Supporting Information for Low Temperature Synthesis of CoO Nanoparticles via Chemically Assisted Oxidative Decarbonylation
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1 Supporting Information for Low Temperature Synthesis of CoO Nanoparticles via Chemically Assisted Oxidative Decarbonylation Anna Lagunas, a Antoni Mairata i Payeras, a,b Ciril Jimeno, a Víctor F. Puntes c,d and Miquel A. Pericàs,*,a,b Institute of Chemical Research of Catalonia (ICIQ). Avga. Països Catalans 16, Tarragona (Spain), Departament de Química Orgànica, Universitat de Barcelona, Barcelona (Spain), Institut Català de Nanotecnologia (ICN), Campus de Bellaterra, E Bellaterra (Spain), and ICREA. Fax: (+34) mapericas@iciq.es 1. TEM micrographs of CoO nanoparticles...s2 2. React-IR setup for decarbonylation in situ monitoring...s2 3. XPS of CoO nanoparticles...s3 4. EELS of CoO nanoparticles...s4 5. Hysteresis loops of CoO nanoparticles...s5 6. Inverse of magnetisation vs. Temperature at high external field for CoO nanoparticles...s6 7. Cartesian coordinates, heats of formation (PM3), electronic energies (B3LYP/LACVP), and imaginary frequencies (for transition states, PM3) of relevant structures in the theoretical study of the oxidation of Co to CoO by amine oxides...s7 S1
2 1. TEM micrographs of CoO nanoparticles agregates obtained using (a) NMO, (b) PPNO and (c) DMONO. Insets, their respective SAED patterns and TEM magnifications. 2. React-IR setup for monitoring the decarbonylation of Co 2 (CO) 8. Articulated arm Probe React-IR Reaction vessel S2
3 3. XPS of CoO nanoparticles. For DMONO: ev ev ev ev For PPNO: Binding energy / ev ev ev ev ev Binding energy / ev S3
4 4. EELS of CoO nanoparticles. For NMO, at r.t. and aging at 50ºC for 1 h: For DMONO, at -10ºC: S4
5 5. Hysteresis loops of CoO nanoparticles at 2 K. (a) with PPNO: M (emu*g -1 ) H (Oe) (b) with DMONO: M (emu*g -1 ) H (Oe) S5
6 6. Inverse of magnetisation vs. temperature at high external field (1 Tesla). (a) PPNO, (b) NMO, (c) DMONO. S6
7 7. Cartesian coordinates, heats of formation (PM3), electronic energies (B3LYP/LACVP), and imaginary frequencies (for transition states, PM3) of relevant structures in the theoretical study of the oxidation of Co to CoO by amine oxides Trimethylamine oxide 1 N N O O C C H H H H H H C C H H H H H H C C H H H H H H Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees Trimethylamine 1 N N C C H H H H H H C C H H H H H H C C H H H H H H S7
8 Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees Co 2 (CO) 7 1 Co Co Co Co C C C C O O O O C C O O C C O O C C O O C C O O C C O O Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees Co 2 O(CO) 7 1 Co Co Co Co C C C C O O O O C C O O C C O O S8
9 11 C C O O C C O O C C O O O O Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees Co 2 O(CO) 7 TMAO-ax 1 Co Co Co Co C C C C O O O O C C O O C C O O C C O O C C O O C C O O O O N N C C H H H H H H C C H H H H H H C C H H H H H H S9
10 Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees TS N-O cleavage-ax 1 Co Co Co Co C C C C O O O O C C O O C C O O C C O O C C O O C C O O O O N N C C H H H H H H C C H H H H H H C C H H H H H H Imaginary frequency (PM3): cm -1 Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees S10
11 Co 2 O(CO) 7 TMAO-eq 1 Co Co Co Co C C C C O O O O C C O O C C O O C C O O C C O O C C O O O O N N C C H H H H H H C C H H H H H H C C H H H H H H Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees S11
12 TS N-O cleavage-eq 1 Co Co Co Co C C C C O O O O C C O O C C O O C C O O C C O O C C O O O O N N C C H H H H H H C C H H H H H H C C H H H H H H Imaginary frequency (PM3): cm -1 Heat of formation (PM3): kcal/mol SCF total energy (B3LYP): hartrees S12
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Spain c Departament de Química Orgànica, Universitat de Barcelona, c/ Martí I Franqués 1-11, 08080, Barcelona, Spain.
a Institute of Chemical Research of Catalonia, Av. Països Catalans, 16, 43007 Tarragona, Spain. b Departament de Química, Universitat Autònoma de Barcelona, Cerdanyola del Vallès, E-08193 Barcelona, Spain
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H C Si 2.492 (2.348) 1.867 (2.005) Fe O 2.106 (2.077) 2.360 (2.497) N 1.126 (1.115) 2.105 (2.175) I quintet (triplet) 0.0 (+4.1) kcal/mol II triplet (quintet) 0.0 (+4.3) kcal/mol 1.857 (2.076) 2.536 (2.351)
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