Photomechanochemistry: harnessing mechanical forces to enhance photochemical reactions

• Francesco Mele,
• Ana M. Constantin,
• Andrea Porcheddu,
• Raimondo Maggi,
• Giovanni Maestri,
• Nicola Della Ca’ and
• Luca Capaldo

Beilstein J. Org. Chem. 2025, 21, 458–472, doi:10.3762/bjoc.21.33

• resulted in 40% yield. Alternating grinding and irradiation, the authors managed to obtain quantitative conversion of 2.1 to 2.3. Overall, in this work, mechanochemistry worked akin to agitation provided by stirring or heating in solution. In fact, 1H NMR spectroscopy, XRD and DFT analyses showed that

Synthesis, structure, ionochromic and cytotoxic properties of new 2-(indolin-2-yl)-1,3-tropolones

• Yurii A. Sayapin,
• Eugeny A. Gusakov,
• Inna O. Tupaeva,
• Alexander D. Dubonosov,
• Igor V. Dorogan,
• Valery V. Tkachev,
• Anna S. Goncharova,
• Gennady V. Shilov,
• Natalia S. Kuznetsova,
• Svetlana Y. Filippova,
• Tatyana A. Krasnikova,
• Yanis A. Boumber,
• Alexey Y. Maksimov,
• Sergey M. Aldoshin and
• Vladimir I. Minkin

Beilstein J. Org. Chem. 2025, 21, 358–368, doi:10.3762/bjoc.21.26

• and DFT quantum chemical calculations for 7a, 7b, 8a and 8b. Supporting Information File 14: Crystallographic information file for compound 7b. Acknowledgements XRD studies were performed in accordance with the State Task, State registration № 124013100858-3 (V. V. Tkachev, G. V. Shilov, S. M

Controlled oligomerization of [1.1.1]propellane through radical polarity matching: selective synthesis of SF₅- and CF₃SF₄-containing [2]staffanes

• Jón Atiba Buldt,
• Wang-Yeuk Kong,
• Yannick Kraemer,
• Masiel M. Belsuzarri,
• Ansh Hiten Patel,
• James C. Fettinger,
• Dean J. Tantillo and
• Cody Ross Pitts

Beilstein J. Org. Chem. 2024, 20, 3134–3143, doi:10.3762/bjoc.20.259

• truncated after incorporation of two bicyclopentane (BCP) units. Synthetic and computational studies suggest this phenomenon can be attributed to alternating radical polarity matching. In addition, single-crystal X-ray diffraction (SC-XRD) data reveal structurally interesting features of the CF3SF4

• bicyclopentyl radical philicities. In addition, we demonstrate that similar reaction conditions can be applied to the synthesis of the analogous CF3SF4-containing [2]staffane (CF3SF4-BCP-BCP-Cl, 3). Finally, we examined compound 3 by SC-XRD and found that it undergoes a phase transition as a function of rate of

• for the first time created an opportunity for structural analysis. We previously reported and contextualized single-crystal X-ray diffraction (SC-XRD) data on 2 [36]; thus, we proceeded to grow crystals of 3 suitable for X-ray analysis through slow evaporation of ethyl acetate. To our surprise, an

Structure and thermal stability of phosphorus-iodonium ylids

• Andrew Greener,
• Stephen P. Argent,
• Coby J. Clarke and
• Miriam L. O’Duill

Beilstein J. Org. Chem. 2024, 20, 2931–2939, doi:10.3762/bjoc.20.245

• ][26][27] and the mechanisms by which they decompose when heated through a systematic investigation of structural data from X-ray diffraction (XRD) and thermal stability data from differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The insights from this study will galvanise

• the rational design and synthesis of novel, unstabilised hypervalent iodine(III) compounds and expand the application of these powerful reagents in organic synthesis. Results and Discussion Structural data Twelve phosphorus-iodonium ylids were synthesised (Figure 2). X-ray diffraction data (XRD) of

• compounds 1a–f and 1i were measured (see Supporting Information File 2), and data for compounds 2–4 were sourced from the literature [24][26][28]. A representative set of structural parameters obtained from XRD is presented in Table 1. All compounds show a trigonal bipyramidal structure, in which the 3

Transition-metal-free decarbonylation–oxidation of 3-arylbenzofuran-2(3H)-ones: access to 2-hydroxybenzophenones

• Bhaskar B. Dhotare,
• Seema V. Kanojia,
• Chahna K. Sakhiya,
• Amey Wadawale and
• Dibakar Goswami

Beilstein J. Org. Chem. 2024, 20, 2655–2667, doi:10.3762/bjoc.20.223

• substitution at the 4-position of benzofuranone hindered the reaction, leading to a very poor yield of the desired benzophenone product. Further, to confirm the structure and the substitution pattern in the 2-hydroxybenzophenones, single crystal XRD data were collected for the representative compounds 4ja, 4fb

• -crystal XRD The data were collected using a similar method as reported by us earlier [23], using a XtaLAB Synergy, Dualflex, HyPix four-circle diffractometer, a micro-focus sealed X-ray tube and a HyPix detector. The data were corrected using SCALE3 ABSPACK and the structure were solved using SHELXT

Asymmetric organocatalytic synthesis of chiral homoallylic amines

• Nikolay S. Kondratyev and
• Andrei V. Malkov

Beilstein J. Org. Chem. 2024, 20, 2349–2377, doi:10.3762/bjoc.20.201

• ’-dibromo-BINOL [25]. aAbsolute configuration was confirmed by a single crystal XRD of the corresponding hydrochloride salt. (R)-3,3’-Di(3,5-di(trifluoromethyl)phenyl-BINOL-catalysed asymmetric geranylation and prenylation of dihydroisoquinolines [25]. aAbsolute configuration was established by single

• crystal XRD of the corresponding hydrochloride salt. Microwave-induced one-pot asymmetric allylation of in situ-formed arylimines, catalysed by (R)-3,3’-diphenyl-BINOL. Aldehyde and amine scope [26]. aThe reaction was conventionally heated at 50 °C for 24 hours instead of microwave irradiation. b1.0 equiv

A laterally-fused N-heterocyclic carbene framework from polysubstituted aminoimidazo[5,1-b]oxazol-6-ium salts

• Andrew D. Gillie,
• Matthew G. Wakeling,
• Bethan L. Greene,
• Louise Male and
• Paul W. Davies

Beilstein J. Org. Chem. 2024, 20, 621–627, doi:10.3762/bjoc.20.54

• . Isolated yield of 17:18 with ratios determined from the 1H NMR spectra. Supporting Information Supporting Information File 42: Experimental procedures and characterisation data, additional cyclisation studies, XRD data and NMR spectra of compounds. Acknowledgements The authors gratefully acknowledge

Synthesis of photo- and ionochromic N-acylated 2-(aminomethylene)benzo[b]thiophene-3(2Н)-ones with a terminal phenanthroline group

• Vladimir P. Rybalkin,
• Sofiya Yu. Zmeeva,
• Lidiya L. Popova,
• Irina V. Dubonosova,
• Olga Yu. Karlutova,
• Oleg P. Demidov,
• Alexander D. Dubonosov and
• Vladimir A. Bren

Beilstein J. Org. Chem. 2024, 20, 552–560, doi:10.3762/bjoc.20.47

• were isolated preparatively and fully characterized by IR, 1H, and 13C NMR spectroscopy as well as HRMS and XRD methods. The reverse thermal reaction was catalyzed by protonic acids. N-Acylated compounds exclusively with Fe2+ formed nonfluorescent complexes with a contrast naked-eye effect: a color

Substitution reactions in the acenaphthene analog of quino[7,8-h]quinoline and an unusual synthesis of the corresponding acenaphthylenes by tele-elimination

• Ekaterina V. Kolupaeva,
• Narek A. Dzhangiryan,
• Alexander F. Pozharskii,
• Oleg P. Demidov and
• Valery A. Ozeryanskii

Beilstein J. Org. Chem. 2024, 20, 243–253, doi:10.3762/bjoc.20.24

• 5. As the XRD study of the crystals showed (Figure 3), the molecular and crystal structure of the isolated compound is strongly dominated, on the one hand, by intra- and intermolecular hydrogen bonds with the participation of N, Cl, and O heteroatoms (forming an endless slightly corrugated ribbon

• compounds 5·HBF4 and 8·HBF4 were recrystallized from acetonitrile and subjected to XRD analysis under the same conditions. Selected data obtained are shown in Table 1. As can be seen, in both protonated quinoquinoline systems, an intramolecular hydrogen bond is realized (strongly asymmetric in crystals, but

• between (Supporting Information File 1, Figure S22). Flat dipyridoacenaphthylene cations 8H+ give a denser packing, which, with an interplanar distance of only 3.328 Å, is the closest among all the studied compounds. Conclusion Using single crystal XRD technique, dipyridoacenaphthene tetrafluoroborate

Aldiminium and 1,2,3-triazolium dithiocarboxylate zwitterions derived from cyclic (alkyl)(amino) and mesoionic carbenes

• Nedra Touj,
• François Mazars,
• Guillermo Zaragoza and
• Lionel Delaude

Beilstein J. Org. Chem. 2023, 19, 1947–1956, doi:10.3762/bjoc.19.145

• . Crystallography Crystals of CAAC·CS2 zwitterions 4a and 4c suitable for X-ray diffraction (XRD) analysis were grown by slow diffusion of cyclohexane in a THF solution at 6 °C. Their molecular structures are depicted in Figure 3. The orange-red needles of compound 4a belonged to the trigonal space group, while

• layered with petroleum ether or n-hexane and kept at −18 °C for a few weeks. This procedure successfully afforded single crystals of products 6b and 6e suitable for XRD analysis (Figure 4). Orange prisms of zwitterion 6b belonged to the monoclinic P21/n space group, while the dark red-brown blocks of

Controlling the reactivity of La@C₈₂ by reduction: reaction of the La@C₈₂ anion with alkyl halide with high regioselectivity

• Yutaka Maeda,
• Saeka Akita,
• Mitsuaki Suzuki,
• Michio Yamada,
• Takeshi Akasaka,
• Kaoru Kobayashi and
• Shigeru Nagase

Beilstein J. Org. Chem. 2023, 19, 1858–1866, doi:10.3762/bjoc.19.138

• @C2v-C82(CHClC6H3Cl2) [19] and La@C2v-C82(CBr(CO2Et)2) [23], by single-crystal X-ray diffraction (SC-XRD) analysis. Based on the similarity in the absorption spectra of La@C2v-C82(CHClC6H3Cl2), the addition site of 3a–c was expected to be at the C10 (for the numbering of carbon atoms in La@C2v-C82; see

• 3a was confirmed by the SC-XRD analysis, which showed that the addition site of addendum was indeed at the C10 position of La@C2v-C82 (Figure 5). The La@C2v-C82 anion can act as an electron donor and a nucleophile. To confirm the reaction mechanism, charge density and the p-orbital axis vector (POAV

• , assuming that La@C2v-C82 and the monoadducts have the same absorption coefficients. X-ray crystallography Black crystalline rods of 3a were obtained using the liquid–liquid bilayer diffusion method with 3a in a CS2 solution and an n-hexane solution in a glass tube (⌀ = 7 mm) at room temperature. The SC-XRD

Charge carrier transport in perylene-based and pyrene-based columnar liquid crystals

• Alessandro L. Alves,
• Simone V. Bernardino,
• Carlos H. Stadtlober,
• Edivandro Girotto,
• Giliandro Farias,
• Rodney M. do Nascimento,
• Sergio F. Curcio,
• Thiago Cazati,
• Marta E. R. Dotto,
• Juliana Eccher,
• Leonardo N. Furini,
• Hugo Gallardo,
• Harald Bock and
• Ivan H. Bechtold

Beilstein J. Org. Chem. 2023, 19, 1755–1765, doi:10.3762/bjoc.19.128

• 1758 cm−1 (C=O). X-ray diffraction (XRD) measurements of 1 and 2 are shown in Figure 2. The Miller indices indicate the Colhex and Colrect character of the mesophases [31]. Despite crystallization of 2, the Colrect order is partially preserved at room temperature. The Colhex lattice parameter (a

• square roughness (Rrms) of 1.7 nm and 2.8 nm for 1 (Figure 5a) and 2 (Figure 5b), respectively. The Rrms of the films deposited on Al for the electron-only devices are 1.1 nm for 1 (Figure 5c) and 16.0 nm for 2 (Figure 5d). XRD measurements of as-casted spin-coated films of 1 and 2 confirm their columnar

• the autofocus. XRD measurements were performed with an X’Pert PRO (PANalytical) diffractometer using Cu Kα radiation (λ = 1.5418 Å) equipped with an X’Celerator detector. A small amount of 1 or 2 was deposited onto a glass substrate and heated to the isotropic liquid phase. The diffracted radiation

Effects of the aldehyde-derived ring substituent on the properties of two new bioinspired trimethoxybenzoylhydrazones: methyl vs nitro groups

• Dayanne Martins,
• Roberta Lamosa,
• Talis Uelisson da Silva,
• Carolina B. P. Ligiero,
• Sérgio de Paula Machado,
• Daphne S. Cukierman and
• Nicolás A. Rey

Beilstein J. Org. Chem. 2023, 19, 1713–1727, doi:10.3762/bjoc.19.125

• liquors and, in both cases, XRD confirmed the obtention of the (E)-isomer, in an anti-conformation. Computational calculations (gas and water phases) were performed in order to confirm some of the structural and vibrational aspects of the compounds. An important intramolecular H bond involving the

• ; phenol acidity; ring substituents; XRD; Introduction N-Acylhydrazones are a class of compounds that contain the hydrazonic functional group (–NH–N=C–) attached to an acyl group, which can be modified to generate a range of different structures with varying properties [1]. The versatility of this class

• vibrational aspects of the compounds. The optimized structures obtained with B3LYP/6-311G(d,p) (both in gas and water phases) were compared to the respective experimental XRD structures (Figure 3). The RMSD values for hdz-NO2 in gas (0.431 Å) and water (0.405 Å) phases were lower than the respective values

Tying a knot between crown ethers and porphyrins

• Maksym Matviyishyn and
• Bartosz Szyszko

Beilstein J. Org. Chem. 2023, 19, 1630–1650, doi:10.3762/bjoc.19.120

• anion. The formed receptor: ion-pair 1:1 complex 4-CsF was stable in solution, as evidenced by 1H NMR spectroscopy. The binding constant Ka = 3.8·105 M−1 in CHCl3/MeOH 9:1 was reported. The XRD analysis in the solid state provided further proof of the binding mode, demonstrating the significant

• , accommodating the axially-positioned water molecule on the cobalt(III) centre. The latter assembled into a remarkable hexagonal wheel architecture when exposed to air in THF, as evidenced by XRD (Figure 12). The hexagonal wheel [16-Co(III)]6 was stabilised by intramolecular hydrogen bonding between the water

• nitrogen in the middle of the ether chain of 19-Cr. The reaction between in situ generated 17-K2 or 19-K2 and CoCl2 produced paramagnetic cobalt(II) complexes 17-Co or 19-Co [67]. The XRD analysis of 17-Co revealed a molecular structure with distorted octahedral Co(II) coordinating water and hydroxide

C3-Alkylation of furfural derivatives by continuous flow homogeneous catalysis

• Grédy Kiala Kinkutu,
• Catherine Louis,
• Myriam Roy,
• Juliette Blanchard and
• Julie Oble

Beilstein J. Org. Chem. 2023, 19, 582–592, doi:10.3762/bjoc.19.43

• Supporting Information File 20: Experimental and copies of spectra. Acknowledgements The authors acknowledge MS3U of Sorbonne Université for HRMS analysis and CNRS. We also thank J. Forté for the XRD analyses (IPCM) and A. Miche for the XPS analyses (LRS). Funding The authors acknowledge H2020-WIDESPREAD-05

Comparison of crystal structure and DFT calculations of triferrocenyl trithiophosphite’s conformance

• Ruslan P. Shekurov,
• Mikhail N. Khrizanforov,
• Ilya A. Bezkishko,
• Tatiana P. Gerasimova,
• Almaz A. Zagidullin,
• Daut R. Islamov and
• Vasili A. Miluykov

Beilstein J. Org. Chem. 2022, 18, 1499–1504, doi:10.3762/bjoc.18.157

• [7]. It is important to know the conformational capabilities of such ligands for construction of such complexes [8][9][10][11]. However, to date, XRD data on phosphorus derivatives containing a ferrocenyl substituent at the sulfur atom are presented only in oxidized and sulfurized forms

Recent developments and trends in the iron- and cobalt-catalyzed Sonogashira reactions

• Surendran Amrutha,
• Sankaran Radhika and
• Gopinathan Anilkumar

Beilstein J. Org. Chem. 2022, 18, 262–285, doi:10.3762/bjoc.18.31

• phenylacetylene in the presence of a series of PdCo bimetallic nanoparticles with different compositions on graphite sheets as highly active catalysts (Scheme 27) [40]. The catalyst was prepared by a chemical reduction method and characterized by various techniques like Raman, XRD, TEM, and XPS. The Pd/Co(1:1)NPs

Synthesis of novel [1,2,4]triazolo[1,5-b][1,2,4,5]tetrazines and investigation of their fungistatic activity

• Anna V. Korotina,
• Svetlana G. Tolshchina,
• Rashida I. Ishmetova,
• Natalya P. Evstigneeva,
• Natalya A. Gerasimova,
• Natalya V. Zilberberg,
• Nikolay V. Kungurov,
• Gennady L. Rusinov,
• Oleg N. Chupakhin and
• Valery N. Charushin

Beilstein J. Org. Chem. 2022, 18, 243–250, doi:10.3762/bjoc.18.29

• XRD data (Figure 1). In order to select optimal conditions for the synthesis of compounds 3, the oxidative systems have been varied for the reactions of tetrazines 2a,b,g bearing methyl, phenyl, and pyrazolyl substituents. Attempts to use Pb(OAc)4 as an oxidizing agent in CHCl3 resulted in the

Ready access to 7,8-dihydroindolo[2,3-d][1]benzazepine-6(5H)-one scaffold and analogues via early-stage Fischer ring-closure reaction

• Irina Kuznetcova,
• Felix Bacher,
• Daniel Vegh,
• Hsiang-Yu Chuang and
• Vladimir B. Arion

Beilstein J. Org. Chem. 2022, 18, 143–151, doi:10.3762/bjoc.18.15

• interchanged. However, to our delight only the formation of the desired species 1a occurred, as evidenced by two-dimensional NMR measurements (for atom labeling scheme used for assignment of resonances see Figure S1 in Supporting Information File 1) and confirmed by SC-XRD (Figure 2), being in agreement with

• [2,3-d][1]benzazepin-6(5H)-one (3a). This procedure delivered analytically pure 3a in 80% yield as also confirmed by SC-XRD (Figure 3). The final step to structure C required removal of the benzyl group. Debenzylation of amines is commonly performed by palladium-catalyzed hydrogenation [40]. However

• glacial acetic acid at 100 °C gave 1c in 53% yield. Compound 2c was obtained by palladium-catalyzed reduction of 1c with hydrogen in an excellent yield and its structure was confirmed by SC-XRD (Figure S4 in Supporting Information File 1). The following ring-closure reaction of 2c with trimethylaluminum

Green synthesis of C5–C6-unsubstituted 1,4-DHP scaffolds using an efficient Ni–chitosan nanocatalyst under ultrasonic conditions

• Soumyadip Basu,
• Sauvik Chatterjee,
• Suman Ray,
• Suvendu Maity,
• Prasanta Ghosh,
• Asim Bhaumik and
• Chhanda Mukhopadhyay

Beilstein J. Org. Chem. 2022, 18, 133–142, doi:10.3762/bjoc.18.14

• characterized by powder Fourier-transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray (EDX) spectroscopy, etc. It was effectively utilized in the eco-friendly synthesis of

• similarity of the two spectra may have been due to the low content of nickel in the catalyst. To understand the crystallinity of the material, we carried out a powder XRD (PXRD) analysis (Figure 2). Chitosan, in general, gives rise to a characteristic, partially crystalline phase by virtue of intramolecular

• with this methodology, as shown in Figure 5. The synthesized products were characterized by 1H NMR, 13C NMR, HRMS, and melting point analysis. The structure of the compounds was also confirmed by single-crystal XRD analysis of 4a (CCDC1949329, Figure 6). Plausible mechanism A plausible reaction

Photophysical, photostability, and ROS generation properties of new trifluoromethylated quinoline-phenol Schiff bases

• Inaiá O. Rocha,
• Yuri G. Kappenberg,
• Wilian C. Rosa,
• Clarissa P. Frizzo,
• Nilo Zanatta,
• Marcos A. P. Martins,
• Isadora Tisoco,
• Bernardo A. Iglesias and
• Helio G. Bonacorso

Beilstein J. Org. Chem. 2021, 17, 2799–2811, doi:10.3762/bjoc.17.191

• solution and no signal belonging to the Z isomer was observed in all cases, which can be confirmed by the chemical shift values in the 1H NMR regarding the –CH=N bond. Finally, in order to determine the real molecular structure of the Schiff bases 3, single-crystal X-ray diffraction (SC-XRD) was performed

Synthesis of new bile acid-fused tetrazoles using the Schmidt reaction

• Dušan Đ. Škorić,
• Olivera R. Klisurić,
• Dimitar S. Jakimov,
• Marija N. Sakač and
• János J. Csanádi

Beilstein J. Org. Chem. 2021, 17, 2611–2620, doi:10.3762/bjoc.17.174

• the aromatic tetrazole ring. A characteristic example of this is the H-17 proton in compound 13 with an unusually high chemical shift (2.85 ppm). Unambiguous confirmation of the tetrazole molecular structure came from the XRD analysis of compounds 13 and 14 (Figure 3) [50][51]. The already established

• additional XRD analysis. A preliminary test of the antiproliferative activity showed that the introduction of C-ring-fused tetrazole lowered the activity towards some tumor cell lines compared to the corresponding ketone, while B-ring-fused tetrazole increased these activities. Experimental General procedure

Free-radical cyclization approach to polyheterocycles containing pyrrole and pyridine rings

• Ivan P. Mosiagin,
• Olesya A. Tomashenko,
• Dar’ya V. Spiridonova,
• Mikhail S. Novikov,
• Sergey P. Tunik and
• Alexander F. Khlebnikov

Beilstein J. Org. Chem. 2021, 17, 1490–1498, doi:10.3762/bjoc.17.105

• ]pyrrolo[2,3,4-ij]quinolizin-14-ium bromide (Scheme 4). The structure of 13 was confirmed by XRD-analysis (Figure 2). The reaction of bromide 13 with aq KOH at room temperature gave quantitatively the corresponding base 14. This new 24π-electron hexacyclic phenalenoid doped with two nitrogens is

• XRD-analysis (Figure 3). It was found that both salt 17a and base 18a can be isomerized into isomer 19 under heating in the presence of AlCl3 via migration of the 3-Ph-group into the position 2 (Scheme 6). Compounds 18a, 19 can be quantitatively N-alkylated by MeI at room temperature and by BnBr at 40

Synthesis of 1-indolyl-3,5,8-substituted γ-carbolines: one-pot solvent-free protocol and biological evaluation

• Premansh Dudhe,
• Mena Asha Krishnan,
• Kratika Yadav,
• Diptendu Roy,
• Krishnan Venkatasubbaiah,
• Biswarup Pathak and
• Venkatesh Chelvam

Beilstein J. Org. Chem. 2021, 17, 1453–1463, doi:10.3762/bjoc.17.101

• derivative 3ac (10 nM, 100 nM, 1 μM, 10 μM, and 100 μM), the cellular uptake and distribution was monitored by using confocal microscopy (λex = 405 nm; λem range = 420–470 nm). Selected examples of compounds containing the γ-carboline core. Single-crystal XRD structure of 3ac (CCDC: 1897787). UV–vis

• various cancer cell lines. Supporting Information Supporting Information File 194: Copies of 1H, 13C NMR spectra of 1a–h, 3aa–ac, 3ba–bc, 3da, 3ea, 3ga, 12a–b, 12e–f, 12i, 14d, 14g and 15, UV calibration curves in different organic solvents for γ-carboline 3ac, and single-crystal XRD data of 3ac

A new and efficient methodology for olefin epoxidation catalyzed by supported cobalt nanoparticles

• Lucía Rossi-Fernández,
• Viviana Dorn and
• Gabriel Radivoy

Beilstein J. Org. Chem. 2021, 17, 519–526, doi:10.3762/bjoc.17.46

• confirming the heterogeneous nature of the catalytic method. The freshly prepared CoNPs/MgO catalyst was characterized by means of transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray diffraction (XRD) and

• Information File 1) confirmed the presence of cobalt with energy bands of 0.8 (L line), 6.9 and 7.7 keV (K lines). The XRD diffractogram showed only the support diffraction pattern, no diffraction peaks owing to cobalt species could be observed. The cobalt loading fixed to the MgO support was 1.9 wt % as

• . X-ray diffraction (XRD) analyses were performed using a Bruker AXS D8 Advance diffractometer, equipped with a Cu-Kα1,2 radiation source. Atomic absorption spectroscopy was carried out on a Perkin Elmer AAnalist200 spectrometer. X-ray photoelectron spectroscopic analyses (XPS) were performed on a PHI