Synthesis evidence

Precise tuning of interlayer electronic coupling in layered conductive metal-organic frameworks

Lu Y., Zhang Y., Yang C.-Y. et al. · Nature Communications · 2022 · 7240

5 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

6 · Synthetic procedures

Metal precursorsNi(OAc)2.4H2O (1.5 eq)
Linker precursorsHATI-C1.6HCl / HATI_C1.6HCl, 5 mg (1 eq) in 1.5 mL DMSO
SolventsDMSO/H2O, total 3.5 mL metal/additive solution plus 1.5 mL DMSO ligand solution; reported total ratio DMSO:H2O = 4.5:0.5
AdditivesNaOAc (150 eq)
Atmosphereair/open glass vial; stirred; main Fig. 1b labels Air
Temperature65
Time2
Oxidant / reductantnone reported
Work-upFiltered; washed with large amount of water and acetone; dried under vacuum at room temperature.
ActivationFor gas adsorption: supercritical CO2 drying 4 h then 90 C overnight. For electrical/Seebeck pellets: 150 C under vacuum for 2 h. For TGA: in-situ activation 100 C for 1 h.
Scalability contextSmall-batch recipe reports 5 mg ligand in a 10 mL open vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2.4H2O1.5 eq6 · Synthetic procedures
LinkerHATI-C1.6HCl5 mg; 1 eq · in 1.5 mL DMSO6 · Synthetic procedures
BaseNaOAc150 eq6 · Synthetic procedures
SolventDMSO/H2Ototal ratio DMSO:H2O = 4.5:0.56 · Synthetic procedures
Complete recipeSource: Both

Route 2: Other

6 · Synthetic procedures

Metal precursorsNi(OAc)2.4H2O (1.5 eq)
Linker precursorsHATI-C2.6HCl / HATI_C2.6HCl, 5 mg (1 eq) in 1.5 mL DMSO
SolventsDMSO/H2O, total 3.5 mL metal/additive solution plus 1.5 mL DMSO ligand solution; reported total ratio DMSO:H2O = 3.5:1.5
AdditivesNaOAc (150 eq)
Atmosphereair/open glass vial; stirred; main Fig. 1b labels Air
Temperature65
Time2
Oxidant / reductantnone reported
Work-upFiltered; washed with large amount of water and acetone; dried under vacuum at room temperature.
ActivationFor gas adsorption: supercritical CO2 drying 4 h then 90 C overnight. For electrical/Seebeck pellets: 150 C under vacuum for 2 h. For TGA: in-situ activation 100 C for 1 h.
Scalability contextSmall-batch recipe reports 5 mg ligand in a 10 mL open vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2.4H2O1.5 eq6 · Synthetic procedures
LinkerHATI-C2.6HCl5 mg; 1 eq · in 1.5 mL DMSO6 · Synthetic procedures
BaseNaOAc150 eq6 · Synthetic procedures
SolventDMSO/H2Ototal ratio DMSO:H2O = 3.5:1.56 · Synthetic procedures
Complete recipeSource: Both

Route 3: Other

6 · Synthetic procedures

Metal precursorsNi(OAc)2.4H2O (1.5 eq)
Linker precursorsHATI-C3.6HCl / HATI_C3.6HCl, 5 mg (1 eq) in 1.5 mL DMSO
SolventsDMSO/H2O, total 3.5 mL metal/additive solution plus 1.5 mL DMSO ligand solution; reported total ratio DMSO:H2O = 3:2
AdditivesNaOAc (150 eq)
Atmosphereair/open glass vial; stirred; main Fig. 1b labels Air
Temperature65
Time2
Oxidant / reductantnone reported
Work-upFiltered; washed with large amount of water and acetone; dried under vacuum at room temperature.
ActivationFor gas adsorption: supercritical CO2 drying 4 h then 90 C overnight. For electrical/Seebeck pellets: 150 C under vacuum for 2 h. For TGA: in-situ activation 100 C for 1 h.
Scalability contextSmall-batch recipe reports 5 mg ligand in a 10 mL open vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2.4H2O1.5 eq6 · Synthetic procedures
LinkerHATI-C3.6HCl5 mg; 1 eq · in 1.5 mL DMSO6 · Synthetic procedures
BaseNaOAc150 eq6 · Synthetic procedures
SolventDMSO/H2Ototal ratio DMSO:H2O = 3:26 · Synthetic procedures
Complete recipeSource: Both

Route 4: Other

6 · Synthetic procedures

Metal precursorsNi(OAc)2.4H2O (1.5 eq)
Linker precursorsHATI-C4.6HCl / HATI_C4.6HCl, 5 mg (1 eq) in 1.5 mL DMSO
SolventsDMSO/H2O, total 3.5 mL metal/additive solution plus 1.5 mL DMSO ligand solution; reported total ratio DMSO:H2O = 3:2
AdditivesNaOAc (150 eq)
Atmosphereair/open glass vial; stirred; main Fig. 1b labels Air
Temperature65
Time2
Oxidant / reductantnone reported
Work-upFiltered; washed with large amount of water and acetone; dried under vacuum at room temperature.
ActivationFor gas adsorption: supercritical CO2 drying 4 h then 90 C overnight. For electrical/Seebeck pellets: 150 C under vacuum for 2 h. For TGA: in-situ activation 100 C for 1 h.
Scalability contextSmall-batch recipe reports 5 mg ligand in a 10 mL open vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2.4H2O1.5 eq6 · Synthetic procedures
LinkerHATI-C4.6HCl5 mg; 1 eq · in 1.5 mL DMSO6 · Synthetic procedures
BaseNaOAc150 eq6 · Synthetic procedures
SolventDMSO/H2Ototal ratio DMSO:H2O = 3:26 · Synthetic procedures
Complete recipeSource: Both

Route 5: Other

6 · Synthetic procedures

Metal precursorsNi(OAc)2.4H2O (1.5 eq)
Linker precursorsHATI-C8.6HCl / HATI_C8.6HCl, 5 mg (1 eq) in 1.5 mL DMSO
SolventsDMSO/H2O, total 3.5 mL metal/additive solution plus 1.5 mL DMSO ligand solution; reported total ratio DMSO:H2O = 3:2
AdditivesNaOAc (150 eq)
Atmosphereair/open glass vial; stirred; main Fig. 1b labels Air
Temperature65
Time2
Oxidant / reductantnone reported
Work-upFiltered; washed with large amount of water and acetone; dried under vacuum at room temperature.
ActivationFor gas adsorption: supercritical CO2 drying 4 h then 90 C overnight. For electrical/Seebeck pellets: 150 C under vacuum for 2 h. For TGA: in-situ activation 100 C for 1 h.
Scalability contextSmall-batch recipe reports 5 mg ligand in a 10 mL open vial; no scale-up demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2.4H2O1.5 eq6 · Synthetic procedures
LinkerHATI-C8.6HCl5 mg; 1 eq · in 1.5 mL DMSO6 · Synthetic procedures
BaseNaOAc150 eq6 · Synthetic procedures
SolventDMSO/H2Ototal ratio DMSO:H2O = 3:26 · Synthetic procedures