Synthesis evidence

Stabilization of cyclic water tetramers and dimers in the crystal host of 2D coordination networks: electrical conductivity and dielectric studies

Dutta B., Ghosh S.R., Ray A. et al. · New Journal of Chemistry · 2020 · 15857-15870

4 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

10 · Thermal stability and dehydration/rehydration studies

Metal precursorspreformed compound 1
Solventsnone
Additivesnone
Atmospherevacuum
Temperature145
Time1
Work-upheated crystals; complete removal of water indicated by TGA below 200 C
Activationthermal dehydration under vacuum
Scalability contextAnalytical dehydration only; no scale stated.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Othercompound 1 crystalsnot specified10 · Thermal stability and dehydration/rehydration studies
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

2 · Synthesis of compound 1

Metal precursorsZn(NO3)2.6H2O (reported as Zn(NO)3.6H2O in text), 0.06 g, 0.2 mmol, in H2O
Linker precursors4-nvp (0.046 g, 0.2 mmol) in MeOH; H2fum (0.023 g, 0.2 mmol) neutralised with Et3N in EtOH
SolventsMeOH 2 mL; H2O 2 mL; 2 mL 1:1 MeOH/H2O buffer layer; EtOH 2 mL
AdditivesEt3N (0.021 g, 0.2 mmol) for neutralisation of H2fum
Atmospherenot specified; ambient layering inferred
Temperatureroom temperature/not specified
Time72
Work-upyellow needle-shaped crystals collected after three days; isolation/washing not specified
Activationnone reported for as-synthesised crystals
Scalability contextLayered crystallisation produced 0.095 g, 70% yield; no scale-up data.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker4-nvp0.046 g, 0.2 mmol · in MeOH (2 mL)2 · Synthesis of compound 1
Metal SourceZn(NO)3.6H2O / Zn(NO3)2.6H2O0.06 g, 0.2 mmol · in H2O (2 mL)2 · Synthesis of compound 1
SolventMeOH/H2O buffer2 mL · 1:1 v/v2 · Synthesis of compound 1
LinkerH2fum0.023 g, 0.2 mmol · in EtOH (2 mL)2 · Synthesis of compound 1
BaseEt3N0.021 g, 0.2 mmol · neutralised H2fum2 · Synthesis of compound 1
SolventEtOH2 mL2 · Synthesis of compound 1
Complete recipeSource: Main

Route 3: Other

10 · Thermal stability and dehydration/rehydration studies

Metal precursorspreformed compound 2
Solventsnone
Additivesnone
Atmospherevacuum
Temperature145
Time1
Work-upheated crystals; complete removal of water indicated by TGA below 200 C
Activationthermal dehydration under vacuum
Scalability contextAnalytical dehydration only; no scale stated.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Othercompound 2 crystalsnot specified10 · Thermal stability and dehydration/rehydration studies
Complete recipeSource: Main

Route 4: Liquid Liquid Interface

3 · Synthesis of compound 2

Metal precursorsZn(NO3)2.6H2O as for compound 1
Linker precursors4-nvp as for compound 1; H2mes (0.026 g, 0.2 mmol) instead of H2fum
Solventssame layered MeOH/H2O buffer/EtOH solvent system as compound 1
AdditivesEt3N presumed as same procedure as compound 1
Atmospherenot specified; ambient layering inferred
Temperatureroom temperature/not specified
Timea few days
Work-upyellow needle-shaped crystals obtained after a few days; isolation/washing not specified
Activationnone reported for as-synthesised crystals
Scalability contextLayered crystallisation produced 0.093 g, 70% yield; no scale-up data.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4-nvp0.046 g, 0.2 mmol · as for compound 13 · Synthesis of compound 2
Metal SourceZn(NO3)2.6H2O0.06 g, 0.2 mmol · as for compound 13 · Synthesis of compound 2
LinkerH2mes0.026 g, 0.2 mmol · in EtOH layer by analogy to compound 13 · Synthesis of compound 2
BaseEt3N0.021 g, 0.2 mmol presumed · same procedure as compound 13 · Synthesis of compound 2
SolventMeOH/H2O/EtOH2 mL MeOH + 2 mL H2O + 2 mL buffer + 2 mL EtOH by analogy3 · Synthesis of compound 2