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3. Selective Carbon Dioxide versus Nitrous Oxide Adsorption in Cerium(IV) Bithiazole and Bipyridyl Metal‐Organic Frameworks.

Author

Pugliesi, Matteo, Cavallo, Margherita, Atzori, Cesare, Garetto, Beatrice, Borfecchia, Elisa, Donà, Lorenzo, Civalleri, Bartolomeo, Tuci, Giulia, Giambastiani, Giuliano, Galli, Simona, Bonino, Francesca, and Rossin, Andrea

Subjects
CARBON dioxide adsorption, EXTENDED X-ray absorption fine structure, CARBON dioxide, NITROUS oxide, ADSORPTION capacity
Abstract

The two CeIV MOFs [Ce6O4(OH)4(TzTz)6] (Ce_TzTz) and [Ce6O4(OH)4(TzTz)4(PyPy)2] (Ce_TzTz_PyPy; H2TzTz = [2,2′‐bithiazole]‐5,5′‐dicarboxylic acid, H2PyPy = 2,2′‐bipyridine‐5,5′‐dicarboxylic acid) are prepared starting from a pre‐formed [Ce6] glycinate‐capped cluster. N2 isotherms collected at 77 K revealed BET specific surface areas of 1136 and 238 m2 g−1, respectively. Their CO2 and N2O adsorption capacity is assessed at T = 273 and 298 K and p = 1 bar. Ce_TzTz shows the highest gas uptake (7.9 and 9.7 wt% at 298 K and 11.5 and 12.5 wt% at 273 K for CO2 and N2O, respectively). More interestingly, this homo‐linker MOF possesses a higher capacity, thermodynamic affinity [(Qst)CO2 = 18.2 kJ mol−1 vs (Qst)N2O = 25.4 kJ mol−1] and selectivity (IAST SN2O/CO2 = 1.6 at T = 273 K) toward N2O than the mixed‐linker sample. At variance, Ce_TzTz_PyPy shows a slightly higher capacity, thermodinamic affinity [(Qst)CO2 = 29.5 kJ mol−1 vs (Qst)N2O = 26.4 kJ mol−1] and selectivity (IAST SCO2/N2O = 1.4 at T = 298 K) toward CO2. DFT optimizations carried out on the [N2O@Ce_TzTz] and [CO2@Ce_TzTz_PyPy] systems revealed that the primary adsorption sites are the cerium ions of the [Ce6] metallic node for N2O and the thiazole N‐atoms on the TzTz linker for CO2, respectively. [ABSTRACT FROM AUTHOR]

Published
2024
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11. CO2 Capture and Conversion to C1 Chemicals with Mixed-Metal Copper/Nickel Bis(amino)bipyrazolate Metal–Organic Frameworks

Author

Campitelli, Patrizio, primary, Tombesi, Alessia, additional, Di Nicola, Corrado, additional, Pettinari, Claudio, additional, Mauri, Anna, additional, Galli, Simona, additional, Yan, Tongan, additional, Liu, Dahuan, additional, Duan, Jiaxin Dawn, additional, Goswami, Subhadip, additional, Tuci, Giulia, additional, Giambastiani, Giuliano, additional, Hupp, Joseph T., additional, and Rossin, Andrea, additional

Published
2023
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12. Synthetic and computational studies of organometallic complexes containing low-coordinate group 13 ligands

Author

Rossin, Andrea

Subjects
546
Abstract

The work presented in this thesis is concerned with synthetic and computational studies of low coordinate transition metal complexes of boron. New symmetrically bridged boryl complexes of iron and manganese have been prepared and characterised. Information obtained from spectroscopic and structural analyses, together with Density Functional theoretical studies, has been used to investigate the nature of the metal-boron bonds in these complexes. Development of the chemistry of related terminal analogues has also been undertaken. The M-B bonds present in these molecules can be considered mainly o in character, with very little n contribution. Attempts to investigate the chemistry of base-stabilised boryl complexes, using PMe3 and THF as Lewis bases, shows that, while PMe3 adducts with haloboranes are very stable and do not react with metallic fragments, THF complexes give more promising results, especially when THF is also used as a solvent for the reaction. Substitution and abstraction chemistry of the new (mesityloxy)chloroborane (MesO)BCl2 has been analysed. Replacement of the chlorine atom in (ti5-C5H5)Fe(CO)2 B(OMes)Cll by other nucleophiles is possible, thereby generating new asymmetric boryl ligands. Chloride abstraction using NalBAr'J leads to the formation of the fluoroboryl complex (Tf-C5Hs)Fe(CO)2 B(OMes)F possibly via the putative terminal borylene (n5-C5R5XCO)2Fe=B(OMes) Oxidative addition of B-H, B-B and B-X bonds to both d-block (Rh, Pt) and p-block (In, Sn) metals as an alternative pathway to boryl complexes has also been examined. Unfortunately, while many of the reactions appear to give the expected products (on the basis of in situ NMR monitoring), purification difficulties have prevented the isolation of many of these species as pure compounds. DFT studies on terminal boron- aluminium- and gamum containing complexes have been undertaken. Geometry optimisation, molecular orbital composition, bond dissociation energies and bond density partitioning have been investigated in order to probe the nature of the M=E bonds (E = B, Al, Ga) and the dependence of compound stability on both the ancillary metal-bound ligands and on the substituent of the group 13 diyl fragment. The examples considered were diyl complexes of general formula (n5-C5R5KL)2M(EX)1D+, the "naked" bridging gallium complex ({(CrMes)Fe(CO)2}2Ga + and five gallium carbene complexes of first row transition metals (V, Mn, Fe, Co, Ni), featuring the heterocyclic ligand {:Ga N(Ph)CH 2}.

Published
2004

15. Not Just Another Methanation Catalyst: Depleted Uranium Meets Nickel for a High‐Performing Process Under Autothermal Regime

Author

Truong‐Phuoc, Lai, primary, Nhut, Jean‐Mario, additional, Sall, Secou, additional, Tuci, Giulia, additional, Rossin, Andrea, additional, Papaefthimiou, Vasiliki, additional, Duong‐Viet, Cuong, additional, Petit, Corinne, additional, Arab, Mehdi, additional, Jourdan, Alex, additional, Vidal, Loic, additional, Giambastiani, Giuliano, additional, and Pham‐Huu, Cuong, additional

Published
2023
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17. Front Cover: Not Just Another Methanation Catalyst: Depleted Uranium Meets Nickel for a High‐Performing Process Under Autothermal Regime (ChemSusChem 5/2023)

Author

Truong‐Phuoc, Lai, primary, Nhut, Jean‐Mario, additional, Sall, Secou, additional, Tuci, Giulia, additional, Rossin, Andrea, additional, Papaefthimiou, Vasiliki, additional, Duong‐Viet, Cuong, additional, Petit, Corinne, additional, Arab, Mehdi, additional, Jourdan, Alex, additional, Vidal, Loic, additional, Giambastiani, Giuliano, additional, and Pham‐Huu, Cuong, additional

Published
2023
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19. Not Just Another Methanation Catalyst: Depleted Uranium Meets Nickel for a High‐Performing Process Under Autothermal Regime

Author

Truong‐Phuoc, Lai, primary, Nhut, Jean‐Mario, additional, Sall, Secou, additional, Tuci, Giulia, additional, Rossin, Andrea, additional, Papaefthimiou, Vasiliki, additional, Duong‐Viet, Cuong, additional, Petit, Corinne, additional, Arab, Mehdi, additional, Jourdan, Alex, additional, Vidal, Loic, additional, Giambastiani, Giuliano, additional, and Pham‐Huu, Cuong, additional

Published
2022
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21. Metal‐Free Electrocatalysts for the Selective 2 e− Oxygen Reduction Reaction: A Never‐Ending Story?

Author

Tuci, Giulia, Rossin, Andrea, Zhang, Xiong, Truong‐Phuoc, Lai, Berretti, Enrico, Liu, Yuefeng, Pham‐Huu, Cuong, Ali, Sajjad, Jan, Faheem, Poggini, Lorenzo, and Giambastiani, Giuliano

Subjects
*OXYGEN reduction, *ELECTROCATALYSTS, *MULTIWALLED carbon nanotubes, *ELECTROSYNTHESIS, *HYDROGEN peroxide
Abstract

Hydrogen peroxide (H2O2) electrosynthesis via the 2e− Oxygen Reduction Reaction (ORR) represents a highly challenging, environmentally friendly and cost‐effective alternative to the current anthraquinone‐based technology. Various lightweight element hetero‐doped carbon nanostructures are promising and cheap metal‐free electrocatalysts for H2O2 synthesis, particularly those containing O‐functionalities. The exact role of O‐containing functional groups as electroactive sites for the process remains debated if not highly controversial. Herein, we have reported on the covalent exohedral functionalization of the outer surface of extra‐pure multi‐walled carbon nanotubes (MWCNTs) with discrete O‐functional groups as a unique approach to prepare selective electrocatalysts for the process. This kind of decoration has added fundamental tiles to the puzzling structure/reactivity relationship of O‐containing carbon‐based catalysts for ORR, clearing doubts on the controversial role of hydroxyl/phenol groups as key functionalities for the design of more performing 2e− ORR electrocatalysts. [ABSTRACT FROM AUTHOR]

Published
2023
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24. Graphite Felt-Sandwiched Ni/SiC Catalysts for the Induction Versus Joule-Heated Sabatier Reaction: Assessing the Catalyst Temperature at the Nanoscale

Author

Lai Truong-Phuoc, Cuong Duong-Viet, Tuci, Giulia, Rossin, Andrea, Nhut, Jean-Mario, Baaziz, Walid, Ersen, Ovidiu, Arab, Mehdi, Jourdan, Alex, Giambastiani, Giuliano, and Cuong Pham-Huu

Subjects
temperature of inductively heated nano-objects, SiC-based catalysts, Joule heating, methanation reaction, induction heating
Abstract

The paper describes a series of graphite felt-sandwiched Ni-k/SiC composites at variable metal loading (k = 10, 15, and 20 wt %) and their application as catalysts for the CO2 methanation process (Sabatier reaction) under two distinct and conceptually different heating setups: Joule heating versus induction heating (IH). A comparative analysis carried out on all catalysts from this series operated under the two heating configurations has unveiled the superior performance of radiofrequency (RF)-heated (IH) catalysts in the process. Most importantly, it has offered a practical tool to map the gap existing between the macroscopic temperature value measured at the catalyst bed using a remotesensing thermometer (pyrometer) and that (real) of the excited metal nano-objects (Ni NPs) directly engaged in the RF-heated catalytic process. Besides the evident advantages of IH technology applied to the methanation process in terms of process rates (lambda) already under nominally low reaction temperatures, the virtual absence of any thermal inertia and the subsequent fast modulation of the temperature at the catalytic bed demonstrate unique features of this heating technology in terms of process safety (cold-reactor walls) and reduction of energy wastes (neither pre- and postcatalyst heating of reagents and products nor that of the whole reactor volume and its peripheral walls).

Published
2022

26. Graphite Felt-Sandwiched Ni/SiC Catalysts for the Induction Versus Joule-Heated Sabatier Reaction: Assessing the Catalyst Temperature at the Nanoscale

Author

Truong-Phuoc, Lai, primary, Duong-Viet, Cuong, additional, Tuci, Giulia, additional, Rossin, Andrea, additional, Nhut, Jean-Mario, additional, Baaziz, Walid, additional, Ersen, Ovidiu, additional, Arab, Mehdi, additional, Jourdan, Alex, additional, Giambastiani, Giuliano, additional, and Pham-Huu, Cuong, additional

Published
2021
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31. Multimodal hybrid 2D networks: via the thiol-epoxide reaction on 1T/2H MoS2polytypes

Author

Tuci, Giulia, Rossin, Andrea, Pham-Huu, Cuong, Mosconi, Dario, Luconi, Lapo, Agnoli, Stefano, Granozzi, Gaetano, and Giambastiani, Giuliano

Subjects
chemical functionalization, Thiol-Epoxides Reaction, 1T/2H MoS2 Polytypes
Abstract

Searching for new protocols aimed at the surface functionalization of TMDCs is the password for filling the gap between reactivity and versatility of 2D carbon-based networks and their inorganic counterparts. This contribution describes a straightforward but effective approach to the chemical decoration of chemically exfoliated MoS2 nanosheets with ß-hydroxyl organic pendant arms. The adopted strategy is based on the thiol-epoxide "click"reaction and generates functional hybrids with a loading of dangling organic groups directly proportional to the epoxide electrophilic character. Most importantly, this grafted methodology occurs for the first time on both phases (1T and 2H) of the model chalcogenide and provides functional samples suitable for an additional functionalization step-forward (post-derivatization).

Published
2021

32. Ammonia–Borane Dehydrogenation Catalyzed by Dual-Mode Proton-Responsive Ir-CNNH Complexes

Author

Universidad de Sevilla. Departamento de Química Inorgánica, Agencia Estatal de Investigación. España, Junta de Andalucía, Ortega Lepe, Isabel, Rossin, Andrea, Sánchez Mellado, Práxedes, López Santos, Laura, Rendón Márquez, Nuria, Álvarez González, Eleuterio, López Serrano, Joaquín, Suárez Escobar, Andrés Luis, Universidad de Sevilla. Departamento de Química Inorgánica, Agencia Estatal de Investigación. España, Junta de Andalucía, Ortega Lepe, Isabel, Rossin, Andrea, Sánchez Mellado, Práxedes, López Santos, Laura, Rendón Márquez, Nuria, Álvarez González, Eleuterio, López Serrano, Joaquín, and Suárez Escobar, Andrés Luis

Abstract

Metal complexes incorporating proton-responsive ligands have been proved to be superior catalysts in reactions involving the H2 molecule. In this contribution, a series of IrIII complexes based on lutidine-derived CNNH pincers containing N-heterocyclic carbene and secondary amino NHR [R = Ph (4a), tBu (4b), benzyl (4c)] donors as flanking groups have been synthesized and tested in the dehydrogenation of ammonia–borane (NH3BH3, AB) in the presence of substoichiometric amounts (2.5 equiv) of tBuOK. These preactivated derivatives are efficient catalysts in AB dehydrogenation in THF at room temperature, albeit significantly different reaction rates were observed. Thus, by using 0.4 mol % of 4a, 1.0 equiv of H2 per mole of AB was released in 8.5 min (turnover frequency (TOF50%) = 1875 h–1), while complexes 4b and 4c (0.8 mol %) exhibited lower catalytic activities (TOF50% = 55–60 h–1). 4a is currently the best performing IrIII homogeneous catalyst for AB dehydrogenation. Kinetic rate measurements show a zero-order dependence with respect to AB, and first order with the catalyst in the dehydrogenation with 4a (−d[AB]/dt = k[4a]). Conversely, the reaction with 4b is second order in AB and first order in the catalyst (−d[AB]/dt = k[4b][AB]2). Moreover, the reactions of the derivatives 4a and 4b with an excess of tBuOK (2.5 equiv) have been analyzed through NMR spectroscopy. For the former precursor, formation of the iridate 5 was observed as a result of a double deprotonation at the amine and the NHC pincer arm. In marked contrast, in the case of 4b, a monodeprotonated (at the pincer NHC-arm) species 6 is observed upon reaction with tBuOK. Complex 6 is capable of activating H2 reversibly to yield the trihydride derivative 7. Finally, DFT calculations of the first AB dehydrogenation step catalyzed by 5 has been performed at the DFT//MN15 level of theory in order to get information on the predominant metal–ligand cooperation mode.

Published
2021

33. Ammonia−Borane Dehydrogenation Catalyzed by Dual-Mode Proton-Responsive Ir-CNNH Complexes

Author

Agencia Estatal de Investigación (España), Junta de Andalucía, Ortega-Lepe, Isabel, Rossin, Andrea, Sánchez, Práxedes, Santos, Laura L., Rendón, Nuria, Álvarez, Eleuterio, López-Serrano, Joaquín, Suárez, Andrés, Agencia Estatal de Investigación (España), Junta de Andalucía, Ortega-Lepe, Isabel, Rossin, Andrea, Sánchez, Práxedes, Santos, Laura L., Rendón, Nuria, Álvarez, Eleuterio, López-Serrano, Joaquín, and Suárez, Andrés

Abstract

Metal complexes incorporating proton-responsive ligands have been proved to be superior catalysts in reactions involving the H2 molecule. In this contribution, a series of IrIII complexes based on lutidine-derived CNNH pincers containing Nheterocyclic carbene and secondary amino NHR [R = Ph (4a), tBu (4b), benzyl (4c)] donors as flanking groups have been synthesized and tested in the dehydrogenation of ammonia− borane (NH3BH3, AB) in the presence of substoichiometric amounts (2.5 equiv) of tBuOK. These preactivated derivatives are efficient catalysts in AB dehydrogenation in THF at room temperature, albeit significantly different reaction rates were observed. Thus, by using 0.4 mol % of 4a, 1.0 equiv of H2 per mole of AB was released in 8.5 min (turnover frequency (TOF50%) = 1875 h−1), while complexes 4b and 4c (0.8 mol %) exhibited lower catalytic activities (TOF50% = 55−60 h−1). 4a is currently the best performing IrIII homogeneous catalyst for AB dehydrogenation. Kinetic rate measurements show a zero-order dependence with respect to AB, and first order with the catalyst in the dehydrogenation with 4a (−d[AB]/dt = k[4a]). Conversely, the reaction with 4b is second order in AB and first order in the catalyst (−d[AB]/dt = k[4b][AB]2). Moreover, the reactions of the derivatives 4a and 4b with an excess of tBuOK (2.5 equiv) have been analyzed through NMR spectroscopy. For the former precursor, formation of the iridate 5 was observed as a result of a double deprotonation at the amine and the NHC pincer arm. In marked contrast, in the case of 4b, a monodeprotonated (at the pincer NHC-arm) species 6 is observed upon reaction with tBuOK. Complex 6 is capable of activating H2 reversibly to yield the trihydride derivative 7. Finally, DFT calculations of the first AB dehydrogenation step catalyzed by 5 has been performed at the DFT//MN15 level of theory in order to get information on the predominant metal−ligand cooperation mode.

Published
2021

38. Benzothiazolium-functionalizedNU-1000: a versatile material for carbon dioxide adsorption and cyanide luminescence sensing

Author

Luconi, Lapo, Mercuri, Giorgio, Islamoglu, Timur, Fermi, Andrea, Bergamini, Giacomo, Giambastiani, Giuliano, and Rossin, Andrea

Subjects
Metal-Organic Frameworks (MOFs) - porous materials - zirconium(IV) - thiazolium salts - carbon dioxide adsorption - luminescent sensing - cyanide
Abstract

A tailor-made benzothiazolium bromide salt functionality (BzTz) is introducedviasolvent-assisted ligand incorporation (SALI) into the mesoporous Zr-based metal-organic frameworkNU-1000. The resultingNU-1000-BzTzcomposite has been thoroughly characterized in the solid state. The functional group loading has been determined throughH NMR analysis of the digested sample (5% HF-DMSO-d): a maximum value of 1.7BzTzligand per [Zr] node is achieved. The material preserves its pristine crystallinity after SALI, as witnessed by powder X-ray diffraction. The functionalized MOF has a slightly lower thermal stability than its parent material (T= 780vs.800 K, respectively). The Nadsorption isotherm collected at 77 K disclosed that its BET specific surface area (1530 mg) is lower than that of prisitineNU-1000(2140 mg), because of the space taken and weight added by the dangling benzothiazolium groups inside the pores. A total COuptake of 2.0 mmol g(8.7 wt% CO) has been calculated from the COadsoprtion isotherm collected atT= 298 K andp= 1 bar. Despite the lower BET area,NU-1000-BzTzshows an increased thermodynamic affinity for CO(isosteric heat of adsorptionQ= 25 kJ mol) if compared withNU-1000(Q= 17 kJ mol), confirming that the presence of a polar functional group in the MOF pores improves the interaction with carbon dioxide. Finally,NU-1000-BzTzhas been exploited as a luminescent sensor for polluting anions (CN, SCN, OCN, and SeCNas sodium or potassium salts) in aqueous solutions, after bromide exchange. A marked reversible blue shift of its emission band from 490 to 450 nm is observed in all cases, with the associated emission color change from light green to blue under a UV lamp. The detection limit of CN(1.08 × 10M) is much lower than that measured for the other "stick-like" anions considered in this study. The process occurs efficiently even in the presence of other competing ions (i.e.in ordinary tap water), opening promising application perspectives in cyanide luminescence sensing in drinking water.

Published
2020

39. Cobalt(II) Bipyrazolate Metal-Organic Frameworks as Heterogeneous Catalysts in Cumene Aerobic Oxidation: A Tag-Dependent Selectivity

Author

European Commission, Ministerio de Economía y Competitividad (España), Ministerio de Ciencia, Innovación y Universidades (España), Nowacka, Anna, Vismara, R., Mercuri, G, Moroni, M., Palomino, Miguel, Domasevitch, K.V., Di Nicola, C., Pettinari, Claudio, Giambastiani, Giuliano, Llabrés i Xamena, Francesc X., Galli, Simona, Rossin, Andrea, European Commission, Ministerio de Economía y Competitividad (España), Ministerio de Ciencia, Innovación y Universidades (España), Nowacka, Anna, Vismara, R., Mercuri, G, Moroni, M., Palomino, Miguel, Domasevitch, K.V., Di Nicola, C., Pettinari, Claudio, Giambastiani, Giuliano, Llabrés i Xamena, Francesc X., Galli, Simona, and Rossin, Andrea

Abstract

Three metal-organic frameworks with the general formula Co(BPZX) (BPZX = 3-X-4,4′-bipyrazolate, X = H, NH, NO) constructed with ligands having different functional groups on the same skeleton have been employed as heterogeneous catalysts for aerobic liquid-phase oxidation of cumene with O as oxidant. O adsorption isotherms collected at p = 1 atm and T = 195 and 273 K have cast light on the relative affinity of these catalysts for dioxygen. The highest gas uptake at 195 K is found for Co(BPZ) (3.2 mmol/g (10.1 wt % O)), in line with its highest BET specific surface area (926 m/g) in comparison with those of Co(BPZNH) (317 m/g) and Co(BPZNO) (645 m/g). The O isosteric heat of adsorption (Q) trend follows the order Co(BPZ) > Co(BPZNH) > Co(BPZNO). Interestingly, the selectivity in the cumene oxidation products was found to be dependent on the tag present in the catalyst linker: While cumene hydroperoxide (CHP) is the main product obtained with Co(BPZ) (84% selectivity to CHP after 7 h, p = 4 bar, and T = 363 K), further oxidation to 2-phenyl-2-propanol (PP) is observed in the presence of Co(BPZNH) as the catalyst (69% selectivity to PP under the same experimental conditions).

Published
2020

43. Bifunctional activation of amine-boranes by the W/Pd bimetallic analogs of “frustrated Lewis pairs”

Author

Osipova, Elena S., primary, Gulyaeva, Ekaterina S., additional, Gutsul, Evgenii I., additional, Kirkina, Vladislava A., additional, Pavlov, Alexander A., additional, Nelyubina, Yulia V., additional, Rossin, Andrea, additional, Peruzzini, Maurizio, additional, Epstein, Lina M., additional, Belkova, Natalia V., additional, Filippov, Oleg A., additional, and Shubina, Elena S., additional

Published
2021
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46. Cover Feature: Highly Nickel‐Loaded γ‐Alumina Composites for a Radiofrequency‐Heated, Low‐Temperature CO 2 Methanation Scheme (ChemSusChem 20/2020)

Author

Wang, Wei, primary, Duong‐Viet, Cuong, additional, Tuci, Giulia, additional, Liu, Yuefeng, additional, Rossin, Andrea, additional, Luconi, Lapo, additional, Nhut, Jean‐Mario, additional, Nguyen‐Dinh, Lam, additional, Giambastiani, Giuliano, additional, and Pham‐Huu, Cuong, additional

Published
2020
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49. Cobalt(II) Bipyrazolate Metal–Organic Frameworks as Heterogeneous Catalysts in Cumene Aerobic Oxidation: A Tag-Dependent Selectivity

Author

Nowacka, Anna, primary, Vismara, Rebecca, additional, Mercuri, Giorgio, additional, Moroni, Marco, additional, Palomino, Miguel, additional, Domasevitch, Kostiantyn V., additional, Di Nicola, Corrado, additional, Pettinari, Claudio, additional, Giambastiani, Giuliano, additional, Llabrés i Xamena, Francesc X., additional, Galli, Simona, additional, and Rossin, Andrea, additional

Published
2020
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