cMOF Evidence Base

Synthesis evidence

1-Hydroxybenzotriazole (HOBt) acidity, formation constant with different metals and thermodynamic parameters: Synthesis and characterization of some HOBt metal complexes - Crystal structures of two polymers: [Cu2(H2O)5(OBt)2(μ-OBt)2] · 2H2O · EtOH (1A) and [Cu(μ-OBt)(HOBt)(OBt)(EtOH)] (1B)

Hammud H.H., Holman K.T., Masoud M.S. et al. · Inorganica Chimica Acta · 2009 · 3526-3540

8 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

3528 / rendered p003 · 2.3.1

Metal precursorsCu(acetate)2 . H2O
Linker precursorsHOBt
Solventshot water; ethanol
Additivesnone stated
Atmospherenot stated
Temperaturereflux; hot water used
Time0.5 h reflux; 2 months slow evaporation
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upbrown-green [Cu(OBt)2(H2O)2] precipitate filtered off; filtrate left for slow evaporation
Activationnone stated
Scalability context20% crystal yield after 2 months slow evaporation; no atmosphere or full isolation/drying details for crystals.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(acetate)2 . H2O0.495 g, 2.48 mmol3528 / rendered p003 · 2.3.1
LinkerHOBt0.67 g, 4.96 mmol3528 / rendered p003 · 2.3.1
Solventhot water20 ml3528 / rendered p003 · 2.3.1
Solventethanol25 ml3528 / rendered p003 · 2.3.1
Partial recipeSource: Main

Route 2: Other

3528 / rendered p003 · 2.3.2

Metal precursorsCu(NO3)2 . H2O
Linker precursorshydroxybenzotriazole / HOBt
Solventsethanol; water
Additivesnone stated
Atmospherenot stated
Temperatureroom temperature implied for slow evaporation; not explicitly stated
Time1 week slow evaporation
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upmixture left for slow evaporation; light olive-green needles obtained
Activationnone stated
Scalability context30% yield after one week; no explicit drying/workup or atmosphere stated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2 . H2O0.135 g, 1 mmol3528 / rendered p003 · 2.3.2
Linkerhydroxybenzotriazole0.137 g, 1 mmol3528 / rendered p003 · 2.3.2
Solventethanolnot stated3528 / rendered p003 · 2.3.2
Solventwaternot stated3528 / rendered p003 · 2.3.2
Partial recipeSource: Main

Route 3: Other

3528 / rendered p003 · 2.3.6

Metal precursorsCoCl2 . 6H2O
Linker precursorsHOBt
Solventsethanol; absolute ethanol
Additivesnone stated
Atmospherenot stated
Temperaturesame as above; room temperature implied
Timesame as above; 2 h implied
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upreaction mixture treated as above; pale pink solid isolated
Activationas above: dried in vacuo over anhydrous calcium chloride
Scalability context0.32 g, 16% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoCl2 . 6H2O0.235 g, 1.48 mmol3528 / rendered p003 · 2.3.6
LinkerHOBt0.40 g, 2.96 mmol3528 / rendered p003 · 2.3.6
Solventethanol25 ml · metal solution3528 / rendered p003 · 2.3.6
Solventabsolute ethanol25 ml · HOBt solution3528 / rendered p003 · 2.3.6
Partial recipeSource: Main

Route 4: Other

3528 / rendered p003 · 2.3.8

Metal precursorsCu(CH3COO)2 . H2O
Linker precursorsHOBt; glycine
Solventshot water; absolute ethanol; ethanol/DMF recrystallisation
Additivesglycine as co-ligand
Atmospherenot stated
Temperature70 deg C stirring; hot water additions
Time0.5 h before glycine addition; later stirring time not stated
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upprecipitated complex filtered, washed with water and ethanol, dried over anhydrous calcium chloride, recrystallised from ethanol/DMF
Activationdried over anhydrous calcium chloride
Scalability context0.35 g, 32% yield.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2 . H2O0.998 g, 5.00 mmol3528 / rendered p003 · 2.3.8
LinkerHOBt0.675 g, 5.00 mmol3528 / rendered p003 · 2.3.8
Additiveglycine0.375 gm, 5.00 mmol3528 / rendered p003 · 2.3.8
Solventhot water10 ml + 10 ml3528 / rendered p003 · 2.3.8
Solventabsolute ethanol25 ml3528 / rendered p003 · 2.3.8
Partial recipeSource: Main

Route 5: Other

3528 / rendered p003 · 2.3.3

Metal precursorsCu(CH3COO)2 . H2O or Cu(NO3)2 . 3H2O
Linker precursorsHOBt
Solventsethanol; absolute ethanol; ethanol/DMF recrystallisation
Additivesnone stated
Atmospherenot stated
Temperature70 deg C stirring; reduced in volume; slow evaporation
Timenot stated for slow evaporation/recrystallisation
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upprecipitated complex filtered, washed with water and ethanol, dried over anhydrous calcium chloride, recrystallised from ethanol/DMF
Activationdried over anhydrous calcium chloride
Scalability context0.37 g, 34% yield; time for evaporation/recrystallisation not stated.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(CH3COO)2 . H2O0.296 g, 1.48 mmol3528 / rendered p003 · 2.3.3
Metal SourceCu(NO3)2 . 3H2O0.358 g, 1.48 mmol · alternative3528 / rendered p003 · 2.3.3
LinkerHOBt0.4 g, 2.96 mmol3528 / rendered p003 · 2.3.3
Solventethanol25 ml for metal solution3528 / rendered p003 · 2.3.3
Solventabsolute ethanol25 ml for HOBt solution3528 / rendered p003 · 2.3.3
Solventethanol/DMFnot stated · recrystallisation3528 / rendered p003 · 2.3.3
Partial recipeSource: Main

Route 6: Other

3528 / rendered p003 · 2.3.4

Metal precursorsCuCl2 . 2H2O
Linker precursorsHOBt
Solventsethanol; absolute ethanol; ethanol/DMF recrystallisation
Additivesnone stated
Atmospherenot stated
Temperatureroom temperature
Time2 h stirring
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upprecipitated complex filtered, washed with water and ethanol, dried in vacuo over anhydrous calcium chloride, recrystallised from ethanol/DMF
Activationdried in vacuo over anhydrous calcium chloride
Scalability context0.36 g, 28% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuCl2 . 2H2O0.252 g, 1.48 mmol3528 / rendered p003 · 2.3.4
LinkerHOBt0.40 g, 2.96 mmol3528 / rendered p003 · 2.3.4
Solventethanol25 ml · metal solution3528 / rendered p003 · 2.3.4
Solventabsolute ethanol25 ml · HOBt solution3528 / rendered p003 · 2.3.4
Partial recipeSource: Main

Route 7: Other

3528 / rendered p003 · 2.3.5

Metal precursorsNiCl2 . 6H2O
Linker precursorsHOBt
Solventsethanol; absolute ethanol
Additivesnone stated
Atmospherenot stated
Temperaturesame as Cu chloride route; room temperature implied
Timesame as above; 2 h implied
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upreaction mixture treated as above; blue solid isolated
Activationas above: dried in vacuo over anhydrous calcium chloride
Scalability context0.35 g, 45% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2 . 6H2O0.352 g, 1.48 mmol3528 / rendered p003 · 2.3.5
LinkerHOBt0.40 g, 2.96 mmol3528 / rendered p003 · 2.3.5
Solventethanol25 ml · metal solution3528 / rendered p003 · 2.3.5
Solventabsolute ethanol25 ml · HOBt solution3528 / rendered p003 · 2.3.5
Partial recipeSource: Main

Route 8: Other

3528 / rendered p003 · 2.3.7

Metal precursorsZnCl2
Linker precursorsHOBt
Solventsethanol; absolute ethanol
Additivesnone stated
Atmospherenot stated
Temperaturesame as above; room temperature implied
Timesame as above; 2 h implied
Substrate orientationnot applicable
Oxidant / reductantnone stated
Work-upreaction mixture treated similarly as above; white solid isolated
Activationas above: dried in vacuo over anhydrous calcium chloride
Scalability context0.38 g, 33% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZnCl20.202 g, 1.48 mmol3528 / rendered p003 · 2.3.7
LinkerHOBt0.40 g, 2.96 mmol3528 / rendered p003 · 2.3.7
Solventethanol25 ml · metal solution3528 / rendered p003 · 2.3.7
Solventabsolute ethanol25 ml · HOBt solution3528 / rendered p003 · 2.3.7