Other — Synthesis, Characterization, and Catalytic Performance of a New Heterobimetallic Y/Tb Metal-Organic Framework with High Catalytic Activity

Measurement evidence

Other

Synthesis, Characterization, and Catalytic Performance of a New Heterobimetallic Y/Tb Metal-Organic Framework with High Catalytic Activity · Lopez-Vargas M.E., Perez J.M., Echenique-Errandonea E. et al. · ACS Omega · 2024 · 26549-26559

10 measurement groups · 54 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Cyanosilylation catalysis

Tb-MOF bulk catalyst powder/crystals · Powder

Ketone 1 (0.25 mmol) + TMSCN (34 uL, 0.275 mmol, 1.1 equiv); 0.5 mol% Tb-MOF; solvent-free; RT; N2; typically 4 h or 24 h.

Atmosphere
N2
Geometry
1 mL vial
Context
pristine monometallic control
Measurement source
p005 / 26553 · Catalytic Activity · Table 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
cyanosilylation conversion product 2aMarked as a best value within this paper>99Table
Range
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2b(61) after 4 h; 88 after 24 hTable
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2c84 after 4 hTable
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2d91 after 4 hTable
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2e80 after 4 hTable
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2fMarked as a best value within this paper(74) after 4 h; >99 after 24 hTable
Range
p005 / 26553 · Catalytic Activity · Table 1
induction period24Text
Rounded Reported
p005 / 26553 · Catalytic Activity · Figure 4
maximum TOF in acetophenone cyanosilylationMarked as a best value within this paper83 h-1 at 69% conversion after 100 minText
Rounded Reported
p006 / 26554 · Catalytic Activity · Figures S30-S31

Cyanosilylation catalysis

Y/Tb-MOF bulk catalyst powder/crystals · Powder

Ketone 1 (0.25 mmol) + TMSCN (34 uL, 0.275 mmol, 1.1 equiv); 0.5 mol% Y/Tb-MOF; solvent-free; RT; N2; 24 h.

Atmosphere
N2
Geometry
1 mL vial
Context
pristine target framework
Measurement source
p005 / 26553 · Catalytic Activity · Table 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
cyanosilylation conversion product 2aMarked as a best value within this paper>99Table
Range
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2b88Table
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2c86Table
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2d94Table
Exact Reported
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2eMarked as a best value within this paper>99Table
Range
p005 / 26553 · Catalytic Activity · Table 1
cyanosilylation conversion product 2fMarked as a best value within this paper>99Table
Range
p005 / 26553 · Catalytic Activity · Table 1
induction period152Text
Rounded Reported
p005 / 26553 · Catalytic Activity · Figure 4
green metric atom economy for 2a100SI Table
Exact Reported
p049 / S49 · Green chemistry metrics · Table S9
green metric mass intensity for 2a1.1SI Table
Exact Reported
p049 / S49 · Green chemistry metrics · Table S9
maximum TOF in acetophenone cyanosilylationMarked as a best value within this paper17 h-1 at 61% conversion after 7 hText
Rounded Reported
p006 / 26554 · Catalytic Activity · Figures S30-S31

CO2/epoxide cycloaddition catalysis

Tb-MOF bulk catalyst powder/crystals · Powder

Epoxide 4 (0.5 mmol), TBAB 2.5 mol%, Tb-MOF 2.0 mol%; solvent-free unless stated; 5 bar CO2; 100 C; 19 h for scope.

Temperature
373
Atmosphere
CO2
Geometry
reactor vial
Context
pristine monometallic control
Measurement source
p006-p007 / 26554-26555 · Catalytic Activity · Tables 3-4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CO2 cycloaddition conversion product 5bMarked as a best value within this paper87Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4
CO2 cycloaddition conversion product 5c46Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4
CO2 cycloaddition conversion product 5d0Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4

CO2/epoxide cycloaddition catalysis

Y/Tb-MOF bulk catalyst powder/crystals · Powder

Epoxide 4 (0.5 mmol), TBAB 2.5 mol%, Y/Tb-MOF 2.0 mol%; solvent-free unless stated; 5 bar CO2; 100 C; 19 h for scope.

Temperature
373
Atmosphere
CO2
Geometry
reactor vial
Context
pristine target framework
Measurement source
p006-p007 / 26554-26555 · Catalytic Activity · Tables 3-4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
CO2 cycloaddition conversion product 5b65Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4
CO2 cycloaddition conversion product 5c41Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4
CO2 cycloaddition conversion product 5d0Table
Exact Reported
p007 / 26555 · Catalytic Activity · Table 4

Hydroboration catalysis

Tb-MOF bulk catalyst powder/crystals · Powder

Ketone 1 (0.25 mmol) + HBpin (40 uL, 0.275 mmol, 1.1 equiv); 0.5 mol% Tb-MOF; solvent-free; RT; N2; 24 h, then NaOH/Et2O hydrolysis overnight.

Atmosphere
N2
Geometry
1 mL vial
Context
pristine monometallic control
Measurement source
p006 / 26554 · Catalytic Activity · Table 2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
hydroboration conversion product 3a70Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3b75Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3c75Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3d89Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3e81Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3f/3f'Marked as a best value within this paper93Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration TOF upper end of reported range4.2 to 7.4Text
Range
p006 / 26554 · Catalytic Activity · Figures S34-S35

Hydroboration catalysis

Y/Tb-MOF bulk catalyst powder/crystals · Powder

Ketone 1 (0.25 mmol) + HBpin (40 uL, 0.275 mmol, 1.1 equiv); 0.5 mol% Y/Tb-MOF; solvent-free; RT; N2; 24 h, then NaOH/Et2O hydrolysis overnight.

Atmosphere
N2
Geometry
1 mL vial
Context
pristine target framework
Measurement source
p006 / 26554 · Catalytic Activity · Table 2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
hydroboration conversion product 3a91Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3b90Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3c85Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3d60Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3e86Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration conversion product 3f/3f'Marked as a best value within this paper97Table
Exact Reported
p006 / 26554 · Catalytic Activity · Table 2
hydroboration TOF upper end of reported range1.4 to 7.6Text
Range
p006 / 26554 · Catalytic Activity · Figures S34-S35

Leaching test and ICP-MS

recovered Y/Tb-MOF catalyst · Powder

Supernatant after first recyclability cycle filtered through celite, dried, then used for additional cyanosilylation or hydroboration; ICP-MS analysed leached Y/Tb.

Atmosphere
N2
Geometry
filtrate test
Context
recycled target framework
Measurement source
p008 / 26556 · Recyclability and Leaching Studies · Scheme 1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
filtrate cyanosilylation conversion85Text
Rounded Reported
p008 / 26556 · Recyclability and Leaching Studies · Scheme 1
filtrate hydroboration conversion96Text
Rounded Reported
p008 / 26556 · Recyclability and Leaching Studies · Scheme 1
leached Y/Tb ratio cyanosilylation cycle 11.05 (2.21/2.10 ug/L)Text
Exact Reported
p008 / 26556 · Recyclability and Leaching Studies

Catalyst recyclability

recovered Tb-MOF catalyst · Powder

Recovered Tb-MOF catalyst by centrifugation, Et2O washing, vacuum drying and reuse in cyanosilylation.

Atmosphere
N2
Geometry
reused catalyst
Context
recycled monometallic control
Measurement source
p007 / 26555 · Recyclability and Leaching Studies · Figure 5; Figure S27
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Tb-MOF cyanosilylation conversion after first recycle52Text
Rounded Reported
p007 / 26555 · Recyclability and Leaching Studies · Figure 5; Figure S27

Catalyst recyclability

recovered Y/Tb-MOF catalyst · Powder

Recovered catalyst by centrifugation, Et2O washing, vacuum drying and reuse in cyanosilylation, hydroboration, and CO2 cycloaddition.

Atmosphere
N2 or CO2 depending reaction
Geometry
reused catalyst
Context
recycled target framework
Measurement source
p007 / 26555 · Recyclability and Leaching Studies · Figure 5; Figure S27
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
cyanosilylation conversion after first recycle24Text
Rounded Reported
p007 / 26555 · Recyclability and Leaching Studies · Figure 5; Figure S27
CO2 cycloaddition recyclabilityno erosion throughout four tested cyclesText
Qualitative
p007 / 26555 · Recyclability and Leaching Studies · Figure 5
hydroboration conversion after first recycle50Text
Rounded Reported
p007 / 26555 · Recyclability and Leaching Studies · Figure 5
hydroboration conversion after second recycle34Text
Rounded Reported
p007 / 26555 · Recyclability and Leaching Studies · Figure 5

Thermogravimetric analysis (TGA/DTG)

Y/Tb-MOF bulk catalyst powder/crystals · Powder

Inert N2 atmosphere; ambient to ca. 1000 C.

Atmosphere
N2
Context
pristine target framework
Measurement source
p003 / 26551 · Synthesis and Characterization of Catalysts · Figure S12
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
framework-collapse range upper bound438Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
framework-collapse range lower bound252Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
final organic-linker decomposition event521Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
final organic-linker decomposition event712Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
final organic-linker decomposition event941Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
solvent-loss DTG peak72Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
solvent-loss range upper bound177Text
Rounded Reported
p003 / 26551 · Synthesis and Characterization · Figure S12
solvent-loss range lower boundroom temperatureText
Approximate
p003 / 26551 · Synthesis and Characterization · Figure S12