cMOF Evidence Base

Synthesis evidence

Two one-dimensional germanium(IV) coordination polymers based on macrocyclic tetraaza[14]annulene with notable semiconducting property

Wang X., Shen X., Zhang Y.-J. et al. · Inorganic Chemistry Communications · 2013 · 45-49

4 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

4 · Reference 31

Metal precursorsGe(tmtaa)Cl2
Linker precursorsdisodium 1,4-benzenedicarboxylate
ActivationNone reported.
Scalability contextBulk powder yield reported as 86%, but stirring time, solvent and isolation details are not given.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceGe(tmtaa)Cl2Not specified4 · Reference 31
Linkerdisodium 1,4-benezedicarboxylateNot specified4 · Reference 31
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

4 · Reference 31 · Scheme 1

Metal precursorsGe(tmtaa)Cl2 (48.6 mg, 0.1 mmol); Ge(tmtaa)Cl2 precursor prepared from H2tmtaa and GeCl4 in Scheme 1
Linker precursorsdisodium 1,4-benzenedicarboxylate (21.0 mg, 0.1 mmol)
Solventsmethanol/ethyl acetate (1:1 v/v, 8 mL) for Ge(tmtaa)Cl2; water (5 mL) for linker solution
AtmosphereLayering route atmosphere not stated; Scheme 1 precursor step states N2 atm.
Temperatureroom temperature
Time504
Work-upOrange crystals formed after three weeks; isolation/washing not stated.
ActivationNone reported.
Scalability contextSingle crystals require three weeks; bulk powder can be obtained faster by direct stirring in 86% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceGe(tmtaa)Cl248.6 mg, 0.1 mmol4 · Reference 31 · Scheme 1
Linkerdisodium 1,4-benezedicarboxylate21.0 mg, 0.1 mmol4 · Reference 31 · Scheme 1
Solventmethanol and ethyl acetate (1:1, v/v%)8 mL4 · Reference 31 · Scheme 1
Solventwater5 mL4 · Reference 31 · Scheme 1
Vague recipeSource: Main

Route 3: Other

4 · Reference 32

Metal precursorsGe(tmtaa)Cl2
Linker precursorsdisodium 2,5-dihydroxyl-1,4-benzenedicarboxylate
ActivationNone reported.
Scalability contextBulk powder yield reported as 83%, but stirring time, solvent and isolation details are not given.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceGe(tmtaa)Cl2Not specified4 · Reference 32
Linkerdisodium 2,5-dihydroxyl-1,4-benezedicarboxylateNot specified4 · Reference 32
Partial recipeSource: Main

Route 4: Liquid Liquid Interface

4 · Reference 32 · Scheme 1

Metal precursorsGe(tmtaa)Cl2
Linker precursorsdisodium 2,5-dihydroxyl-1,4-benzenedicarboxylate
SolventsSimilar method as compound 1: methanol/ethyl acetate and water inferred from the stated method.
AtmosphereLayering route atmosphere not stated; Scheme 1 precursor step states N2 atm.
Temperatureroom temperature
Time504
Work-upOrange single crystals formed; isolation/washing not stated.
ActivationNone reported.
Scalability contextPowder of 2 obtained in 83% yield.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceGe(tmtaa)Cl2Not specified4 · Reference 32 · Scheme 1
Linkerdisodium 2,5-dihydroxyl-1,4-benezedicarboxylateNot specified4 · Reference 32 · Scheme 1