Synthesis · Multiple-Hydrogen-Bond Approach to Uncommon Pd(III) Oxidation State: A Pd-Br Chain with High Conductivity and Thermal Stability

3 structured synthesis routes

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

Partial recipeSource: Both

SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)

Metal precursors[Pd(dabdOH)2]Br2 precursor

Linker precursorsdabdOH already coordinated in [Pd(dabdOH)2]Br2

Solvents1:4 H2O/CH3OH solution for precursor; Br2/1,4-dioxane solution as Br2 vapour source

AtmosphereBr2 vapour diffusion

Temperaturenot specified, likely room temperature

Timeabout 24

Oxidant / reductantBr2 oxidant

Work-upCopper-luster rod-like single crystals collected after vapour diffusion; no activation reported.

Scalability contextReported yield 53.9%; crystals grew in about one day.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	[Pd(dabdOH)2]Br2	not specified for final diffusion step	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)
Oxidant	Br2	not specified · Br2/1,4-dioxane solution, concentration not specified	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)
Solvent	H2O/CH3OH	not specified · 1:4 H2O/CH3OH	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)
Solvent	1,4-dioxane	not specified · Br2/1,4-dioxane solution	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)

Partial recipeSource: SI

SI p.S3 · Synthesis of (2S,3S)-2,3-diaminobutane-1,4-diol (dabdOH)

Linker precursorsdiazide A, 850 mg, 4.93 mmol

Solventsanhydrous methanol, 50 mL

Additives10% Pd/C, 165 mg

AtmosphereH2 at atmospheric pressure

Temperatureroom temperature

Time24

Oxidant / reductantH2/Pd-C reduction of azide groups to amine groups

Work-upCatalyst removed by filtration over celite; solvent removed under vacuum; residue dried.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	diazide A	850 mg, 4.93 mmol	SI p.S3 · Synthesis of (2S,3S)-2,3-diaminobutane-1,4-diol (dabdOH)
Solvent	anhydrous methanol	50 mL	SI p.S3 · Synthesis of (2S,3S)-2,3-diaminobutane-1,4-diol (dabdOH)
Additive	10% Pd/C	165 mg · 10%	SI p.S3 · Synthesis of (2S,3S)-2,3-diaminobutane-1,4-diol (dabdOH)
Reductant	H2	atmospheric pressure	SI p.S3 · Synthesis of (2S,3S)-2,3-diaminobutane-1,4-diol (dabdOH)

Complete recipeSource: SI

SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)

Metal precursorspalladium bromide, 208 mg, 0.78 mmol

Linker precursorsdabdOH, 206 mg, 1.7 mmol

SolventsH2O, 25 mL

Atmospherenot specified

Temperature55

Time6

Work-upSolution filtered and evaporated under reduced pressure to give white solid.

Scalability contextReported isolated yield 91%.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	dabdOH	206 mg, 1.7 mmol	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)
Metal Source	palladium bromide	208 mg, 0.78 mmol	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)
Solvent	H2O	25 mL	SI p.S3 · Syntheses of [Pd(dabdOH)2]Br2 and [Pd(dabdOH)2Br]Br2 (3)