	electrolyte solvent	p004 (journal p1616) · 2.5. Fabrication of DSSCs

Partial recipeSource: Main

Route 11: Other

p004 (journal p1616) · 2.5. Fabrication of DSSCs

Metal precursorscoordination polymer 3; TiO2 paste PECC-K01; PEDOT-TMA counter-electrode material

Linker precursorscoordination polymer ligand already present in sensitizer

Solventsethanol for PEDOT-TMA mixture; polyethylene glycol electrolyte medium

AdditivesLiI (0.5 M), I2 (0.05 M), PEDOT-TMA; TiO2 paste; Kapton tape spacer

Atmospherenot specified

Temperature50 C annealing for photoelectrode and counter-electrode

Time10 min mortar grinding; 0.5 h photoelectrode anneal; 10 s spin coating; 10 min counter-electrode anneal

Substrate orientationITO glass substrate, sheet resistance 10 ohm/sq

Oxidant / reductantLiI/I2 redox electrolyte

Work-upPolymer/TiO2 mixture painted on ITO with 50 um Kapton spacer; annealed; assembled with PEDOT-TMA counter-electrode; electrolyte injected.

Activation50 C annealing of photoelectrode for 0.5 h and counter-electrode for 10 min

Scalability contextManual mortar mixing and painted films; no scale-up discussion.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	coordination polymer 3	0.3 mol	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	TiO2 paste PECC-K01	0.1 mL	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Other	PEDOT-TMA	mixed with ethanol at volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	ethanol	PEDOT-TMA:ethanol volume ratio 5:1	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	LiI	0.5 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Electrolyte	I2	0.05 M	p004 (journal p1616) · 2.5. Fabrication of DSSCs
Solvent	polyethylene glycol	electrolyte solvent	p004 (journal p1616) · 2.5. Fabrication of DSSCs

Vague recipeSource: Main

Route 12: Other

p003 (journal p1615) · 2.1. Materials

Metal precursorsnot specified in this paper

Linker precursorsHm-dtc source not specified in this paper

Solventsnot specified in this paper

Atmospherenot specified

Work-upnot specified

Scalability contextNo scale-up discussion.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	not specified in this paper; Ni(Hm-dtc)2 prepared using a procedure similar to refs 33 and 34	Not specified	p003 (journal p1615) · 2.1. Materials