ChemCatChem
10.1002/cctc.201601424
FULL PAPER
between the incident X-rays and the analyzer is 58°. The detection angle
of the photoelectrons is 30°.
The authors gratefully acknowledge financial support from the
Centre National de Recherche Scientifique (CNRS). RB and SS
thank the Université Lille 1, the Nord Pas de Calais region. S.S
thanks the Institut Universitaire de France (IUF) for financial
support.
Zeta potential measurements were performed with a Zetasizer Nano ZS
(
Malvern Instruments S.A., Worcestershire, U.K). The pH of all the
samples was maintained at ~7.
Vibrational spectroscopy data were obtained using a Bruker-Tensor 27 FT-
IR spectrometer with the OPUS Data Collection Program for the analysis.
Keywords: catechol ligand, immobilized catalysts, diamond
The gas chromatography measurements were performed on
Hewlett_Packard HP 5 (l = 30 m, i.d. = 0.32 mm, film thickness = 0.25 µm),
equipped with a FID detector (N as carrier gas (1.6 mL/min); temperature
a
nanoparticles, hydrogenation, rhodium complex
2
[
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program: 80 °C for 1 min then 10 °C/min to 250 °C).
ICP-OES was performed on a Thermo Fisher Scientific iCAP 6300. For the
calibration curve, solutions at different concentrations of rhodium were
prepared form a commercial ICP standard solution of Rh at 1000 µg/mL in
2
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% nitric acid aqueous solution.
1
402.
1H and 31P NMR spectra were recorded with a 400 MHz spectrometer fitted
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with a 5 mm BBFO probe (Larmor frequencies of 400.16 MHz and 161.99
MHz for H and 31P, respectively). The temperature was set to 303 K. 1
and 13C NMR spectra were recorded on a 500 MHz spectrometer fitted
with a 5mm i.d. 13C/1H cryoprobe (Larmor frequency of 500.13 MHz and
[
1
H
[
[
[
25.76 MHz for H and 13C, respectively. The temperature was set to 303
1
1
2
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ppm for 1H MeOD and 49.00 ppm for 13C MeOD). Two-dimensional
heteronuclear correlation 1H-13C (edited HSQC) and 1H-31P (HMQC)
spectra were recorded using standard Bruker pulse programs.
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1
performed on a Bruker Avance III spectrometer operating at 9.4 T ( H and
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31P Larmor frequencies of 400 and 161.9 MHz, respectively) using a 4 mm
double-resonance MAS probe. 31P quantitative MAS spectra were
recorded using a pulse length of 3 µs (90° flip angle) and a recycle delay
[
[
[
of 20 s allowing avoiding saturation effects. { H}-31P cross-polarization
1
CP) MAS spectra were recorded with H and 31P nutation frequencies of
1
(
7
0 and 56 kHz during a CP contact time of 0.5 ms and using a recycle
[
[
[
[
delay of 0.5 s. The 31P 2D homonuclear J-resolved spectra of the
functionalized ND and ND-Rh particles were recorded using a CP spin-
echo sequence with a spinning frequency of 14 kHz. 52 rotor-synchronized
t
1
time increments of 428 µs were acquired with 1024 transients each. The
2
D homonuclear though-bond correlation spectrum was recorded using
the refocused-INADEQUATE pulse sequence.[64,65] The DQ excitation and
reconversion periods were set to 857 µs corresponding to 12 rotor periods.
2
2
1
4 rotor-synchronized t time increments of 71.4 µs were acquired with
[
048 transients each. For all experiments, 1H SPINAL-64[66] decoupling
[
[
[
[
(
radio-frequency field strength of 70 kHz) was applied during signal
acquisition, as well as during the incremented t
spectra.
1
evolution period of the 2D
2 3
Thermogravimetric measurements (TGA) were made in Al O crucibles in
an atmosphere of nitrogen at a heating rate of 10 °C min-1 using a TA
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Instruments Q50 thermogravimetric analyzer.
[
The particle size of the ND suspensions was measured at 25 °C using a
Zetasizer Nano ZS (Malvern Instruments S.A., Worcestershire, U.K.) in
[
1
73° scattering geometry, and the zeta potential was measured using the
electrophoretic mode.
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Acknowledgements
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