Synthesis evidence

Ruthenium(II) complex-grafted conductive metal-organic frameworks with conductivity- and confinement-enhanced electrochemiluminescence for ultrasensitive biosensing application

Zhang J.-L., Gao S., Yang Y. et al. · Biosensors and Bioelectronics · 2023 · 115157

7 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

SI text · S-3.2 Synthesis of Co3(HITP)2

Metal precursorsCobalt(II) nitrate hexahydrate, Co(NO3)2.6H2O, 162.7 mg (0.56 mmol)
Linker precursorsHATP.6HCl, 30 mg (0.056 mmol)
Solvents9 mL DMF for cobalt salt; 9 mL water for HATP; 12 mL aqueous NaOAc
AdditivesNaOAc aqueous solution, 2 mol L-1, 12 mL
AtmosphereOpen beaker; atmosphere not otherwise specified
Temperature65
Time2
Work-upCentrifuged; washed with ultrapure water and methanol.
ActivationDried under vacuum at 60 deg C.
Scalability context20 mL open beaker batch.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt(II) nitrate hexahydrate (Co(NO3)2.6H2O)162.7 mg (0.56 mmol)SI text · S-3.2 Synthesis of Co3(HITP)2
LinkerHATP.6HCl30 mg (0.056 mmol)SI text · S-3.2 Synthesis of Co3(HITP)2
SolventDMF9 mLSI text · S-3.2 Synthesis of Co3(HITP)2
Solventwater9 mLSI text · S-3.2 Synthesis of Co3(HITP)2
BaseNaOAc aqueous solution12 mL · 2 mol L-1SI text · S-3.2 Synthesis of Co3(HITP)2
Complete recipeSource: SI

Route 2: Other

SI text · S-3.1 Synthesis of Cu3(HITP)2

Metal precursorsCopper(II) sulfate pentahydrate, CuSO4.5H2O, 21 mg (0.084 mmol)
Linker precursorsHATP.6HCl, 30 mg (0.056 mmol)
Solvents9 mL DMA for copper salt; 9 mL water for HATP; 12 mL aqueous NaOAc
AdditivesNaOAc aqueous solution, 2 mol L-1, 12 mL
AtmosphereOpen beaker; atmosphere not otherwise specified
Temperature65
Time2
Work-upCentrifuged; washed with ultrapure water and methanol.
ActivationDried under vacuum at 60 deg C.
Scalability context20 mL open beaker batch.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) sulfate pentahydrate (CuSO4.5H2O)21 mg (0.084 mmol)SI text · S-3.1 Synthesis of Cu3(HITP)2
LinkerHATP.6HCl30 mg (0.056 mmol)SI text · S-3.1 Synthesis of Cu3(HITP)2
SolventDMA9 mLSI text · S-3.1 Synthesis of Cu3(HITP)2
Solventwater9 mLSI text · S-3.1 Synthesis of Cu3(HITP)2
BaseNaOAc aqueous solution12 mL · 2 mol L-1SI text · S-3.1 Synthesis of Cu3(HITP)2
Complete recipeSource: Main

Route 3: Drop Cast

p003 · 2.3 Construction of the ECL sensing platform · Scheme 1B

Metal precursorsRu@Ni3(HITP)2 dispersion; AuNP dispersion
Linker precursorsTB aptamer; Fc-S1; hexanethiol blocking reagent
SolventsWater/PBS-related electrode rinsing; HT in ethanol
AdditivesAuNPs, hexanethiol, Fc-S1, Exo I, TB analyte
AtmosphereAmbient laboratory atmosphere implied; not specified
Temperature4; 37
Timeovernight aptamer incubation; 0.667 h HT blocking; 2 h Fc-S1; 2.5 h TB/Exo I
Substrate orientationClean glass carbon electrode
Work-upAfter every modified step, each electrode was gently rinsed with ultrapure water.
Scalability contextElectrode-scale biosensor fabrication.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
OtherRu@Ni3(HITP)2 dispersion12 uL · 1 mg/mLp003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
OtherAuNPs dispersion10 uLp003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
Otherprepared thrombin aptamer, HS-(CH2)6-TTGGTTGGTGTGGTTGG10 uLp003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
Additivehexanethiol (HT) in ethanol10 uL · 1.0 mMp003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
OtherFc-S1, CCAACCACACCAACC-Fc10 uL · 2 uMp003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
OtherExo I10 Up003 · 2.3 Construction of the ECL sensing platform · Scheme 1B
Complete recipeSource: Main

Route 4: Other

p002 · 2.1 Synthesis of Ni3(HITP)2

Metal precursorsNickel acetate tetrahydrate, Ni(OAc)2.4H2O, 20.85 mg (0.084 mmol)
Linker precursorsHATP.6HCl, 30 mg (0.056 mmol)
Solvents9 mL DMSO for Ni salt; 9 mL water for HATP; 12 mL aqueous NaOAc
AdditivesNaOAc aqueous solution, 4 mol L-1, 12 mL
AtmosphereNot specified
Temperature65
Time2
Work-upCentrifuged; washed with ultrapure water and methanol.
ActivationDried in vacuum at 60 deg C.
Scalability contextSmall-scale batch using tens of mg precursors.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate (Ni(OAc)2.4H2O)20.85 mg (0.084 mmol)p002 · 2.1 Synthesis of Ni3(HITP)2
LinkerHATP.6HCl30 mg (0.056 mmol)p002 · 2.1 Synthesis of Ni3(HITP)2
SolventDMSO9 mLp002 · 2.1 Synthesis of Ni3(HITP)2
Solventwater9 mLp002 · 2.1 Synthesis of Ni3(HITP)2
BaseNaOAc aqueous solution12 mL · 4 mol L-1p002 · 2.1 Synthesis of Ni3(HITP)2
Complete recipeSource: SI

Route 5: Other

SI text · S-3.3

Metal precursorsCo3(HITP)2 host; Ru(H2dcbpy)Cl2, 13.7 mg
Linker precursorsRu bpydc complex precursor
Solvents20 mL DMF
AtmosphereNot specified
Temperature60
Time36
Work-upCentrifuged and washed with DMF and ultrapure water.
ActivationDried under vacuum at 60 deg C.
Scalability context20 mg host-MOF scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo3(HITP)220 mgSI text · S-3.3
Metal SourceRu(H2dcbpy)Cl213.7 mgSI text · S-3.3
SolventDMF20 mLSI text · S-3.3
Complete recipeSource: SI

Route 6: Other

SI text · S-3.3

Metal precursorsCu3(HITP)2 host; Ru(H2dcbpy)Cl2, 13.3 mg
Linker precursorsRu bpydc complex precursor
Solvents20 mL DMF
AtmosphereNot specified
Temperature60
Time36
Work-upCentrifuged and washed with DMF and ultrapure water.
ActivationDried under vacuum at 60 deg C.
Scalability context20 mg host-MOF scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HITP)220 mgSI text · S-3.3
Metal SourceRu(H2dcbpy)Cl213.3 mgSI text · S-3.3
SolventDMF20 mLSI text · S-3.3
Complete recipeSource: Main

Route 7: Other

p003 · 2.2 Synthesis of Ru@Ni3(HITP)2

Metal precursorsNi3(HITP)2 host; Ru(H2dcbpy)Cl2, 13.6 mg
Linker precursorsRu bpydc complex precursor, reported as Ru(H2dcbpy)Cl2 / [Ru(H2bpydc)3]Cl2
Solvents20 mL DMF
AtmosphereNot specified
Temperature60
Time36
Work-upCentrifuged and washed with DMF and ultrapure water.
ActivationDried under vacuum at 60 deg C.
Scalability context20 mg host-MOF scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi3(HITP)220 mgp003 · 2.2 Synthesis of Ru@Ni3(HITP)2
Metal SourceRu(H2dcbpy)Cl213.6 mgp003 · 2.2 Synthesis of Ru@Ni3(HITP)2
SolventDMF20 mLp003 · 2.2 Synthesis of Ru@Ni3(HITP)2