Synthesis evidence

Controlled synthesis of Cu-/Ni-based 1D c-MOFs and their application in near-linear temperature sensing

Zhang J., Xu C., Li J. et al. · Vacuum · 2023 · 111937

16 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.25 mL
Atmospherenot reported
Temperature80
Time3
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.25 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 2: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.75 mL
Atmospherenot reported
Temperature80
Time6
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.75 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 3: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.75 mL
Atmospherenot reported
Temperature80
Time12
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.75 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 4: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.75 mL
Atmospherenot reported
Temperature80
Time24
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.75 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 5: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.25 mL
Atmospherenot reported
Temperature80
Time6
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.25 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 6: Hydrothermal

main p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.25 mL
Atmospherenot reported
Temperature80
Time12
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
LinkerHHTP35 mg, 0.110 mmolmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
Solventdeionised water7 mLmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
SolventDMF0.25 mLmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
Partial recipeSource: Main

Route 7: Hydrothermal

main p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.25 mL
Atmospherenot reported
Temperature80
Time24
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
LinkerHHTP35 mg, 0.110 mmolmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
Solventdeionised water7 mLmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
SolventDMF0.25 mLmain p.4 · 2.2-2.3 Preparation; Table 1 · Fig. 3; Table 1
Partial recipeSource: Main

Route 8: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.50 mL
Atmospherenot reported
Temperature80
Time3
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.50 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 9: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.50 mL
Atmospherenot reported
Temperature80
Time6
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.50 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 10: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Abstract

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.50 mL
Atmospherenot reported
Temperature80
Time12
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Abstract
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Abstract
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Abstract
SolventDMF0.50 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Abstract
Partial recipeSource: Main

Route 11: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.50 mL
Atmospherenot reported
Temperature80
Time24
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.50 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 12: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3

Metal precursorsCu(CH3COO)2.H2O (39 mg, 0.195 mmol)
Linker precursorsHHTP (35 mg, 0.110 mmol)
Solventsdeionised water 7 mL; DMF 0.75 mL
Atmospherenot reported
Temperature80
Time3
Oxidant / reductantnone reported
Work-upPowders collected after drying to constant weight; washing not reported for Cu route.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2.H2O39 mg, 0.195 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
LinkerHHTP35 mg, 0.110 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Solventdeionised water7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
SolventDMF0.75 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 3
Partial recipeSource: Main

Route 13: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2

Metal precursorsNi(CH3COO)2.4H2O (114 mg, 0.458 mmol)
Linker precursorsHHTP (50 mg, 0.154 mmol)
Solventsdioxane added to reach total volume of 7 mL
Atmospherenot reported
Temperature80
Time3
Oxidant / reductantnone reported
Work-upCooled to room temperature naturally; crude products washed three times by anhydrous ethanol and deionised water; dried to constant weight.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(CH3COO)2.4H2O114 mg, 0.458 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
LinkerHHTP50 mg, 0.154 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Solventdioxanetotal reaction volume 7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Partial recipeSource: Main

Route 14: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2

Metal precursorsNi(CH3COO)2.4H2O (114 mg, 0.458 mmol)
Linker precursorsHHTP (50 mg, 0.154 mmol)
Solventsdioxane added to reach total volume of 7 mL
Atmospherenot reported
Temperature80
Time6
Oxidant / reductantnone reported
Work-upCooled to room temperature naturally; crude products washed three times by anhydrous ethanol and deionised water; dried to constant weight.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(CH3COO)2.4H2O114 mg, 0.458 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
LinkerHHTP50 mg, 0.154 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Solventdioxanetotal reaction volume 7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Partial recipeSource: Main

Route 15: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2

Metal precursorsNi(CH3COO)2.4H2O (114 mg, 0.458 mmol)
Linker precursorsHHTP (50 mg, 0.154 mmol)
Solventsdioxane added to reach total volume of 7 mL
Atmospherenot reported
Temperature80
Time12
Oxidant / reductantnone reported
Work-upCooled to room temperature naturally; crude products washed three times by anhydrous ethanol and deionised water; dried to constant weight.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(CH3COO)2.4H2O114 mg, 0.458 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
LinkerHHTP50 mg, 0.154 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Solventdioxanetotal reaction volume 7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Partial recipeSource: Main

Route 16: Hydrothermal

main p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2

Metal precursorsNi(CH3COO)2.4H2O (114 mg, 0.458 mmol)
Linker precursorsHHTP (50 mg, 0.154 mmol)
Solventsdioxane added to reach total volume of 7 mL
Atmospherenot reported
Temperature80
Time24
Oxidant / reductantnone reported
Work-upCooled to room temperature naturally; crude products washed three times by anhydrous ethanol and deionised water; dried to constant weight.
Activationnot reported
Scalability context10 mL glass vial batch; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(CH3COO)2.4H2O114 mg, 0.458 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
LinkerHHTP50 mg, 0.154 mmolmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2
Solventdioxanetotal reaction volume 7 mLmain p.3 · 2.2-2.3 Preparation; Table 1 · Table 1; Fig. 2