Other — A Mixed Heterobimetallic Y/Eu-MOF for the Cyanosilylation and Hydroboration of Carbonyls

9 measurement groups · 73 results

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

catalytic cyanosilylation; conversion by 1H NMR

Nuclear magnetic resonance

Y/Eu-MOF crystalline catalyst · Single Crystal

Y/Eu-MOF 0.5 mol%, carbonyl compound 0.25 mmol, TMSCN 34 uL/0.275 mmol/1.1 equiv, solvent-free, room temperature, N2, 24 h unless otherwise noted.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: 5, 7-8 · 2.4 Study of Catalytic Activity; 3.2 · Scheme 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
cyanosilylation conversion 2aMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 2b	89%	—	—	Visual Estimate Exact Reported	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 2cMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 2dMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 2eMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3aMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3b	77%	—	—	Visual Estimate Exact Reported	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3c	74%	—	—	Visual Estimate Exact Reported	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3d	91%	—	—	Visual Estimate Exact Reported	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3e	94%	—	—	Visual Estimate Exact Reported	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3fMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation conversion 3gMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
cyanosilylation aldehyde conversion range	89-99% after 24 h	—	range 89-99	Text Range	5 · 2.4 Study of Catalytic Activity · Scheme 1
blank cyanosilylation conversion	8% conversion after 14 h	—	—	Text Exact Reported	5 · 2.4 Study of Catalytic Activity

green chemistry metric calculation

Y/Eu-MOF crystalline catalyst · Single Crystal

Atomic economy, mass intensity, reaction mass efficiency, and carbon efficiency calculated for cyanosilylation and hydroboration.

Context: pristine mixed-metal framework catalyst
Measurement source: S32 · 17. Green chemistry metrics · Table S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
cyanosilylation atom economy	100%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
cyanosilylation carbon efficiency	96.8%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
cyanosilylation mass intensity	1.127	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
cyanosilylation reaction mass efficiency	95.7%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
hydroboration atom economy	49.1%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
hydroboration carbon efficiency	52.1%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
hydroboration mass intensity	2.406	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9
hydroboration reaction mass efficiency	46.8%	—	—	SI Table Exact Reported	S32 · 17. Green chemistry metrics · Table S9

1H and 11B NMR hidden-boron catalysis controls

Nuclear magnetic resonance

Y/Eu-MOF crystalline catalyst · Single Crystal

Monitored Y/Eu-MOF plus HBpin under catalytic conditions; also tested acetophenone hydroboration with BH3.THF instead of HBpin.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: 6 · 2.4 Study of Catalytic Activity

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
acetophenone conversion with BH3.THF control	no substrate conversion	—	—	Text Qualitative	6 · 2.4 Study of Catalytic Activity
BH3 signal under catalytic conditions	no BH3 signals observed	—	—	Text Qualitative	6 · 2.4 Study of Catalytic Activity

hydroboration condition optimisation by 1H NMR conversion

Nuclear magnetic resonance

Y/Eu-MOF crystalline catalyst · Single Crystal

Acetophenone 28 uL/0.25 mmol and HBPin 40 uL/0.275 mmol in 0.5 mL solvent or solvent-free, room temperature, N2, 24 h.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: S23 · 12. Optimization of the hydroboration reaction conditions · Table S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
hydroboration optimisation best conversionMarked as a best value within this paper	0.5 mol% Y/Eu-MOF, no solvent, 95%	—	—	SI Table Exact Reported	S23 · 12. Optimization of the hydroboration reaction conditions · Table S8
hydroboration optimisation entry 1 conversion	0.35 mol% Y/Eu-MOF, no solvent, 71%	—	—	SI Table Exact Reported	S23 · 12. Optimization of the hydroboration reaction conditions · Table S8
hydroboration optimisation THF conversion	0.35 mol% Y/Eu-MOF, THF, 25%	—	—	SI Table Exact Reported	S23 · 12. Optimization of the hydroboration reaction conditions · Table S8

catalytic hydroboration; conversion/yield by 1H NMR

Nuclear magnetic resonance

Y/Eu-MOF crystalline catalyst · Single Crystal

Y/Eu-MOF 0.5 mol%, ketone 0.25 mmol, HBpin 40 uL/0.275 mmol/1.1 equiv, solvent-free, room temperature, N2; hydrolysis with 0.1 M NaOH and Et2O.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: 5-6, 8 · 2.4 Study of Catalytic Activity; 3.2 · Scheme 2; Table S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
hydroboration conversion 4a	95%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4b	67%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4c	45%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4d	71%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4e	80%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4f	90%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4g	77%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4h	71%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4i	88%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4jMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4kMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4l	<5%	—	upper bound	Visual Estimate Range	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4mMarked as a best value within this paper	>99%	—	lower bound	Visual Estimate Range	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4n	95%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4o	61%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2
hydroboration conversion 4p	63%	—	—	Visual Estimate Exact Reported	6 · 2.4 Study of Catalytic Activity · Scheme 2

catalyst recyclability and leaching test

Y/Eu-MOF crystalline catalyst · Single Crystal

Recovered catalyst by centrifugation, washed with dichloromethane, dried under vacuum, reused; leaching test on hydroboration filtrate.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: S28-S30 · 14. Catalyst Recyclability; 15. Leaching test · Schemes S1-S3; Figure S10

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
leaching test product after first cycle	38% of product 4j	—	—	Text Exact Reported	S30 · 15. Leaching test · Scheme S3
leaching test product after second cycle	13% of product 4j	—	—	Text Exact Reported	S30 · 15. Leaching test · Scheme S3
cyanosilylation conversion after first reuse cycle	28%	—	—	Text Exact Reported	7 · 2.5 Recyclability and Leaching Studies · Figure S10 referenced
cyanosilylation conversion after second reuse cycle	0%	—	—	Text Exact Reported	7 · 2.5 Recyclability and Leaching Studies · Figure S10 referenced
cyanosilylation recyclability initial run conversionMarked as a best value within this paper	99%	—	—	Figure Axis Rounded Reported	S29 · 14. Catalyst Recyclability · Figure S10
hydroboration conversion after first reuse cycle	61%	—	—	Text Exact Reported	7 · 2.5 Recyclability and Leaching Studies · Figure S10 referenced
hydroboration conversion after second reuse cycle	15%	—	—	Text Exact Reported	7 · 2.5 Recyclability and Leaching Studies · Figure S10 referenced
hydroboration recyclability initial run conversionMarked as a best value within this paper	95%	—	—	Figure Axis Rounded Reported	S29 · 14. Catalyst Recyclability · Figure S10

turnover frequency analysis

Y/Eu-MOF crystalline catalyst · Single Crystal

TOF for cyanosilylation and hydroboration of acetophenone using Y/Eu-MOF 0.5 mol% under optimised conditions.

Atmosphere: N2
Context: pristine mixed-metal framework catalyst
Measurement source: S31 · 16. TOF of Y/Eu-MOF · Figures S11-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
best cyanosilylation TOFMarked as a best value within this paper	8.4 h-1 at 7 h	—	—	Figure Axis Rounded Reported	S31 · 16. TOF of Y/Eu-MOF · Figure S11
best hydroboration TOFMarked as a best value within this paper	21 h-1 at 0.5 h	—	—	Figure Axis Rounded Reported	S31 · 16. TOF of Y/Eu-MOF · Figure S12

zeta potential

Dynamic light scattering and zeta potential

Eu-MOF comparison catalyst · Unknown

Eu-MOF comparison plotted with Y/Eu-MOF; constant conductivity 330 uS/cm.

Context: pristine Eu-MOF control
Measurement source: 4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Eu-MOF zeta potential at pH 10Marked as a best value within this paper	-25.0 +/- 0.6 mV	—	+/- 0.6 mV	Text Exact Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 4	2.4 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 5	1.1 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 6	1.3 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 7	6.3 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 8	4.0 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF zeta potential at pH 9	-6.9 mV	—	—	Figure Axis Rounded Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Eu-MOF isoelectric point range	between pH 8 and 9	—	range 8-9	Text Range	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2

zeta potential and electrophoretic mobility

Dynamic light scattering and zeta potential

Y/Eu-MOF crystalline catalyst · Single Crystal

Particles dispersed in water at 0.05% w/w; pH adjusted with NaOH/HCl; sonicated 1 min, sedimented 5 min, conductivity set to 330 uS/cm with 0.1 M NaCl; average of 5 measurements.

Context: pristine mixed-metal framework
Measurement source: S4-S5, S21-S22 · General experimental information; 11. Study of zeta-potential · Figures S7-S9; Table S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
zeta measurement conductivity setpoint	330 uS/cm	—	—	Text Exact Reported	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure S7
Y/Eu-MOF electrophoretic mobility at pH 10Marked as a best value within this paper	-2.252 +/- 0.035 um cm/V s	—	+/- 0.035	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF electrophoretic mobility at pH 4	0.460 +/- 0.032 um cm/V s	—	+/- 0.032	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
NaCl equivalent concentration for conductivity	about 3.7 mM NaCl	—	about	Text Approximate	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure S7
Y/Eu-MOF isoelectric point range	between pH 4 and 5	—	range 4-5	Text Range	4 · 2.3 Chemical Stability and Electrophoretic Behavior · Figure 2
Y/Eu-MOF zeta potential at pH 10Marked as a best value within this paper	-35.8 +/- 0.5 mV	—	+/- 0.5	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF zeta potential at pH 4	5.9 +/- 0.4 mV	—	+/- 0.4	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF zeta potential at pH 5	-1.0 +/- 0.3 mV	—	+/- 0.3	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF zeta potential at pH 6	-5.1 +/- 0.5 mV	—	+/- 0.5	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF zeta potential at pH 7	-6.7 mV	—	+/- 0.6 in Table S7, but sign conflict	Figure Axis Rounded Reported	S21-S22 · 11. Study of zeta-potential · Figure S8; Table S7
Y/Eu-MOF zeta potential at pH 8	-8.5 +/- 0.4 mV	—	+/- 0.4	SI Table Exact Reported	S22 · 11. Study of zeta-potential · Table S7
Y/Eu-MOF zeta potential at pH 9	-18.1 mV	—	+/- 0.3 in Table S7, but sign conflict	Figure Axis Rounded Reported	S21-S22 · 11. Study of zeta-potential · Figure S8; Table S7