cMOF Evidence Base

Synthesis evidence

Co-Ca Phosphonate Showing Humidity-Sensitive Single Crystal to Single Crystal Structural Transformation and Tunable Proton Conduction Properties

Bao S.-S., Li N.-Z., Taylor J.M. et al. · Chemistry of Materials · 2015 · 8116-8125

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: Other

main p.3, article p.8118 · Experimental Section - Preparation of CoCa.2H2O

Metal precursorsFresh CoCa.4H2O crystals
Linker precursorsnotpH2(4-) framework already formed in CoCa.4H2O
AtmosphereAir, ca. 50% RH
Temperatureca. 30 C
Timeca. 336 h (2 weeks)
Work-upDried in air.
ActivationHumidity-driven removal of two lattice water molecules.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otherfresh crystals of CoCa.4H2ONot specifiedmain p.3, article p.8118 · Experimental Section - Preparation of CoCa.2H2O
Complete recipeSource: Main

Route 2: Other

main p.3, article p.8118 · Experimental Section - Preparation of CoCa.4H2O

Metal precursorsCa(OH)2; Co(notpH3).3H2O precursor
Linker precursorsnotpH6 is pre-incorporated in Co(notpH3).3H2O; Co(notpH3).3H2O was prepared according to literature.
SolventsWater, 10 mL
Additives1.0 mol/L HClO4 to adjust pH to 1.9
AtmosphereAir/ambient atmosphere not explicitly controlled.
Temperature100 C for stirring, then room temperature crystallisation
TimeStirred overnight at 100 C; stood 3 days at room temperature
Work-upSuspension filtered; filtrate adjusted to pH 1.9; crystals isolated after standing.
Scalability contextReported yield 77.2% based on Co; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCa(OH)20.60 mmol, 0.044 gmain p.3, article p.8118 · Experimental Section - Preparation of CoCa.4H2O
Metal SourceCo(notpH3).3H2O0.20 mmol, 0.104 gmain p.3, article p.8118 · Experimental Section - Preparation of CoCa.4H2O
Solventwater10 mLmain p.3, article p.8118 · Experimental Section - Preparation of CoCa.4H2O
AcidHClO4added to pH 1.9 · 1.0 mol/Lmain p.3, article p.8118 · Experimental Section - Preparation of CoCa.4H2O
Partial recipeSource: Main

Route 3: Other

main p.5, article p.8120 · Water Adsorption/Desorption Isotherms · Figure 2c

Metal precursorsCoCa.nH2O
Linker precursorsnotpH2(4-) framework already formed in CoCa.nH2O
AtmosphereVacuum for sorption pretreatment; nitrogen flow for TGA/PXRD heating assignment
Temperature120 C for sorption pretreatment; fully dehydrated by 220 C in nitrogen during PXRD/TGA discussion
Time2 h at 120 C under vacuum
Work-upPretreated under vacuum before sorption measurements.
ActivationRemoval of lattice and coordinated water to form CoCa-de.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCoCa.nH2ONot specifiedmain p.5, article p.8120 · Water Adsorption/Desorption Isotherms · Figure 2c