Synthesis · Magnetic and electrical behaviors of the homo-and heterometallic 1d and 3d coordination polymers based on the partial decomposition of the [cr(C2o4)3]3− building block

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Liquid Liquid Interface

3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)

Metal precursorsK3[Cr(C2O4)3]·3H2O (0.049 g; 0.1 mmol); MnCl2·4H2O (0.020 g; 0.1 mmol)

Linker precursors2,2'-bipyridine (bpy; 0.016 g; 0.1 mmol); oxalate supplied by tris(oxalato)chromate(III) decomposition

Solventswater (4 mL); methanol (4 mL + 4 mL)

Atmosphereair / not otherwise specified

Temperatureroom temperature

Time336

Work-upisolated, washed with a small amount of water, dried in air

Activationnone reported

Scalability contextSmall-volume layered crystallisation in a test tube.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	K3[Cr(C2O4)3]·3H2O	0.049 g; 0.1 mmol · in 4 mL aqueous solution	3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)
Metal Source	MnCl2·4H2O	0.020 g; 0.1 mmol · in 4 mL methanol solution	3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)
Linker	bpy	0.016 g; 0.1 mmol · in 4 mL methanol solution	3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)
Solvent	water	4 mL	3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)
Solvent	methanol	8 mL total	3 · 2.2.1. Synthesis of {[Mn(bpy)(C2O4)]·1.5H2O}n (1)

Complete recipeSource: Main

Route 2: Liquid Liquid Interface

3 · 2.2.2. Synthesis of compound 2

Metal precursorsCuCl2·2H2O (0.017 g; 0.1 mmol); K3[Cr(C2O4)3]·3H2O (0.049 g; 0.1 mmol)

Linker precursors2,2'-bipyridine (bpy; 0.016 g; 0.1 mmol); oxalate from tris(oxalato)chromate(III)

Solventsmethanol/dichloromethane 1:1 (8 mL); water (3 mL)

Atmosphereair / not otherwise specified

Temperatureroom temperature

Time240

Work-upisolated, washed with water, dried in air

Activationnone reported

Scalability contextSmall-volume layered crystallisation in a test tube; transient blue {[Cu(bpy)(C2O4)]·2.5H2O}n crystals decomposed before final product formation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuCl2·2H2O	0.017 g; 0.1 mmol · in 8 mL methanol/dichloromethane (1:1) mixture with bpy	3 · 2.2.2. Synthesis of compound 2
Metal Source	K3[Cr(C2O4)3]·3H2O	0.049 g; 0.1 mmol · in 3 mL aqueous solution	3 · 2.2.2. Synthesis of compound 2
Linker	bpy	0.016 g; 0.1 mmol · in 8 mL methanol/dichloromethane (1:1) mixture with CuCl2·2H2O	3 · 2.2.2. Synthesis of compound 2
Solvent	methanol/dichloromethane (1:1)	8 mL	3 · 2.2.2. Synthesis of compound 2
Solvent	water	3 mL	3 · 2.2.2. Synthesis of compound 2

Complete recipeSource: Main

Route 3: Liquid Liquid Interface

3-4 · 2.2.3. Synthesis of compound 3

Metal precursorsK3[Cr(C2O4)3]·3H2O (0.049 g; 0.1 mmol); Cu(NO3)2·3H2O (0.025 g; 0.1 mmol); Ca(NO3)2·4H2O (0.007 g; 0.03 mmol)

Linker precursors1,10-phenanthroline (phen; 0.020 g; 0.1 mmol); oxalate from tris(oxalato)chromate(III)

Solventswater (4 mL); acetonitrile (4 mL + 5 mL); methanol wash

Atmosphereair / not otherwise specified

Temperatureroom temperature

Timea few days

Work-upisolated, washed with a diluted matrix and a small amount of methanol, quickly dried in air

Activationnone reported

Scalability contextSmall-volume multilayer crystallisation in a test tube.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	K3[Cr(C2O4)3]·3H2O	0.049 g; 0.1 mmol · in 4 mL aqueous solution	3-4 · 2.2.3. Synthesis of compound 3
Metal Source	Cu(NO3)2·3H2O	0.025 g; 0.1 mmol · in 5 mL acetonitrile solution with Ca(NO3)2·4H2O	3-4 · 2.2.3. Synthesis of compound 3
Metal Source	Ca(NO3)2·4H2O	0.007 g; 0.03 mmol · in 5 mL acetonitrile solution with Cu(NO3)2·3H2O	3-4 · 2.2.3. Synthesis of compound 3
Linker	phen	0.020 g; 0.1 mmol · in 4 mL acetonitrile solution	3-4 · 2.2.3. Synthesis of compound 3
Solvent	water	4 mL	3-4 · 2.2.3. Synthesis of compound 3
Solvent	acetonitrile	9 mL total	3-4 · 2.2.3. Synthesis of compound 3