Synthesis · Structural, magnetic and electrical properties of one-dimensional tetraamidatodiruthenium compounds

12 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol)

Linker precursorso-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Linker	o-toluamide	0.20 g, 1.5 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Additive	potassium bromide	0.24 g, 2 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Base	triethylamine	0.25 mL	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Solvent	absolute ethanol	8 mL	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)

Complete recipeSource: Main

Route 2: Solvothermal

p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol)

Linker precursorso-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Linker	o-toluamide	0.20 g, 1.5 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Additive	potassium bromide	0.24 g, 2 mmol	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Base	triethylamine	0.25 mL	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)
Solvent	absolute ethanol	same quantity as method (a)	p008-p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-o-Me)4]n (1)

Complete recipeSource: Main

Route 3: Other

p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol, by analogy to compound 1)

Linker precursorsm-toluamide (0.20 g, 1.5 mmol)

Solventsmethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol, by analogy to compound 1)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Linker	m-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Additive	potassium bromide	0.24 g, 2 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Solvent	methanol	8 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)

Complete recipeSource: Main

Route 4: Solvothermal

p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol, by analogy to compound 1)

Linker precursorsm-toluamide (0.20 g, 1.5 mmol)

Solventsmethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol, by analogy to compound 1)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Linker	m-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Additive	potassium bromide	0.24 g, 2 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)
Solvent	methanol	not restated; follows referenced method	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-m-Me)4]n (2)

Complete recipeSource: Main

Route 5: Other

p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol, by analogy to compound 1)

Linker precursorsp-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol, by analogy to compound 1)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Linker	p-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Additive	potassium bromide	0.24 g, 2 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Solvent	absolute ethanol	8 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)

Partial recipeSource: Main

Route 6: Solvothermal

p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)

Metal precursorsBromidotetrakis(acetato)diruthenium(II,III) (0.13 g, 0.25 mmol, by analogy to compound 1)

Linker precursorsp-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium bromide (0.24 g, 2 mmol, by analogy to compound 1)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Bromidotetrakis(acetato)diruthenium(II,III)	0.13 g, 0.25 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Linker	p-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Additive	potassium bromide	0.24 g, 2 mmol (by analogy to compound 1)	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)
Solvent	absolute ethanol	not restated; follows referenced method	p009 · Synthesis of [Ru2Br(mu-NHOCC6H4-p-Me)4]n (3)

Complete recipeSource: Main

Route 7: Other

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol)

Linker precursorso-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Linker	o-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Additive	potassium iodide	0.34 g, 2 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Solvent	absolute ethanol	8 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)

Complete recipeSource: Main

Route 8: Solvothermal

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol)

Linker precursorso-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Linker	o-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Additive	potassium iodide	0.34 g, 2 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)
Solvent	absolute ethanol	same quantity as method (a)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-o-Me)4]n (4)

Complete recipeSource: Main

Route 9: Other

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol, by analogy to compound 4)

Linker precursorsm-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol, by analogy to compound 4)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Linker	m-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Additive	potassium iodide	0.34 g, 2 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Solvent	absolute ethanol	8 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)

Complete recipeSource: Main

Route 10: Solvothermal

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol, by analogy to compound 4)

Linker precursorsm-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol, by analogy to compound 4)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Linker	m-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Additive	potassium iodide	0.34 g, 2 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)
Solvent	absolute ethanol	not restated; follows referenced method	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-m-Me)4]n (5)

Complete recipeSource: Main

Route 11: Other

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol, by analogy to compound 4)

Linker precursorsp-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol (8 mL)

Additivestriethylamine (0.25 mL)

Atmospheresealed TFM Teflon microwave vessel; atmosphere not specified

Temperature120

Time16 h isotherm after 15 min ramp; 20 min cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol, by analogy to compound 4)

Work-upBrown suspension/solid filtered and washed twice with 10 mL cold ethanol

ActivationMicrowave heating in ETHOS ONE oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Linker	p-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Additive	potassium iodide	0.34 g, 2 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Solvent	absolute ethanol	8 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)

Complete recipeSource: Main

Route 12: Solvothermal

p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)

Metal precursorsIodotetrakis(acetato)diruthenium(II,III) (0.14 g, 0.25 mmol, by analogy to compound 4)

Linker precursorsp-toluamide (0.20 g, 1.5 mmol)

Solventsabsolute ethanol

Additivestriethylamine (0.25 mL)

Atmosphereclosed 23 mL Teflon-lined autoclave; atmosphere not specified

Temperature100

Time24 h isotherm after 2 h ramp; 24 h cooling ramp

Oxidant / reductantpotassium iodide (0.34 g, 2 mmol, by analogy to compound 4)

Work-upCrystalline/microcrystalline brown solid filtered and washed with cold ethanol (5 x 10 mL)

ActivationSolvothermal heating in Memmert UFE 400 oven

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Iodotetrakis(acetato)diruthenium(II,III)	0.14 g, 0.25 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Linker	p-toluamide	0.20 g, 1.5 mmol	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Additive	potassium iodide	0.34 g, 2 mmol (by analogy to compound 4)	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Base	triethylamine	0.25 mL	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)
Solvent	absolute ethanol	not restated; follows referenced method	p009 · Synthesis of [Ru2I(mu-NHOCC6H4-p-Me)4]n (6)