cMOF Evidence Base

Synthesis evidence

Two 3D supramolecular polymers constructed from an amino acid and a high-nuclear Ln6Cu24 cluster node

Zhang J.-J., Sheng T.-L., Hu S.-M. et al. · Chemistry - A European Journal · 2004 · 3963-3969

2 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

3968 · Experimental Section - Synthesis of the complexes

Metal precursorsNd(ClO4)3.6H2O substituted for Sm source; Cu(ClO4)2.6H2O as in complex 1
Linker precursorsL-proline substituted for glycine
SolventsWater, as in complex 1
Additives0.1 M NaOH to adjust pH to about 6.6, as in complex 1; phosphorus pentaoxide desiccant
AtmosphereNot specified
Temperature50 during two stirring stages by analogy to route 1; subsequent desiccator crystallisation temperature not specified
Timeabout 2 h before Cu addition plus about 2 h after Cu addition by analogy to route 1; crystallisation duration not separately specified
Work-upSame procedure as complex 1; filtered and crystallised in a phosphorus-pentaoxide desiccator by analogy.
ActivationNo post-synthetic activation reported.
Scalability contextYield reported as 0.23 g, 17.3%; no scale-up information.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNd(ClO4)3.6H2Onot restated; used in place of Sm(ClO4)3.6H2O in the same procedure as 13968 · Experimental Section - Synthesis of the complexes
Metal SourceCu(ClO4)2.6H2Oas in route 1, 2 g, 6 mmol by stated same procedure3968 · Experimental Section - Synthesis of the complexes
LinkerL-prolinenot restated; used in place of glycine in the same procedure as 13968 · Experimental Section - Synthesis of the complexes
SolventH2Oas in route 13968 · Experimental Section - Synthesis of the complexes
BaseNaOH solutionas in route 1, slow addition to pH about 6.6 · 0.1 M3968 · Experimental Section - Synthesis of the complexes
Additivephosphorus pentaoxideas in route 1, desiccator filled with phosphorus pentaoxide3968 · Experimental Section - Synthesis of the complexes
Complete recipeSource: Main

Route 2: Other

3968 · Experimental Section - Synthesis of the complexes

Metal precursorsSm(ClO4)3.6H2O (0.557 g, 1 mmol); Cu(ClO4)2.6H2O (2 g, 6 mmol)
Linker precursorsGlycine (0.3 g, 4 mmol)
SolventsWater, 10 mL aqueous lanthanide solution
Additives0.1 M NaOH to adjust pH to about 6.6; phosphorus pentaoxide desiccant
AtmosphereNot specified
Temperature50 during two stirring stages; subsequent desiccator crystallisation temperature not specified
Timeabout 2 h before Cu addition plus about 2 h after Cu addition; about one month crystallisation
Work-upFiltered and placed in a desiccator filled with phosphorus pentaoxide; blue crystals obtained about one month later.
ActivationNo post-synthetic activation reported.
Scalability contextYield reported as 0.27 g, 21.7%; no scale-up information.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceSm(ClO4)3.6H2O0.557 g, 1 mmol3968 · Experimental Section - Synthesis of the complexes
Metal SourceCu(ClO4)2.6H2O2 g, 6 mmol3968 · Experimental Section - Synthesis of the complexes
LinkerGlycine0.3 g, 4 mmol3968 · Experimental Section - Synthesis of the complexes
SolventH2O10 mL aqueous solution3968 · Experimental Section - Synthesis of the complexes
BaseNaOH solutionslow addition to pH about 6.6, repeated after Cu source addition · 0.1 M3968 · Experimental Section - Synthesis of the complexes
Additivephosphorus pentaoxidedesiccator filled with phosphorus pentaoxide3968 · Experimental Section - Synthesis of the complexes