cMOF Evidence Base

Synthesis evidence

Semiconducting lanthanide polymers of pyridine-2,6-dicarboxylate: Hydrothermal synthesis, structural characterization, electrical conductivity and luminescence properties

Ay B., Yildiz E., Kani I. · Polyhedron · 2018 · 1-8

2 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

2 · 2.2. Synthesis of (H2pip)n[La2(pydc)4(H2O)2]n

Metal precursorslanthanum(III) nitrate hexahydrate, 0.130 g, 0.30 mmol
Linker precursors2,6-pyridinedicarboxylic acid, 0.150 g, 0.90 mmol; piperazine, 0.078 g, 0.90 mmol
SolventsH2O, 5 mL, 278 mmol
Additivespiperazine also acts as base/counter-cation precursor
AtmosphereAutogenous pressure in 23 mL PTFE-lined stainless-steel container
Temperature170
Time84
Work-upHeterogeneous solution mixture separated from solid phase; crystals washed with water and dried at room temperature.
ActivationNone reported.
Scalability contextSmall-volume hydrothermal batch in 23 mL PTFE-lined container; isolated yield 93.3% based on La.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcelanthanum (III) nitrate hexahydrate0.130 g, 0.30 mmol2 · 2.2. Synthesis of (H2pip)n[La2(pydc)4(H2O)2]n
Linker2,6-pyridinedicarboxylic acid0.150 g, 0.90 mmol2 · 2.2. Synthesis of (H2pip)n[La2(pydc)4(H2O)2]n
Basepiperazine0.078 g, 0.90 mmol2 · 2.2. Synthesis of (H2pip)n[La2(pydc)4(H2O)2]n
SolventH2O5 mL, 278 mmol2 · 2.2. Synthesis of (H2pip)n[La2(pydc)4(H2O)2]n
Complete recipeSource: Main

Route 2: Hydrothermal

2 · 2.3. Synthesis of (H2pip)n[Nd2(pydc)4(H2O)2]n

Metal precursorsneodymium(III) nitrate hexahydrate, 0.132 g, 0.30 mmol
Linker precursors2,6-pyridinedicarboxylic acid, 0.150 g, 0.90 mmol; piperazine, 0.078 g, 0.90 mmol by analogy to route for 1
SolventsH2O, 5 mL, 278 mmol by analogy to route for 1
Additivespiperazine also acts as base/counter-cation precursor
AtmosphereAutogenous pressure in 23 mL PTFE-lined stainless-steel container
Temperature170
Time84
Work-upPrepared similarly to compound 1; crystals obtained under hydrothermal conditions, washed/dried as in the route for 1.
ActivationNone reported.
Scalability contextSmall-volume hydrothermal batch in 23 mL PTFE-lined container; isolated yield 76% based on Nd.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNd(NO3)3.6H2O0.132 g, 0.30 mmol2 · 2.3. Synthesis of (H2pip)n[Nd2(pydc)4(H2O)2]n
Linker2,6-pyridinedicarboxylic acid0.150 g, 0.90 mmol (by similarity to route for 1)2 · 2.3. Synthesis of (H2pip)n[Nd2(pydc)4(H2O)2]n
Basepiperazine0.078 g, 0.90 mmol (by similarity to route for 1)2 · 2.3. Synthesis of (H2pip)n[Nd2(pydc)4(H2O)2]n
SolventH2O5 mL, 278 mmol (by similarity to route for 1)2 · 2.3. Synthesis of (H2pip)n[Nd2(pydc)4(H2O)2]n