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1. A new compound in the BEDT-TTF family [BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene] with a tetrathiocyanatocuprate(II) anion, (BEDT-TTF)4[Cu(NCS)4]

Author: Christophe Faulmann, Benoît Cormary, Lydie Valade, Kane Jacob, and Dominique de Caro
Subjects: crystal structure, BEDT-TTF, Cu(NCS)2, superconductor, pseudo-κ arrangement, Crystallography, QD901-999
Abstract: A new phase combining BEDT-TTF and [Cu(NCS)4]2– as the counter-anion, namely bis[bis(ethylenedithio)tetrathiafulvalenium] tetrathiocyanatocuprate(II) bis[bis(ethylenedithio)tetrathiafulvalene], (C10H8S8)2[Cu(NCS)4]·2C10H8S8 or (BEDT-TTF)4[Cu(NCS)4] was obtained during a galvanostatic electrocrystallization process. As previously observed with BEDT-TTF-based compounds with oxalatometallate anions, the BEDT-TTF molecules in (BEDT-TTF)4[Cu(NCS)4] exhibit the so-called pseudo-κ arrangement, with two BEDT-TTF molecules being positively charged and two electronically neutral. The bond lengths and angles in the two unique BEDT-TTF molecules differ slightly. The crystal structure consists of layers of BEDT-TTF molecules extending parallel to (001). The width of this layer corresponds to the length of the a axis [16.9036 (17) Å]. The BEDT-TTF layers are separated by layers of centrosymmetric square-planar [Cu(NCS)4]2– dianions.
Published: 2018
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2. First Nanoparticles of a Conductor Based on the Organic Donor Molecule BETS: κ-(BETS)2FeCl4

Author: Dominique de Caro, Christophe Faulmann, Lydie Valade, Kane Jacob, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre d'élaboration de matériaux et d'études structurales (CEMES), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), and Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP)
Subjects: Diffraction, Technology, Materials science, molecular conductors, Band gap, electrocrystallization technique, Imine, Nanoparticle, 02 engineering and technology, 010402 general chemistry, Electrochemistry, 01 natural sciences, chemistry.chemical_compound, Saturation current, Molecule, General Materials Science, [CHIM.COOR]Chemical Sciences/Coordination chemistry, bis(ethylenedithio)tetraselenafulvalene BETS, Superconductivity, Microscopy, QC120-168.85, Communication, QH201-278.5, [CHIM.MATE]Chemical Sciences/Material chemistry, Engineering (General). Civil engineering (General), 021001 nanoscience & nanotechnology, TK1-9971, 0104 chemical sciences, Descriptive and experimental mechanics, chemistry, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Physical chemistry, nanoparticles, amphiphilic imine, Electrical engineering. Electronics. Nuclear engineering, TA1-2040, 0210 nano-technology
Abstract: Nanoparticles of the molecular superconductor (BETS)2FeCl4 were obtained by the electrochemical oxidation of BETS in the presence of [(C2H5)4N]FeCl4 and an amphiphilic imine (OATM), acting as a growth controlling agent. When the reaction was carried out with a molar ratio OATM/BETS of 10, roughly spherical nanoparticles exhibiting sizes in the 10–40 nm range were observed. X-ray diffraction patterns evidenced the growth of (BETS)2FeCl4 nanoparticles with the κ-type structure. The current-voltage characteristic recorded on an individual nanoparticle aggregate was fitted with a Shockley diode model. A saturation current of 1216 pA and a threshold voltage of 0.62 V were extracted from this model. This latter value was consistent with roughly half of the energy gap of the semiconducting nano-crystalline aggregate.
Published: 2021
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3. Characterization of Charge States in Conducting Organic Nanoparticles by X-ray Photoemission Spectroscopy

Author: Lydie Valade, Jordi Fraxedas, Christophe Faulmann, Antje Vollmer, Dominique de Caro, Norbert Koch, Kane Jacob, Catalan Institute of Nanoscience and Nanotechnology (ICN2), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC)-Barcelona Institute of Science and Technology (BIST), Helmholtz-Zentrum Berlin für Materialien und Energie GmbH (HZB), Humboldt University of Berlin, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Ministerio de Economía y Competitividad (España), Generalitat de Catalunya, Humboldt University Of Berlin, Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Spanish Ministry of Economy and Competitiveness (MINECO) - Contract No. PGC2018-095032-B-100, Severo Ochoa program (Grant SEV-2017-0706), Generalitat de Catalunya - CERCA program, BESSY IA-SFS program (BESSY-ID.09.2.90190), and European Project
Subjects: Technology, Materials science, Photoemission spectroscopy, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Bis(ethilenedithio)tetrathiafulvelene, Article, conducting nanoparticles, bis(ethilenedithio)tetrathiafulvalene, chemistry.chemical_compound, Condensed Matter::Materials Science, X-ray photoelectron spectroscopy, tetrathiafulvalene, Condensed Matter::Superconductivity, Molecule, General Materials Science, Molecular orbital, [CHIM.COOR]Chemical Sciences/Coordination chemistry, charge-transfer complexes, Spectroscopy, Microscopy, QC120-168.85, 600 Technik und Technologie, synchrotron radiation, Chemical shift, QH201-278.5, Engineering (General). Civil engineering (General), 021001 nanoscience & nanotechnology, Acceptor, TK1-9971, 0104 chemical sciences, Tetrahiafulvalene, Descriptive and experimental mechanics, chemistry, Chemical physics, bis ethilenedithio tetrathiafulvalene, charge transfer complexes, mixed valence materials, X ray photoemission spectroscopy, Condensed Matter::Strongly Correlated Electrons, Electrical engineering. Electronics. Nuclear engineering, TA1-2040, 0210 nano-technology, mixed-valence materials, X-ray photoemission spectroscopy, ddc:600, Tetrathiafulvalene
Abstract: The metallic and semiconducting character of a large family of organic materials based on the electron donor molecule tetrathiafulvalene (TTF) is rooted in the partial oxidation (charge transfer or mixed valency) of TTF derivatives leading to partially filled molecular orbital-based electronic bands. The intrinsic structure of such complexes, with segregated donor and acceptor molecular chains or planes, leads to anisotropic electronic properties (quasi one-dimensional or two-dimensional) and morphology (needle-like or platelet-like crystals). Recently, such materials have been synthesized as nanoparticles by intentionally frustrating the intrinsic anisotropic growth. X-ray photoemission spectroscopy (XPS) has emerged as a valuable technique to characterize the transfer of charge due to its ability to discriminate the different chemical environments or electronic configurations manifested by chemical shifts of core level lines in high-resolution spectra. Since the photoemission process is inherently fast (well below the femtosecond time scale), dynamic processes can be efficiently explored. We determine here the fingerprint of partial oxidation on the photoemission lines of nanoparticles of selected TTF-based conductors., This research was supported by the Spanish Ministry of Economy and Competitiveness (MINECO) under Contract No. PGC2018-095032-B-100. The ICN2 is funded by the CERCA program/Generalitat de Catalunya. The ICN2 is supported by the Severo Ochoa program of MINECO (Grant SEV-2017-0706). The research leading to these results received funding from the European Community’s Seventh Framework Program (FP7/2007-2013) under grant agreement no. 226716. We also acknowledge support through the BESSY IA-SFS program (BESSY-ID.09.2.90190).
Published: 2021
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4. Possible observation of the signature of the bad metal phase and its crossover to a Fermi liquid in K(BEDT-TTF)2Cu(NCS)2 bulk and nanoparticles by Raman scattering

Author: Christophe Faulmann, Maximilien Cazayous, Alain Sacuto, Kane Jacob, L. Valade, Yann Gallais, D. de Caro, M. Revelli Beaumont, Pierre Hemme, Laboratoire Matériaux et Phénomènes Quantiques (MPQ (UMR_7162)), Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Materials science, Phonon, Nanoparticle, FOS: Physical sciences, 02 engineering and technology, Low frequency, Plateau (mathematics), 01 natural sciences, Metal, symbols.namesake, Condensed Matter - Strongly Correlated Electrons, Phase (matter), 0103 physical sciences, General Materials Science, [CHIM.COOR]Chemical Sciences/Coordination chemistry, 010306 general physics, Condensed matter physics, Strongly Correlated Electrons (cond-mat.str-el), 021001 nanoscience & nanotechnology, Condensed Matter Physics, visual_art, visual_art.visual_art_medium, symbols, Fermi liquid theory, 0210 nano-technology, Raman scattering
Abstract: κ‐(BEDT‐TTF)2Cu(NCS)2 has been investigated by Raman scattering in both bulk and nanoparticle compounds. Phonon modes from 20 to 1600 cm−1 have been assigned. Focusing on the unexplored low frequency phonons, a plateau in frequencies is observed in the bulk phonons between 50 and 100 K and assigned to the signature of the bad metal phase. Nanoparticles of κ‐(BEDT‐TTF)2Cu(NCS)2 exhibit anomalies at 50 K associated to the crossover from a bad metal to a Fermi liquid whose origins are discussed.
Published: 2021
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5. Amplitude mode of charge density wave in TTF[Ni(dmit)2]2 observed by electronic Raman scattering

Author: Yann Gallais, M. Revelli Beaumont, D. de Caro, Alain Sacuto, C. Faulmann, Maximilien Cazayous, Kane Jacob, and L. Valade
Subjects: Materials science, Condensed matter physics, Charge density, 02 engineering and technology, 021001 nanoscience & nanotechnology, 01 natural sciences, Conductor, symbols.namesake, Amplitude, Condensed Matter::Superconductivity, 0103 physical sciences, symbols, Condensed Matter::Strongly Correlated Electrons, 010306 general physics, 0210 nano-technology, Anisotropy, Raman spectroscopy, Charge density wave, Raman scattering, Energy (signal processing)
Abstract: We measured the optical signature of charge density waves (CDWs) in the multiband conductor $\mathrm{TTF}{[\mathrm{Ni}{(\mathrm{dmit})}_{2}]}_{2}$ by electronic Raman scattering. At low energies, a hump develops below 60 K. This hump is associated to the amplitude mode of the CDW with an energy around 9 meV. Raman symmetry-resolved measurements show that the CDW amplitude mode is anisotropic and that the CDW can be associated to the band nesting of $\mathrm{Ni}{(\mathrm{dmit})}_{2}$ chains.
Published: 2021
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6. Possible observation of the signature of the bad metal phase and its crossover to a Fermi liquid in Κ-(BEDT-TTF)

Author: Marco, Revelli, Pierre, Hemme, Yann, Gallais, A, Sacuto, Kane, Jacob, Lydie, Valade, Dominique, De Caro, Christophe, Faulmann, and Maximilien, Cazayous
Abstract: Κ-(BEDT-TTF)
Published: 2021

7. Superconducting super-organized nanoparticles of the superconductor (BEDT-TTF)2Cu(NCS)2

Author: Tadashi Kawamoto, Jordi Fraxedas, Dominique de Caro, Christophe Faulmann, Shuxiang Fan, Marco Revelli-Beaumont, Kane Jacob, Marine Tassé, Takehiko Mori, Sonia Mallet-Ladeira, Lydie Valade, Laboratoire de chimie de coordination (LCC), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Centre d'élaboration de matériaux et d'études structurales (CEMES), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Tokyo Institute of Technology [Tokyo] (TITECH), ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Institut de Chimie de Toulouse (ICT-FR 2599), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)
Subjects: Materials science, Analytical chemistry, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, superconductor, Saturation current, Electrical resistivity and conductivity, Phase (matter), Seebeck coefficient, Materials Chemistry, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Molecular conductor, Superconductivity, Mechanical Engineering, Metals and Alloys, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Magnetic susceptibility, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, [PHYS.COND.CM-S]Physics [physics]/Condensed Matter [cond-mat]/Superconductivity [cond-mat.supr-con], chemistry, Mechanics of Materials, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], nanoparticles, 0210 nano-technology, Tetrathiafulvalene
Abstract: International audience; The synthesis of (BEDT-TTF)2Cu(NCS)2 in the presence of poly(ethylene glycol) leads to super-organized nanoparticles of 2–8 nm size. Samples contain crystalline nanoparticles of the κ-(BEDT-TTF)2Cu(NCS)2 phase. The electrical conductivity at room temperature is about 0.08 S · cm–1, a typical value for nanopowders of tetrathiafulvalene-based conducting compounds. The current-voltage characteristic for an individual nanoparticle aggregate is fitted with a Shockley diode model. A saturation current of 4.1 pA and a threshold voltage of 0.45 V are extracted. N1s and S2p lines in X-ray photoelectron spectroscopy evidence a charge transfer, characteristic for tetrathiafulvalene-based conducting salts. Magnetic susceptibility studies show a superconducting transition at 9.1 K, a characteristic value for the κ-(BEDT-TTF)2Cu(NCS)2 phase. The thermoelectric power of the nanopowder is represented by the average //c and //b values for the single-crystal. Finally, resistivity for the nanopowder is nearly flat in the metallic region.
Published: 2021
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8. Reproducible nanostructuration of the superconducting κ-(BEDT-TTF)2Cu(NCS)2 phase

Author: Maximilien Cazayous, Kane Jacob, Alain Sacuto, Claude Pasquier, Miguel Monteverde, Yann Gallais, Pascale Auban Senzier, Marco Revelli Beaumont, Dominique de Caro, Lydie Valade, Christophe Faulmann, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Matériaux et Phénomènes Quantiques (MPQ (UMR_7162)), Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP), Laboratoire de Physique des Solides (LPS), Centre National de la Recherche Scientifique (CNRS)-Université Paris-Sud - Paris 11 (UP11), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité), and Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Superconducting transition, Materials science, Nanoparticle, 02 engineering and technology, 010402 general chemistry, SQUID, 01 natural sciences, symbols.namesake, Quality (physics), Phase (matter), biology.animal, Materials Chemistry, [CHIM.COOR]Chemical Sciences/Coordination chemistry, BEDT-TTF, Superconductivity, Squid, Condensed matter physics, biology, Mechanical Engineering, Metals and Alloys, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, Mechanics of Materials, Homogeneous, symbols, 0210 nano-technology, Raman spectroscopy
Abstract: International audience; The synthesis of the superconductor κ-(BEDT-TTF)2Cu(NCS)2 is optimized following a two-pot procedure to obtain high quality nanoparticles This leads to homogeneous sized-nanoparticles, 30 nm diameter, which are further characterized by XRD and Raman spectroscopy. SQUID measurements confirm the occurrence of the superconducting transition at 9.1 K.
Published: 2020
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9. Synthesis and Characterization of the Thermoelectric Nickel Tetrathiooxalate Polymer as Nanoparticles

Author: Christophe Faulmann, Pascale De Caro, Lydie Valade, Benoît Cormary, Dominique de Caro, Kane Jacob, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de physique et chimie des nano-objets (LPCNO), Institut de Recherche sur les Systèmes Atomiques et Moléculaires Complexes (IRSAMC), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche sur les Systèmes Atomiques et Moléculaires Complexes (IRSAMC), Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)
Subjects: chemistry.chemical_classification, Conductive coordination polymers, Materials science, Tetrathiooxalate, Coordination polymer, [SDV]Life Sciences [q-bio], Nanoparticle, chemistry.chemical_element, Infrared spectroscopy, Polyethylene glycol, Polymer, Atmospheric temperature range, Polyethylene Glycol, Polyester, chemistry.chemical_compound, Nickel, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Nanoparticles, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Biobased Polyesters
Abstract: International audience; Nanoparticles of the conductive coordination polymer Ni(tto) have been synthesized under mild conditions in the presence of bio-based polyesters or polyethylene glycol acting as growth controlling agents. With polyesters, aggregates of particles are observed whereas well dispersed nanoparticles are obtained with polyethylene glycol. Indeed, for a Ni2+/polyethylene glycol weight ratio of 0.031, transmission electron micrographs evidence dispersed particles exhibiting sizes in the 3 - 10 nm range. Infrared spectra for nanopowders show two CS stretching modes in the 1100 - 1190 cm−1 range, confirming the presence of the tetrathiooxalate ligand coordinated to the nickel center. The room-temperature electrical conductivity for the nanopowder prepared in the presence of polyethylene glycol is about 0.8 S∙cm−1, a decent value for tetrathiolate-based polymers. Finally, magnetic susceptibility measurements for well-dispersed Ni(tto) particles evidence a Curie-Weiss law in a large temperature range. Moreover, low temperatures measurement would confirm intra- or interchain interactions between nickel atoms within the Ni(tto) polymer chains.
Published: 2020
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10. First nanoparticles of Per2[Au(mnt)2]

Author: Christophe Faulmann, Lydie Valade, Dominique de Caro, Marine Tassé, Kane Jacob, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Centre d'élaboration de matériaux et d'études structurales (CEMES), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), and Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP)
Subjects: Materials science, Infrared, Nanoparticle, 02 engineering and technology, 010402 general chemistry, Electrochemistry, 01 natural sciences, chemistry.chemical_compound, symbols.namesake, Electrical resistivity and conductivity, [CHIM]Chemical Sciences, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Electrical and Electronic Engineering, Current–voltage curves, Perylene, Zwitterionic ionic liquid, Building and Construction, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Electrocrystallization, Maleonitrile dithiolate gold(III) complex, chemistry, Nanocrystal, Ionic liquid, symbols, Physical chemistry, Nanoparticles, 0210 nano-technology, Raman spectroscopy, Amphiphilic species
Abstract: International audience; Nanoparticles of the Per2[Au(mnt)2] (Per perylene; mnt2- maleonitrile dithiolate) compound have been obtained by the electrochemical oxidation of perylene in the presence of [(n-C4H9)4N][Au(mnt)2] and, either an amphiphilic molecule (OATM), or a zwitterionic ionic liquid (BIBS), acting as growth controlling agents. When the reaction is carried out with OATM, nanocrystals exhibiting sizes in the 35–100 nm range are grown whereas roughly spherical nanoparticles are observed if BIBS is used (10–40 nm in diameter). Infrared and Raman spectra confirm the presence of both perylene donor and maleonitrile dithiolate ligands within the nanopowders. Electrical conductivity measurements at room temperature lead to about 0.025 S.cm-1, a typical value for nanopowders of bis(dithiolene)-based conducting compounds. Finally, current–voltage characteristics for the spherical nanoparticles are fitted with a Shockley diode model. A saturation current of 19.3 pA and a threshold voltage of 0.149 V are extracted from this model.
Published: 2020
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11. Nanoparticles of molecular conductors and superconductors: Progress over the last ten years

Author: Christophe Faulmann, Lydie Valade, Kane Jacob, Dominique de Caro, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), CNRS, French Ministry of Higher Education and Research, CNES, and EU
Subjects: Superconductivity, Molecular conductors, Chemistry, Nanoparticle, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Inorganic Chemistry, Colloidal solutions, Coordination polymers, Organic superconductors, Nanoparticles, [CHIM.COOR]Chemical Sciences/Coordination chemistry, 0210 nano-technology, Electrical conductor, Size‐controlling agent
Abstract: International audience; We review conditions for growing molecular conductors and superconductors as nanoparticles, an attractive morphology for integrating them into electronic components or composite materials. Although the one-dimensional character of these materials does not favor their growth as spheroidal objects, by adding growth controlling molecules to the reaction mixture, we succeeded in growing particles from 2 to 50 nm in size for fourteen systems. The choice of the growth controller depends on the nature of the chemical interactions it can establish with the reactive species to limit growth, and on the chemical or electrochemical synthesis procedure. We show that the chemical nature of the nanoparticles is alike single crystals. Due to resistive boundaries, conducting properties of nanoparticle powders are alike microcrystalline powders. Nevertheless, superconductivity occurs in three of the studied materials. The potential application of these nanomaterials is reported in four fields: composite materials, field effect transistors, thermoelectric components and biomedical materials.
Published: 2020
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12. Supramolecular organization of perfluorinated 1H-indazoles in the solid state using X-ray crystallography, SSNMR and sensitive (VCD) and non sensitive (MIR, FIR and Raman) to chirality vibrational spectroscopies

Author: Kane Jacob, Juan Jesús López-González, María Mar Quesada-Moreno, José Elguero, Ibon Alkorta, Rosa M. Claramunt, Juan Ramón Avilés-Moreno, Michel Etienne, Laure Vendier, Ministerio de Economía y Competitividad (España), Junta de Andalucía, Comunidad de Madrid, European Commission, Grupo de Investigacion Quimica Fisica Teorica y Experimental (FQM-173), Departamento de Quimica Fisica y Analitica, Facultad de Ciencias Experimentales, Universidad de Jaen, Universidad de Jaén (UJA), Departamento de Sistemas Fisicos, Quimicos y Naturales, Facultad de Ciencias Experimentales, Universidad Pablo de Olavide, Universidad Pablo de Olavide [Sevilla] (UPO), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, Instituto de Quimica Médica (CSIC), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Departamento de Quimica Organica y Bio-Organica, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia, and Universidad Nacional de Educación a Distancia (UNED)
Subjects: 010405 organic chemistry, Chemistry, Supramolecular chemistry, General Physics and Astronomy, 010402 general chemistry, 01 natural sciences, 0104 chemical sciences, Crystallography, symbols.namesake, Solid-state nuclear magnetic resonance, Helix, X-ray crystallography, symbols, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Physical and Theoretical Chemistry, Enantiomer, Enantiomeric excess, Chirality (chemistry), Raman spectroscopy
Abstract: 1H-Indazole derivatives exhibit a remarkable property since some of them form chiral supramolecular structures starting from achiral monomers. The present work deals with the study of three perfluorinated 1H-indazoles that resolve spontaneously as conglomerates. These conglomerates can contain either a pure enantiomer (one helix) or a mixture of both enantiomers (both helices) with an enantiomeric excess (e.e.) of one of them. The difficulty of the structural analysis of these types of compounds is thus clear. We outline a complete strategy to determine the structures and configurations (M or P helices) of the enantiomers (helices) forming the conglomerates of these perfluorinated 1H-indazoles based on X-ray crystallography, solid state NMR spectroscopy and different solid state vibrational spectroscopies that are either sensitive (VCD) or not (FarIR, IR and Raman) to chirality, together with quantum chemical calculations (DFT)., This work was carried out with financial support from the Ministerio de Economía y Competitividad (Project No. CTQ2014- 56833R and CTQ2015-63997-C2-2-P), CICE/Junta de Andalucía (P08-FQM-04096) and CICE/JA-FEDER-UJA: Plan de Fortalecimiento de las Capacidades de I+D+i/2014-15 (UJA2013/08/03) and Comunidad Autónoma de Madrid (Project FOTOCARBON, ref. S2013/MIT-2841). Computer, storage and other resources from the CTI (CSIC) are gratefully acknowledged. Authors thank the University of Jaén for continuing financial support, for bridge projects (UJA2015/08/07) and (UJA2016/08/15) and for Accion 2: Financiacion de Incentivos a la Excelencia de I+D+i de la UJA 2014-15 in 2014 and 2015 calls and to its CICT for instrumental facilities. Authors also thank the FQM-323 research group, especially Rafael Lopez Blanco, David Moreno Gonzalez and Jose Robles Molina, for their help in the laboratory. M. M. Q. M. thanks the University of Jaen for a pre-doctoral fellowship. The CNRS is acknowledged for support
Published: 2017
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13. A new compound in the BEDT-TTF family [BEDT-TTF = bis-(ethyl-enedi-thio)-tetra-thia-fulvalene] with a tetra-thio-cyanato-cuprate(II) anion, (BEDT-TTF)

Author: Christophe, Faulmann, Benoît, Cormary, Lydie, Valade, Kane, Jacob, and Dominique, de Caro
Subjects: crystal structure, superconductor, pseudo-κ arrangement, BEDT-TTF, Research Communications, Cu(NCS)2
Abstract: The new compound (BEDT-TTF)4[Cu(NCS)4] based on the organic donor BEDT-TTF [bis(ethylenedithio)tetrathiafulvalene] has been obtained during a galvanostatic electrocrystallization process with Cu(NCS). It exhibits a pseudo-κ arrangement, never observed up to now in the BEDT-TTF family with thiocyanatocuprate(II) anions., A new phase combining BEDT-TTF and [Cu(NCS)4]2– as the counter-anion, namely bis[bis(ethylenedithio)tetrathiafulvalenium] tetrathiocyanatocuprate(II) bis[bis(ethylenedithio)tetrathiafulvalene], (C10H8S8)2[Cu(NCS)4]·2C10H8S8 or (BEDT-TTF)4[Cu(NCS)4] was obtained during a galvanostatic electrocrystallization process. As previously observed with BEDT-TTF-based compounds with oxalatometallate anions, the BEDT-TTF molecules in (BEDT-TTF)4[Cu(NCS)4] exhibit the so-called pseudo-κ arrangement, with two BEDT-TTF molecules being positively charged and two electronically neutral. The bond lengths and angles in the two unique BEDT-TTF molecules differ slightly. The crystal structure consists of layers of BEDT-TTF molecules extending parallel to (001). The width of this layer corresponds to the length of the a axis [16.9036 (17) Å]. The BEDT-TTF layers are separated by layers of centrosymmetric square-planar [Cu(NCS)4]2– dianions.
Published: 2018

14. Adjusting the cation and anion nature in ionic liquids used for the growth control of nanoparticles of organic conductors

Author: Kane Jacob, Lydie Valade, Christophe Faulmann, Dominique de Caro, Benoît Cormary, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de physique et chimie des nano-objets (LPCNO), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut de Recherche sur les Systèmes Atomiques et Moléculaires Complexes (IRSAMC), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche sur les Systèmes Atomiques et Moléculaires Complexes (IRSAMC), Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Superconductivity, ionic liquid, Materials science, Supporting electrolyte, nanoparticle, Inorganic chemistry, Nanoparticle, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Ion, Conductor, chemistry.chemical_compound, superconductor, chemistry, Ionic liquid, [CHIM]Chemical Sciences, organic conductor, electrocrystallization, 0210 nano-technology, Electrical conductor, Tetrathiafulvalene
Abstract: International audience; Ionic liquids are used for controlling the growth of organic conductors as nanoparticles. We review the conditions of preparation of nanoparticles of conductors derived from tetrathiafulvalene (TTF), tetramethyltetraselenafulvalene (TMTSF) and bis-ethylenedithiotetrathiafulvalene (BEDT-TTF). They are prepared by electrocrystallization using imidazolium or ammonium - based ionic liquids supporting electrolyte in which the cation plays the role of growth controller and the anion enters the composition of the expected organic conductor. Stable suspensions of anoparticles are obtained in one case, a valuable characteristic for potential applications in electronic devices.
Published: 2016
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15. Measuring the Relative Reactivity of the Carbon-Hydrogen Bonds of Alkanes as Nucleophiles

Author: Andrea Olmos, Kane Jacob, Pedro J. Pérez, Ana Caballero, Bárbara Noverges, Gregorio Asensio, Riccardo Gava, Maria Besora, Feliu Maseras, Michel Etienne, W. M. Chamil Sameera, Delia Bellezza, Laboratorio de Catalisis Homogenea, Unidad Asociada al CSIC CIQSO-Centro de Investigacion en Quimica Sostenible and Departamento de Quimica, Universidad de Huelva, Universidad de Huelva, Departamento de Quimica Organica, Facultad de Farmacia, Universitat de Valencia, Universitat de València (UV), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institute of Chemical Research of Catalonia (ICIQ), Departament de Química [Barcelona] (UAB), Universitat Autònoma de Barcelona (UAB), Institute of Low Temperature Science [Sapporo], Hokkaido University [Sapporo, Japan], Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées
Subjects: Alkane, chemistry.chemical_classification, C-H bond functionalization, 010405 organic chemistry, Hydrogen bond, Nucleophilicity, chemistry.chemical_element, General Medicine, General Chemistry, 010402 general chemistry, 01 natural sciences, Medicinal chemistry, Catalysis, 0104 chemical sciences, chemistry, Nucleophile, Alkanes, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Reactivity (chemistry), Electrophilicity, Carbon, Metal carbene complexes
Abstract: We report quantitative measurements of the relative reactivities of a series of C-H bonds of gaseous or liquid CnH2n+2 alkanes (n = 1-8, 29 different C-H bonds) towards insitu generated electrophiles (copper, silver, and rhodium carbenes), with methane as the reference. This strategy surpasses the drawback of previous model reactions of alkanes with strong electrophiles suffering from C-C cleavage processes, which precluded direct comparison of the relative reactivities of alkane C-H bonds., We thank MINECO for support with Grants CTQ2014-52769-C03-01, CTQ2014-52769-C03-02, CTQ2017-82893-C2-1-R, CTQ2014-62234-EXP, CTQ2015-73693-JIN, CTQ2017-87792-R, Severo Ochoa Excellence Accreditation 2014-2018 (SEV-2013-0319), and Red Intecat (CTQ2016-81923-REDC). Junta de Andalucia is also acknowledged for Grant P12-FQM-1765. R.G. and A.O. thank MINECO for FPI and Juan delaCierva fellowships, respectively. B.N. thanks MEC for a FPU fellowship. The CNRS is thanked for support.
Published: 2018
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16. Catalytic Functionalization of Methane and Light Alkanes in Supercritical Carbon Dioxide

Author: Andrea Olmos, M. Ángeles Fuentes, M. Elena González‐Núñez, Ana Caballero, Pedro J. Pérez, Bianca K. Muñoz, Gregorio Asensio, Michel Etienne, Kane Jacob, Rossella Mello, Laboratorio de Catalisis Homogenea, Unidad Asociada al CSIC CIQSO-Centro de Investigacion en Quimica Sostenible and Departamento de Quimica, Universidad de Huelva, Universidad de Huelva, Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Departamento de Quimica Organica, Facultad de Farmacia, Universitat de Valencia, and Universitat de València (UV)
Subjects: Silver, Ligands, 010402 general chemistry, 01 natural sciences, 7. Clean energy, Catalysis, chemistry.chemical_compound, Ethyl propionate, Ethyl diazoacetate, Coordination Complexes, Methyl bisulfate, Alkanes, Organic chemistry, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Supercritical carbon dioxide, 010405 organic chemistry, Organic Chemistry, Butane, Diazonium Compounds, General Chemistry, Carbon Dioxide, 0104 chemical sciences, Solubility, chemistry, Isobutane, Oxidative coupling of methane, Methane
Abstract: International audience; The development of catalytic methods for the effective functionalization of methane yet remains a challenge. The best system known to date is the so-called Catalytica Process based on the use of platinum catalysts to convert methane into methyl bisulfate with a TOF rate of 10−3 s. In this contribution, we report a series of silver complexes containing perfluorinated tris(indazolyl)borate ligands that catalyze the functionalization of methane into ethyl propionate upon reaction with ethyl diazoacetate (EDA) by using supercritical carbon dioxide (scCO2) as the reaction medium. The employment of this reaction medium has also allowed the functionalization of ethane, propane, butane, and isobutane.
Published: 2014
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17. Silver-Catalyzed Functionalization of Esters by Carbene Transfer: The Role of Ylide Zwitterionic Intermediates

Author: Pedro J. Pérez, Tomás R. Belderrain, Riccardo Gava, Feliu Maseras, Kane Jacob, M. Ángeles Fuentes, Ana Caballero, Michel Etienne, Maria Besora, Laboratorio de Catalisis Homogenea, Unidad Asociada al CSIC CIQSO-Centro de Investigacion en Quimica Sostenible and Departamento de Quimica, Universidad de Huelva, Universidad de Huelva, Institute of Chemical Research of Catalonia (ICIQ), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées
Subjects: chemistry.chemical_classification, 010405 organic chemistry, Organic Chemistry, Context (language use), 010402 general chemistry, 01 natural sciences, Medicinal chemistry, Catalysis, 0104 chemical sciences, Inorganic Chemistry, chemistry.chemical_compound, Ethyl diazoacetate, chemistry, Ylide, Acetone, Surface modification, Organic chemistry, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Diazo, Physical and Theoretical Chemistry, Carbene
Abstract: International audience; The reaction of esters with ethyl diazoacetate catalyzed by the complex [F-27-Tp(4 Bo, 3CF2CF3)Ag(acetone)] generates alpha-(acyloxy)acetates in moderate to high yields. This is a novel transformation in the context of carbene-transfer reactions from diazo compounds that, according to experimental and theoretical data, is suggested to occur through zwitterionic intermediates.
Published: 2014
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18. Perfluorinated 1H-indazoles and hydrotris(indazol-1-yl)borates. Supramolecular organization and a new synthetic procedure to form scorpionate ligands

Author: Kane Jacob, Nuria Romero, Emmanuelle Despagnet-Ayoub, Laure Vendier, Bianca K. Muñoz, Michel Etienne, Wilfried-Solo Ojo, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Indazole, Stereochemistry, Supramolecular chemistry, General Chemistry, Crystal structure, Catalysis, chemistry.chemical_compound, Crystallography, chemistry, Group (periodic table), Intramolecular force, Helix, Materials Chemistry, Molecule, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Nest (protein structural motif)
Abstract: International audience; This paper describes the syntheses and full characterization of perfluorinated 1H-indazoles 2-5 and hydrotris(indazolyl)borate thallium complexes 6-9 that contain linear perfluoroalkyl chains varying from two to six carbon atoms in the 3-position. In the solid state, the perfluorinated 1H-indazoles exhibit supramolecular structures that depend on the length of the perfluoroalkyl chain. A catemer of order 3 is observed for the CF2CF3 derivative 2 (chiral space group P32), catemers of order 2 are observed for the C3F7 and C4F9 derivatives 3 (chiral space group P212121, one type of helix in the unit cell) and 4 (space group P21/n, two types of helices in the unit cell), respectively, and stacks of dimers are observed for the indazole with the longer C6F13 chain 5 (space group P21/c). The perfluorinated hydrotris(indazolyl)borate thallium complexes 6-9 [TlFn-Tp4Bo,3Rf] have been obtained by a new reaction based on the reaction of HBBr2 (generated in situ from BBr3 and Et3SiH) with the indazolates of 2-5 followed by cation exchange. The X-ray crystal structure of [TlF33-Tp4Bo,3C3F7] 7 shows that, in addition to coordination to the three nitrogens, the thallium is buried in a nest of fluorines with seven short intramolecular TlF contacts with the pendant perfluoropropyl chains. The potential of these highly fluorinated molecules to act as ligands is highlighted.
Published: 2014
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19. CH bond activation of unsaturated hydrocarbons by a niobium methyl cyclopropyl precursor. Cyclopropyl ring opening and alkyne coupling reaction

Author: Chiara Dinoi, Chen Li, Michel Etienne, Laure Vendier, Pascal Oulié, Kane Jacob, Alix Sournia-Saquet, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées
Subjects: chemistry.chemical_classification, 010405 organic chemistry, Stereochemistry, Organic Chemistry, Alkyne, Nuclear magnetic resonance spectroscopy, Cyclopropene, 010402 general chemistry, 01 natural sciences, Medicinal chemistry, Coupling reaction, 3. Good health, 0104 chemical sciences, Inorganic Chemistry, chemistry.chemical_compound, chemistry, Intramolecular force, Moiety, Reactivity (chemistry), [CHIM.COOR]Chemical Sciences/Coordination chemistry, Physical and Theoretical Chemistry, Bicyclobutane
Abstract: International audience; The transient intermediate η2-cyclopropene/bicyclobutane niobium complex [TpMe2Nb(η2-c-C3H4)(MeCCMe)] A, generated by an intramolecular β-H abstraction of methane from the methyl cyclopropyl complex [TpMe2NbMe(c-C3H5)(MeCCMe)] (1), is able to cleave the CH bond of a variety of unsaturated hydrocarbons RH in a selective manner to give the corresponding hydrocarbyl complexes [TpMe2NbR(c-C3H5)(MeCCMe)] (R = 2-furyl, 2-thienyl, 1-alkynyl, 1-cyclopentenyl, 1-ferrocenyl (Fc), pentafluorophenyl). The activation of the C–H bond occurs stereospecifically via a 1,3-CH addition across the Nb(η2-cyclopropene) bond of A. Full characterization of several of these complexes includes multinuclear NMR spectroscopy, X-ray diffraction, UV/vis spectroscopy, and electrochemical data. A charge transfer between the ferrocenyl moiety and the niobium center is responsible for the characteristic purple color of the bimetallic complex [TpMe2NbFc(c-C3H5)(MeCCMe)]. The reactivity of these complexes with benzene follows qualitatively the strength and the pKa of the CH bond that is cleaved. The pentafluorophenyl complex [TpMe2Nb(C6F5)(c-C3H5)(MeCCMe)] undergoes cyclopropyl ring opening and alkyne coupling to give two isomeric η4-butadienyl complexes, with [TpMe2Nb(C6F5)(η4-CMeCMeCHCHMe)] as the major isomer.
Published: 2017
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20. Cover Picture: Measuring the Relative Reactivity of the Carbon–Hydrogen Bonds of Alkanes as Nucleophiles (Angew. Chem. Int. Ed. 42/2018)

Author: Riccardo Gava, W. M. Chamil Sameera, Kane Jacob, Feliu Maseras, Ana Caballero, Bárbara Noverges, Gregorio Asensio, Pedro J. Pérez, Andrea Olmos, Michel Etienne, Delia Bellezza, and Maria Besora
Subjects: Nucleophile, Hydrogen bond, Chemistry, Electrophile, INT, chemistry.chemical_element, Cover (algebra), Reactivity (chemistry), General Chemistry, Medicinal chemistry, Carbon, Catalysis
Published: 2018
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21. Titelbild: Measuring the Relative Reactivity of the Carbon–Hydrogen Bonds of Alkanes as Nucleophiles (Angew. Chem. 42/2018)

Author: Riccardo Gava, Feliu Maseras, Ana Caballero, W. M. Chamil Sameera, Bárbara Noverges, Gregorio Asensio, Kane Jacob, Maria Besora, Michel Etienne, Andrea Olmos, Pedro J. Pérez, and Delia Bellezza
Subjects: Nucleophile, Hydrogen bond, Chemistry, Polymer chemistry, chemistry.chemical_element, Reactivity (chemistry), General Medicine, Carbon
Published: 2018
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22. Ionic liquid-stabilized nanoparticles of charge transfer-based conductors

Author: Kane Jacob, Christophe Faulmann, Jordi Fraxedas, J.-P. Legros, François Senocq, Lydie Valade, Dominique de Caro, Centre National de la Recherche Scientifique (France), Ministerio de Ciencia y Tecnología (España), and Generalitat de Catalunya
Subjects: Tetrafluoroborate, Molecular conductors, Mechanical Engineering, Dithiolene complexes, Inorganic chemistry, Metals and Alloys, Nanoparticle, Condensed Matter Physics, Ionic liquids, Electronic, Optical and Magnetic Materials, chemistry.chemical_compound, chemistry, X-ray photoelectron spectroscopy, Mechanics of Materials, Electrical resistivity and conductivity, Ionic liquid, Tetrathiafulvalene, Materials Chemistry, Nanoparticles, Physical chemistry, Molecule, Particle size
Abstract: 5 páginas, 9 figuras.-- et al., Well-dispersed nanoparticles of molecule-based conductors, namely TTF·TCNQ and TTF[Ni(dmit)2]2, have been prepared in organic solution using 1-butyl-3-metylimidazolium tetrafluoroborate as a stabilizing agent. TTF·TCNQ nanoparticles (prepared at room temperature) exhibit sizes ranging from 2 to 5.5 nm, whereas those of TTF[Ni(dmit)2]2 (prepared at −80 °C) are larger (sizes in the 16–45 nm range). Nanoparticle powders have been characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and by transport measurements., This work was supported by the Centre National de la Recherche Scientifique (France), by the Ministerio de Ciencia y Tecnologia (Spain), through project FIS2006-12117-C04-01, and by the Generalitat de Catalunya (SGR 00909).
Published: 2010
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23. TTF[Ni(dmit)2]2: From single-crystals to thin layers, nanowires, and nanoparticles

Author: Lydie Valade, Christophe Faulmann, Dominique de Caro, Kane Jacob, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Nanowire, Nanoparticle, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Inorganic Chemistry, Metal, Transition metal, Materials Chemistry, Molecule, [CHIM]Chemical Sciences, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Thin film, Physical and Theoretical Chemistry, Superconductivity, Thin layers, Chemistry, Transition metal complex, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Crystallography, Molecular material, visual_art, visual_art.visual_art_medium, Superconductor, 0210 nano-technology, Bisdithiolene
Abstract: International audience; The molecular superconductor TTF[Ni(dmit)2]2 is part of the scientific heritage of the Laboratoire de Chimie de Coordination (LCC). Research into molecular materials using transition metal complexes as building blocks was introduced at the LCC by Patrick Cassoux in 1979. The “Molecules and Materials” team isolated the first molecular superconductor containing a transition metal complex, TTF[Ni(dmit)2]2, the metallic behavior of which was demonstrated at ambient pressure and its superconductivity under pressure. This compound was first prepared and studied as single crystals, and processed further to obtain thin films and nanoparticles. In this review, we describe the synthetic procedures used for growing TTF[Ni(dmit)2]2 as single crystals, nanowires, thin films, and nanoparticles, as well as the physical properties of each morphological type and the potential integration of nanoparticles into electronic components.
Published: 2016
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24. Synthesis, characterization, and thermoelectric properties of superconducting (BEDT-TTF)(2)I-3 nanoparticles

Author: Christophe Faulmann, Eden Steven, Lydie Valade, Jordi Fraxedas, I. Chtioui-Gay, Etienne Yvenou, Shermane M. Benjamin, Kane Jacob, Belén Ballesteros, Alexandre Carella, Eun Sang Choi, D. de Caro, Jean-Pierre Simonato, Minseong Lee, P. de Caro, Laboratoire de chimie de coordination (LCC), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT), Chimie Agro-Industrielle (CAI), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT), Catalan Institute of Nanoscience and Nanotechnology (ICN2), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC)-Barcelona Institute of Science and Technology (BIST), Barcelona Institute of Science and Technology (BIST), Facultad de Ciencias y Tecnologias Quimicas, Universidad de Castilla-La Mancha = University of Castilla-La Mancha (UCLM), Instituto de Combustión y Contaminación, National High Magnetic Field Laboratory (NHMFL), National High Magnetic Field Laboratory, Département des Technologies des NanoMatériaux (DTNM), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Ministere de l'Enseignement Superieur et de la Recherche, DGA, Severo Ochoa Program (MINECO) [SEV-2013-0295], NSF-DMR [1309146], Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Université Fédérale Toulouse Midi-Pyrénées, Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Consejo Superior de Investigaciones Científicas [Spain] (CSIC)-Barcelona Institute of Science and Technology (BIST), Universidad de Castilla-La Mancha (UCLM), Institut de Chimie de Toulouse (ICT-FR 2599), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Departamento de Química Física, Facultad de Ciencias Quimicas, Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Department of Chemistry, Università degli studi di Napoli Federico II, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), National Science Foundation (US), Ministère de l’Enseignement supérieur et de la Recherche (France), and Ministerio de Economía y Competitividad (España)
Subjects: Materials science, PHASE, Analytical chemistry, Nanoparticle, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, power, alpha-(bedt-ttf)2i3, organic conductors, beta-(bedt-ttf)2i3, nanocrystals, Phase (matter), Thermoelectric effect, Materials Chemistry, [CHIM]Chemical Sciences, [CHIM.COOR]Chemical Sciences/Coordination chemistry, arrays, Superconductivity, Amphiphilic molecule, Atomic force microscopy, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, gold, 021001 nanoscience & nanotechnology, Magnetic susceptibility, 0104 chemical sciences, Characterization (materials science), thin-films, 0210 nano-technology, absorption
Abstract: The synthesis of (BEDT-TTF)I in the presence of two neutral amphiphilic molecules [N-octylfurfurylimine and 1-octanamine, N-(2-thienylmethylene)] leads to single and aggregated nanoparticles of 2 to 6 nm size. The samples contain highly crystalline nanoparticles of the β-(BEDT-TTF)I phase, confirmed by XRD. Temperature dependent resistance and magnetic susceptibility studies evidence the superconducting transition characteristics of the β-(BEDT-TTF)I phase. The I-V curve of a single nanoparticle aggregate, measured using AFM, exhibits an expected semiconductor-like behaviour. Thermoelectric studies led to a ZT of 1.47 × 10 at 300 K., I. C.-G. thanks the Ministere de l’Enseignement Superieur et de la Recherche for a PhD grant. The authors acknowledge DGA for funding the E. Y. PhD ICN2 acknowledges support from the Severo Ochoa Program (MINECO, Grant SEV-2013-0295). E. S., E. S. C., M. L. and S. M. B. are supported by NSF-DMR 1309146.
Published: 2016
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25. Crystal structure, magnetic properties and Mössbauer studies of [Fe(qsal)2][Ni(dmit)2]

Author: José Antonio Real, Bénédicte Garreau de Bonneval, Gábor Molnár, Stéphane Lampert, Azzedine Bousseksou, Stéphane Dorbes, Lydie Valade, Christophe Faulmann, and Kane Jacob
Subjects: Inorganic Chemistry, Crystallography, Spin crossover, Chemistry, Mössbauer spectroscopy, Materials Chemistry, Crystal structure, Physical and Theoretical Chemistry
Abstract: A new compound of formula [Fe(qsal)2][Ni(dmit)2] (1) has been synthesised, structurally and magnetically characterised (qsalH = N-(8-quinolyl)salicylaldimine, dmit2− = 1,3-dithiol-2-thione-4,5-dithiolato). Its structural features and its magnetic behaviour were compared with those of [Fe(qsal)2]-based complexes, and more particularly [Fe(qsal)2][Ni(dmit)2] · 2CH3CN.
Published: 2007
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26. (BETS)2[RuX5NO] (X = Cl, Br): An Explanation of Different Conductive Properties Through Structural and Spectroscopic Studies

Author: Marie-Liesse Doublet, Lydie Valade, Kane Jacob, A. Glaria, Jean-François Lamère, D. de Caro, Isabelle Malfant, Antoine Zwick, S. Vincendeau, and B. Garreau de Bonneval
Subjects: Materials science, Bromine, business.industry, chemistry.chemical_element, Activation energy, Condensed Matter Physics, Atomic and Molecular Physics, and Optics, chemistry.chemical_compound, symbols.namesake, Semiconductor, chemistry, Electrical resistivity and conductivity, Chlorine, symbols, Physical chemistry, General Materials Science, Raman spectroscopy, business, Derivative (chemistry), Stoichiometry
Abstract: (BETS)2[RuX5NO] (X=Cl, Br) exhibit an identical 2:1 stoichiometry. However, while the chlorine derivative shows an insulating behavior, the bromine behaves as a semiconductor with very small activation energy (0.03 eV). The different electrical behaviors are analyzed through the use of a detailed study of structural data and analysis of Raman spectra
Published: 2006
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27. The First Platinum-Catalyzed Hydroamination of Ethylene

Author: Ousmane Diallo, Ngoc Chau Chu, Magali Cadena, Emmanuelle Mothes, Jean-Jacques Brunet, and Kane Jacob
Subjects: Ethylene, Organic Chemistry, chemistry.chemical_element, Decane, Medicinal chemistry, Catalysis, Inorganic Chemistry, chemistry.chemical_compound, Aniline, chemistry, Organic chemistry, Hydroamination, Ton, Physical and Theoretical Chemistry, Platinum, Bar (unit)
Abstract: The platinum-catalyzed hydroamination of ethylene with aniline is reported for the first time. Using PtBr2 as a catalyst precursor in n-Bu4PBr under 25 bar of ethylene pressure affords N-ethylaniline with 80 turnovers after 10 h at 150 °C. The reaction simultaneously produces 2-methylquinoline in ca. 10 cycles. The catalytic activity is slightly improved by increasing the reaction temperature or the ethylene pressure and strongly depends on the aniline/platinum ratio. The beneficial effects of added P(OMe)3 (2 equiv/PtBr2) or of a proton source (3 equiv/PtBr2) have also been pointed out. A gradual poisoning by N-ethylaniline has been observed, which could be minimized by using biphasic systems. The best result for the hydroamination with aniline (TON = 145 after 10 h at 150 °C) has been obtained in a biphasic system (n-Bu4PBr/decane) in the presence of C6H5NH3+ (3 equiv/PtBr2). The basicity of the arylamine has been shown to play an important role: the lower the basicity, the higher the TON. Thus, the hy...
Published: 2004
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28. ChemInform Abstract: Silver-Catalyzed Functionalization of Esters by Carbene Transfer: The Role of Ylide Zwitterionic Intermediates

Author: Feliu Masera, Tomás R. Belderrain, Riccardo Gava, Pedro J. Pérez, Michel Etienne, M. Ángeles Fuentes, Maria Besora, Kane Jacob, and Ana Caballero
Subjects: chemistry.chemical_classification, Tris, chemistry.chemical_compound, chemistry, Ylide, Polymer chemistry, Surface modification, chemistry.chemical_element, General Medicine, Boron, Carbene, Catalysis
Abstract: A novel carbene transfer reaction from diazoesters to carboxylic acids is developed using a highly fluorinated tris(indazolyl)borate silver complex as catalyst.
Published: 2015
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29. Spin density wave and superconducting properties of nanoparticle organic conductor assemblies

Author: Laurel Winter, Shermane M. Benjamin, Christophe Faulmann, Eden Steven, Lydie Valade, James S. Brooks, Imane Chtioui, Kane Jacob, Belén Ballesteros, Ju-Hyun Park, Dominique de Caro, Jordi Fraxedas, Los Alamos National Laboratory, State of Florida, Department of Energy (US), Ministère de l’Enseignement supérieur et de la Recherche (France), National Science Foundation (US), Florida State University [Tallahassee] (FSU), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Universitat Autònoma de Barcelona (UAB), and Consejo Superior de Investigaciones Cientificas, Barcelone
Subjects: Superconductivity, Phase transition, Materials science, Condensed matter physics, 02 engineering and technology, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 01 natural sciences, 7. Clean energy, Electronic, Optical and Magnetic Materials, Magnetic field, Electrical resistivity and conductivity, 0103 physical sciences, Diamagnetism, Spin density wave, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Crystallite, 010306 general physics, 0210 nano-technology, Stoichiometry
Abstract: Under the terms of the Creative Commons Attribution License 3.0 (CC-BY).-- et al., The magnetic susceptibilities of nanoparticle assemblies of two Bechgaard salts (TMTSF)2PF6 and (TMTSF)2ClO4, have been studied vs temperature and magnetic field. In the bulk these materials exhibit a spin density wave formation (TSDW=12K) and superconductivity (Tc=1.2K), respectively. We show from inductive (susceptibility) measurements that the nanoparticle assemblies exhibit ground-state phase transitions similar to those of randomly oriented polycrystalline samples of the parent materials. Resistivity and diamagnetic shielding measurements yield additional information on the functional nanoparticle structure in terms of stoichiometric and nonstoichiometric composition., This work was supported by NSF-DMR Grants No. 1005293 and No. 1309146, and the NHMFL is supported by NSF Cooperative Agreement No. DMR-1157490, the State of Florida, and the U.S. Department of Energy. I.C. thanks the French Ministére de l’Enseignement Supérieur et de la Recherche (MESR) for a Ph.D. grant.
Published: 2015
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30. Four molecular superconductors isolated as nanoparticles

Author: Imane Chtioui, Dominique de Caro, Christophe Faulmann, Manon Bergez-Lacoste, Jordi Fraxedas, Soukaina Foulal, James S. Brooks, Kane Jacob, Eden Steven, Belén Ballesteros, Laurel Winter, Lydie Valade, Pascale Satgé-De Caro, State of Florida, Ministère de l’Enseignement Supérieur et de la Recherche Scientifique (Algérie), Centre National de la Recherche Scientifique (France), National Science Foundation (US), Department of Energy (US), Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Agro-Industrielle (LCA), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Toulouse, Universitat Autònoma de Barcelona [Barcelona] (UAB), National High Magnetic Field Laboratory (NHMFL), Florida State University [Tallahassee] (FSU), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées, ICN2 - Institut Catala de Nanociencia i Nanotecnologia (ICN2), Consejo Superior de Investigaciones Cientificas, Barcelone, Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Chimie Agro-Industrielle (CAI), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques-Institut National de la Recherche Agronomique (INRA), Universitat Autònoma de Barcelona (UAB), National Science Foundation (NSF) [DMR-1309146], NSF [DMR-1157490], U.S. Department of Energy, French Centre National de la Recherche Scientifique (CNRS), French Ministere de l'Enseignement Superieur et de la Recherche (MESR), Centre National de la Recherche Scientifique - CNRS (FRANCE), Florida State University - FSU (USA), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Institut National de la Recherche Agronomique - INRA (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Universitat Autònoma de Barcelona - UAB (SPAIN), National High Magnetic Field Laboratory - NHMFL (Tallahassee, USA), Institut National Polytechnique de Toulouse - INPT (FRANCE), Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Institut National de la Recherche Agronomique (INRA)-Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université de Toulouse (UT)-Université de Toulouse (UT)
Subjects: Superconductivity, Matériaux, Nanoparticle, Nanotechnology, [CHIM.MATE]Chemical Sciences/Material chemistry, Electrochemistry, [SPI.MAT]Engineering Sciences [physics]/Materials, Ionic liquids, Inorganic Chemistry, chemistry.chemical_compound, Crystallography, chemistry, Bechgaard salts, Ionic liquid, Nanoparticles, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Particle size, Superconductors, Tetrathiafulvalene
Abstract: (TMTSF)2PF6 and (TMTSF)2ClO4 Bechgaard salts, (BEDT-TTF)2I3, and TTF[Ni(dmit)2]2 [TMTSF = tetramethyltetraselenafulvalene; BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene; TTF = tetrathiafulvalene; dmit = 1,3-dithiole-2-thione-4,5-dithiolate] are among the most popular molecular superconductors. They are grown as nanoparticles that exhibit properties in agreement with those of the bulk. The shape, size, and homogeneity of particles depend on the stabilizing agent and synthesis conditions. We report on the more recent conditions investigated (i) to produce nanoparticles of 35 nm for β-(BEDT-TTF)2I3, (ii) to reduce the particle size to 10–15 nm for TTF[Ni(dmit)2]2 and 3–5 nm for (TMTSF)2ClO4, and (iii) to improve the growth duration from days to one hour for (TMTSF)2PF6. Finally, we report evidence of superconductivity in (TMTSF)2ClO4 particles., Work done at the National High Magnetic Field Laboratory (NHMFL) was supported by the National Science Foundation (NSF) (DMR-1309146) (grant to J. S. B). The NHMFL was supported by the NSF Cooperative, Agreement Number DMR-1157490, the State of Florida, and the U.S. Department of Energy. Collaboration within the European Associated Laboratory TransPyrénéen (LEA) (program: “de la Molécule aux Matériaux”) is appreciated. Work done at the Laboratoire de Chimie de Coordination (LCC) was supported by the French Centre National de la Recherche Scientifique (CNRS). I. C. thanks the French Ministère de l’Enseignement Supérieur et de la Recherche (MESR) for a Ph.D. grant.
Published: 2014
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31. Nickel ethylene tetrathiolate polymers as nanoparticles: a new synthesis for future applications?

Author: Christophe Faulmann, Joe Chahine, Kane Jacob, Lydie Valade, Yannick Coppel, Dominique de Caro, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Morphology (linguistics), Ethylene, Materials science, Inorganic chemistry, Nanoparticle, chemistry.chemical_element, Bioengineering, 02 engineering and technology, Conductivity, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Metal ethylene tetrathiolate, General Materials Science, chemistry.chemical_classification, Microscopy, Molecular conductors, Ligand, General Chemistry, Polymer, 021001 nanoscience & nanotechnology, Condensed Matter Physics, NMR, Atomic and Molecular Physics, and Optics, 0104 chemical sciences, Nickel, chemistry, Chemical engineering, Modeling and Simulation, Ionic liquid, Nanoparticles, 0210 nano-technology
Abstract: Coordination polymers (CP) based on the ethylene tetrathiolate ligand (C2S4)4− and Ni2+, and previously isolated as insoluble conductive powders are grown as nanoparticles (NP) using ionic liquid (IL) as stabilizing agent. The time of addition of the IL determines the morphology, and consequently the properties of the CP. The smaller (10–20 nm) and soluble NP are obtained when IL is present at the complexation step. The mechanism of growth of NP is studied. The NP size is sensitive to the amount of IL and to the reaction temperature. NPs are studied by TEM/EDX, DLS, liquid- and solid-state NMR, and conductivity.
Published: 2013
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32. First nanoparticles of Bechgaard salts

Author: Dominique de Caro, Kane Jacob, Christophe Faulmann, Lydie Valade, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Absorption spectroscopy, Supporting electrolyte, Infrared, General Chemical Engineering, Inorganic chemistry, Nanoparticle, Salt (chemistry), 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, symbols.namesake, Long alkyl-chains quaternary ammonium salts, Liquides ioniques, Ammonium, chemistry.chemical_classification, Molecular superconductors, Supraconducteurs moléculaires, Nanoparticules, General Chemistry, 021001 nanoscience & nanotechnology, sels d'ammonium quaternaires à longues chaînes alkyles, 0104 chemical sciences, Ionic liquids, chemistry, Bechgaard salts, Sels de Bechgaard, Ionic liquid, symbols, Nanoparticles, 0210 nano-technology, Raman spectroscopy
Abstract: 1631-0748; Abstract Well-dispersed nanoparticles of the superconducting Bechgaard salts, namely (TMTSF)2PF6 and (TMTSF)2ClO4, have been electrochemically grown in organic solution in the presence of a supporting electrolyte either being an ionic liquid or a long alkyl-chains quaternary ammonium salt. Nanoparticles exhibit sizes in the 20-75 nm range. Nanoparticle powders have been characterized by infrared, Raman, visible absorption spectroscopy, and by preliminary transport measurements at room temperature.
Published: 2013
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33. Nanoparticles of molecule-based conductors

Author: Christophe Faulmann, Emile Perez, Kane Jacob, Jordi Fraxedas, Imane Chtioui, Dominique de Caro, Diane Van Dorsselaer, Souad El Hajjaji, Lionel Salmon, Abdelaziz Sabbar, Lydie Valade, Sophie Franceschi, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Faculté des sciences [Rabat], Université Mohammed V de Rabat [Agdal], Interactions moléculaires et réactivité chimique et photochimique (IMRCP), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Université Mohammed V de Rabat [Agdal] (UM5), Université de Toulouse (UT)-Institut Ecologie et Environnement (INEE), Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Fédération de Recherche Fluides, Energie, Réacteurs, Matériaux et Transferts (FERMAT), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), and Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Superconductivity, chemistry.chemical_classification, Chemistry, Vapor pressure, Nanoparticle, Nanotechnology, 02 engineering and technology, General Chemistry, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Catalysis, 0104 chemical sciences, chemistry.chemical_compound, Ionic liquid, Materials Chemistry, Molecule, 0210 nano-technology, Electrical conductor, Nanoscopic scale
Abstract: State of the art molecule-based conductors that have been isolated as nanoparticles are reviewed. Research efforts in this field is justified by their insolubility and low vapour pressure, making their integration into electronic devices difficult. Their availability as nanoparticles would allow researchers to study their properties at the nanoscale and as stable dispersions, offering new opportunities for processing. Molecular conductors and superconductors that have been isolated as nanoparticles are: TTF·TCNQ, TTF[Ni(dmit) 2]2, TTFCl0.77 and TTFBr0.59, (BEDT-TTF)Cl0.66 and (BEDT-TTF)2Br, (TMTSF) 2ClO4 and (TMTSF)2PF6. Nanoparticle formation and shape depend on the stabilizing agent used for controlling the growth: ionic liquids, long-chain ammonium salts or neutral liquid polymers. The conductivities of the nanoparticle powders are reported. © 2013 The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
Published: 2013
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34. Functionalization of non-activated C-H bonds of alkanes: An effective and recyclable catalytic system based on fluorinated silver catalysts and solvents

Author: Pedro J. Pérez, M. Ángeles Fuentes, Michel Etienne, Kane Jacob, Laure Vendier, Bianca K. Muñoz, Ana Caballero, Universidad de Huelva, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: 010405 organic chemistry, Ligand, fluorous catalysis, Organic Chemistry, Regioselectivity, General Chemistry, 010402 general chemistry, 01 natural sciences, Medicinal chemistry, Catalysis, 0104 chemical sciences, Hexane, carbenes, chemistry.chemical_compound, chemistry, Ethyl diazoacetate, Acetone, Organic chemistry, biphasic catalysis, Diazo, alkanes, silver, Tetrahydrofuran
Abstract: The complexes F(n)-Tp(4Bo,3Rf)Ag(L) (F(n)-Tp(4Bo,3Rf)=a perfluorinated hydrotris(indazolyl) borate ligand; L=acetone or tetrahydrofuran) efficiently catalyze the functionalization of non-activated alkanes such as hexane, 2,3-dimethylbutane, or 2-methylpentane by insertion of CHCO(2)Et units (from N(2)CHCO(2)Et, ethyl diazoacetate, EDA) into their C-H bonds. The reactions are quantitative (EDA-based), with no byproducts derived from diazo coupling being formed. In the case of hexane, the functionalization of the methyl C-H bonds has been achieved with the highest regioselectivity known to date with this diazo compound. This catalytic system also operates under biphasic conditions by using fluorous solvents such as Fomblin or perfluorophenanthrene. Several cycles of catalyst recovery and reuse have been performed, with identical chemo- and regioselectivities.
Published: 2013
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35. 'TTF[Ni(dmit)2]2 :Now as Nanoparticles'

Author: Dominique de Caro, Christophe Faulmann, Lydie Valade, Kane Jacob, Lydie Viau, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), and Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC)
Subjects: Superconductivity, Diffraction, Materials science, General Chemical Engineering, Inorganic chemistry, Infrared spectroscopy, Nanoparticle, 02 engineering and technology, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Crystallography, chemistry.chemical_compound, chemistry, Ionic liquid, Molecule, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract: Well-dispersed nanoparticles of the molecule-based superconductor TTF[Ni(dmit) 2 ] 2 have been prepared in organic solution in the presence of an imidazolium- or a long-alkyl chains quaternary ammonium-based ionic liquid. TTF[Ni(dmit) 2 ] 2 nanoparticles exhibit mean diameters in the 17–27 nm range. Nanoparticle powders have been characterized by infrared spectroscopy, X-ray diffraction, and by transport measurements at room temperature.
Published: 2012
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36. First TTF-based conductor nanoparticles by electrocrystallization

Author: Lydie Valade, Dominique de Caro, Christophe Faulmann, Kane Jacob, Soumia Mazzi, Marie-Thérèse Carayon, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), and Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Supporting electrolyte, Inorganic chemistry, chemistry.chemical_element, Nanoparticle, 02 engineering and technology, Conductivity, 010402 general chemistry, 01 natural sciences, symbols.namesake, chemistry.chemical_compound, Materials Chemistry, Molecule, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Molecular conductors, Chemistry, Mechanical Engineering, Metals and Alloys, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, Electrocrystallization, Mechanics of Materials, Electrode, symbols, Tetrathiafulvalene, Nanoparticles, 0210 nano-technology, Raman spectroscopy, Platinum, Long alkyl-chain quaternary ammonium salts
Abstract: International audience; Well-dispersed spherical nanoparticles of the mixed-valence conductor TTFCl0.77 have been electrochemically grown on a platinum electrode in the presence of long-alkyl chains quaternary ammonium salts acting as both supporting electrolyte and protecting agent. The nanoparticles prepared at room temperature under galvanostatic conditions exhibit sizes ranging from 50 to 150 nm. Conducting molecule-based nanoparticles have been studied by X-ray diffraction, infrared and Raman spectroscopy. Their room-temperature conductivity has been measured to about 0.2 S cm−1.
Published: 2012
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37. Structural Influence on the Photochromic Response of a Series of Ruthenium Mononitrosyl Complexes

Author: Pascal G. Lacroix, Sonia Ladeira, Benoit Cormary, Kane Jacob, Isabelle Malfant, Dominik Schaniel, Theo Woike, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Technische Universität Dresden = Dresden University of Technology (TU Dresden), Cristallographie, Résonance Magnétique et Modélisations (CRM2), and Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Models, Molecular, Stereochemistry, chemistry.chemical_element, 010402 general chemistry, Crystallography, X-Ray, 01 natural sciences, Ruthenium, Inorganic Chemistry, chemistry.chemical_compound, Photochromism, Transition metal, Metastability, Pyridine, Organometallic Compounds, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Physical and Theoretical Chemistry, Linkage isomerism, Molecular Structure, 010405 organic chemistry, Chemistry, Ligand, Photochemical Processes, 0104 chemical sciences, Crystallography, Quantum Theory, Ground state, Nitroso Compounds
Abstract: In mononitrosyl complexes of transition metals two long-lived metastable states corresponding to linkage isomers of the nitrosyl ligand can be induced by irradiation with appropriate wavelengths. Upon irradiation, the N-bound nitrosyl ligand (ground state, GS) turns into two different conformations: isonitrosyl O bound for the metastable state 1 (MS1) and a side-on nitrosyl conformation for the metastable state 2 (MS2). Structural and spectroscopic investigations on [RuCl(NO)py(4)](PF(6))(2)·1/2H(2)O (py = pyridine) reveal a nearly 100% conversion from GS to MS1. In order to identify the factors which lead to this outstanding photochromic response we study in this work the influence of counteranions, trans ligands to the NO and equatorial ligands on the conversion efficiency: [RuX(NO)py(4)]Y(2)·nH(2)O (X = Cl and Y = PF(6)(-) (1), BF(4)(-) (2), Br(-)(3), Cl(-) (4); X = Br and Y = PF(6)(-) (5), BF(4)(-) (6), Br(-)(7)) and [RuCl(NO)bpy(2)](PF(6))(2) (8), [RuCl(2)(NO)tpy](PF(6)) (9), and [Ru(H(2)O)(NO)bpy(2)](PF(6))(3) (10) (bpy = 2,2'-bipyridine; tpy = 2,2':6',2"-terpyridine). Structural and infrared spectroscopic investigations show that the shorter the distance between the counterion and the NO ligand the higher the population of the photoinduced metastable linkage isomers. DFT calculations have been performed to confirm the influence of the counterions. Additionally, we found that the lower the donating character of the ligand trans to NO the higher the photoconversion yield.
Published: 2012
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38. Vibrational and Optical Studies of Organic Conductor Nanoparticles

Author: Lydie Valade, Dominique de Caro, Matthieu Souque, and Kane Jacob
Subjects: chemistry.chemical_classification, chemistry.chemical_compound, Crystallography, Materials science, chemistry, Infrared spectroscopy, Electron donor, Crystal structure, Electron acceptor, Conductivity, Tetracyanoquinodimethane, Acceptor, Tetrathiafulvalene
Abstract: To create free electrons in organic solids and thus generate an organic material exhibiting electrical conductivity, a simple way is to build an organic complex, in which there is a charge transfer from the atoms or molecules of an electron donor (D) to those of an electron acceptor (A). In 1973, the charge transfer salt TTF·TCNQ (donor: tetrathiafulvalene, TTF; acceptor: tetracyanoquinodimethane, TCNQ) was synthesized (figure 1) (Ferraris et al., 1973). In TTF·TCNQ single crystals, TTF and TCNQ form segregated columnar stacks along the b-axis of the crystal structure. The interplanar spacings in the TTF and TCNQ molecular stacks at room temperature are 3.47 A and 3.17 A, respectively (Kistenmacher et al., 1974). The TTF and TCNQ molecular planes tilt at an angle of 24.5 ° and 34.0 °, respectively with respect to the b-axis forming a herringbone arrangement. As single crystals, this compound behaves like a metal (the dc conductivity increases with decreasing temperature) down to 54 K, temperature at which it undergoes a metal-to-semiconductor transition. The maximum of conductivity in TTF·TCNQ is along the b-axis (about 600 1 cm1). Conductivity values range from 10−2 to 1 1 cm1 in a direction perpendicular to the direction of maximum conductivity. The amount of charge transfer from the TTF donor molecule to the TCNQ acceptor molecule has been investigated by various techniques. Using X-ray photoelectron spectroscopy, a value of 0.56  0.05 has been extracted from the shape of the S2p signal (Ikemoto et al., 1977). Values in the range 0.500.60 have been obtained by a numerical integration of X-ray diffraction amplitudes (Coppens, 1975). However, the most convenient technique is based on infrared spectroscopy. Using the linear correlation of the nitrile stretching mode for TCNQ as a function of the degree of charge transfer, a value of 0.59  0.01 has been obtained (Chappell et al., 1981). Although synthesized for many years, TTF·TCNQ currently attracts much interest because of its interesting physical properties. Moreover, it is the one-dimensional conductor which is the most intensively processed in forms others than single crystals. For instance, TTF·TCNQ was prepared as thin films on (100)-oriented alkali halide substrates (Fraxedas et al., 2002), as self-organized monolayers on Au(111) (Yan et al., 2009), or as nanowires on stainless steel conversion coatings (Savy et al., 2007). We report in this chapter the preparation and spectral studies of TTF·TCNQ prepared as nanoparticles.
Published: 2012

39. Highly fluorinated aryl-substituted tris(indazolyl)borate thallium complexes: diverse regiochemistry at the B-N bond

Author: Kane Jacob, Viet-Hoang Nguyen, Bianca K. Muñoz, Wilfried-Solo Ojo, Michel Etienne, Sergio Gonell, Emmanuelle Despagnet-Ayoub, and Laure Vendier
Subjects: Trifluoromethyl, Hydrogen bond, Aryl, Regioselectivity, chemistry.chemical_element, Fluorine-19 NMR, Borohydride, Medicinal chemistry, Inorganic Chemistry, chemistry.chemical_compound, chemistry, Structural isomer, Organic chemistry, Thallium, Physical and Theoretical Chemistry
Abstract: The synthesis and characterization (mainly by (19)F NMR and X-ray diffraction) of highly fluorinated aryl-4,5,6,7-tetrafluoroindazoles and their corresponding thallium hydrotris(indazolyl)borate complexes are reported [aryl = phenyl, pentafluorophenyl, 3,5-dimethylphenyl, 3,5-bis(trifluoromethyl)phenyl]. Thanks to N-H···N hydrogen bonds, the indazoles crystallize as dimers that pack differently depending on the nature of the aryl group. The thallium hydrotris(indazolyl)borate complexes Tl[Fn-Tp(4Bo,3aryl)] resulting from the reaction of aryl-4,5,6,7-tetrafluoroindazoles [aryl = phenyl, 3,5-dimethylphenyl, 3,5-bis(trifluoromethyl)phenyl] with thallium borohydride adopt overall C(3v) symmetry with the indazolyl groups bound to boron via their N-1 nitrogen in a conventional manner. When the perfluorinated pentaphenyl-4,5,6,7-tetrafluoroindazole is reacted with thallium borohydride, a single regioisomer of C(s) symmetry having one indazolyl ring bound to boron via its N-2 nitrogen, TlHB(3-pentafluorophenyl-4,5,6,7-tetrafluoroindazol-1-yl)(2)(3-pentafluorophenyl-4,5,6,7-tetrafluoroindazol-2-yl) Tl[F27-Tp((4Bo,3C6F5)*)], is obtained for the first time. Surprisingly, the perfluorinated dihydrobis(indazolyl)borate complex Tl[F(18)-Bp(3Bo,3C6F5)], an intermediate on the way to the hydrotris(indazolyl)borate complex, has C(s) symmetry with two indazolyl rings bound to boron via N-2. The distortion of the coordination sphere around Tl and the arrangement of the complexes in the crystal are discussed.
Published: 2012

40. Co-Design of Antenna and LNA for 1.7 - 2.7 GHz

Author: Bhaskar Gudey, Bala and Kane, Jacob
Abstract: In a radio frequency (RF) system, the front-end of a radio receiver consists of an active antenna arrangement with a conducting mode antenna along with an active circuit. This arrangement helps avoid losses and SNR degradation due to the use of a coaxial cable. The active circuit is essentially an impedance matching network and a low noise amplification (LNA) stage. The input impedance of the antenna is always different from the source impedance required to be presented at the LNA input for maximum power gain and this gives rise to undesired reflections at the antenna-LNA junction. This necessitates a matching network that provides the impedance matching between the antenna and the LNA at a central frequency (CF). From the Friis formula it is seen that the total noise figure (NF) of the system is dependent on the noise figure and gain of the first stage. So, by having an LNA that provides a high gain (typically >15 dB) which inserts minimum possible noise (desirably < 1 dB), the overall noise figure of the system can be maintained low. The LNA amplifies the signal to a suitable power level that will enable the subsequent demodulation and decoding stages to efficiently recover the original signal. The antenna and the LNA can be matched with each other in two possible ways. The first approach is the traditional method followed in RF engineering where in both the antenna and LNA are matched to 50 Ω terminations and connected to each other. In this classical method, the antenna and LNA are matched to 50 Ω at the CF and does not take into account the matching at other frequencies in the operation range. The second approach employs a co-design method to match the antenna and LNA without a matching network or with minimum possible components for matching. This is accomplished by varying one or more parameters of either the antenna or LNA to control the impedances and ultimately achieve a matching over a substantial range of frequencies instead at the CF alone. The co-design method is shown to provide higher gain and a lower NF with reduced number of components, cost and size as compared to the classical method. The thesis work presented here is a study, design and manufacturing of an antenna-LNA module for a wide frequency range of 1.7 GHz – 2.7 GHz to explore the gain and NF improvements in the co-design approach. Planar micro strip patch antennas and GaAs E-pHEMT transistor based LNA’s are designed and the matching and co-design are simulated to test the gain and NF improvements. Furthermore, fully functional prototypes are developed with Roger R04360 substrate and the results from simulations and actual measurements are compared and discussed
Published: 2012

41. Nanoparticles of organic conductors: synthesis and application as electrode material in organic ﬁeld eﬀect transistors

Author: Christophe Faulmann, Jordi Fraxedas, Kane Jacob, Tomofumi Kadoya, Lydie Valade, Takehiko Mori, Dominique de Caro, Hanan Hahioui, Lydie Viau, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Instituto de Ciencia de Materiales de Aragón [Saragoza, España] (ICMA-CSIC), University of Zaragoza - Universidad de Zaragoza [Zaragoza], Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), and Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC)
Subjects: Inorganic chemistry, Nanoparticle, 02 engineering and technology, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Catalysis, 0104 chemical sciences, Solvent, chemistry.chemical_compound, chemistry, Ionic liquid, Materials Chemistry, Acetone, Field-effect transistor, 0210 nano-technology, Acetonitrile, Dispersion (chemistry), Electrical conductor, ComputingMilieux_MISCELLANEOUS
Abstract: Stabilization of TTF·TCNQ nanoparticles is studied by varying the ionic liquid nature and solvent medium. The best dispersion is obtained in an acetonitrile/acetone mixture and the smaller size by using [BMIM][BF4], as a stabilizing ionic liquid. Applications of well-dispersed TTF·TCNQ nanoparticles (mean diameter of about 35 nm) as electrode material in organic field-effect transistors are also reported.
Published: 2011
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42. A New Perfluorinated F21-Tp Scorpionate Ligand: Enhanced Alkane Functionalization by Carbene Insertion with (F21-Tp)M Catalysts (M = Cu, Ag)

Author: Laure Vendier, Emmanuelle Despagnet-Ayoub, Ana Caballero, M. Mar Diaz-Requejo, Kane Jacob, Michel Etienne, Eleuterio Álvarez, and Pedro J. Pérez
Subjects: Alkane, chemistry.chemical_classification, Silver, Ligand, Organic Chemistry, Inorganic chemistry, Scorpionate ligand, Medicinal chemistry, Catalysis, Inorganic Chemistry, Metal, X-ray, chemistry.chemical_compound, Ethyl diazoacetate, chemistry, Perfluorinated, Metal complexes, visual_art, Alkanes, visual_art.visual_art_medium, Carbenes, Physical and Theoretical Chemistry, Trifluoromethanesulfonate, Carbene
Abstract: 9 páginas, 3 figuras, 2 tablas, 6 esquemas., The new tris(indazolyl)borate ligand [F21-Tp4Bo,3CF3]Tl (1) has been prepared and structurally characterized. The reaction of its thalium salt with copper iodide or silver triflate afforded the complexes [F21-Tp4Bo,3CF3]ML (M = Cu, L = NCMe, 2; M = Ag, L = Me2CO, 4), from which the carbonyl adducts [F21-Tp4Bo,3CF3]M(CO) (M = Cu, 3; M = Ag, 5) have also been obtained. Complexes 2−5 have been characterized by spectroscopic and X-ray studies, from which the existence of electron-deficient metal centers could be envisaged. Complexes 2 and 4 have been employed as catalysts for the reaction of alkanes and cycloalkanes with ethyl diazoacetate. The silver complex displays excellent catalytic activity for the insertion of the carbene into the alkane CH bonds. Functionalized products are obtained in high yield (>90%) with low catalyst loadings (0.5%). TON values of 200 have been reached, 10 times higher than any other group 11 metal-based catalyst already reported for this transformation., We thank the MEC for financial support (CTQ2005-00324), the ERA Chemistry Programme, and the Junta de Andalucía (P07-FQM-2870). A.C. thanks the MEC for a research fellowship (Ramón y Cajal Program).
Published: 2008

43. The structure of fluorinated indazoles: The effect of the replacement of a H by a F atom on the supramolecular structure of NH-indazoles

Author: Michel Etienne, José Elguero, Johannes F. Teichert, Kane Jacob, Ibon Alkorta, Pascal Oulié, Rosa M. Claramunt, Carlos Pérez Medina, Concepción López, and Laure Vendier
Subjects: Crystal, Crystallography, Hydrogen, Group (periodic table), Chemistry, Hydrogen bond, Atom, Materials Chemistry, Supramolecular chemistry, chemistry.chemical_element, General Chemistry, Nuclear magnetic resonance spectroscopy, Catalysis
Abstract: The structures of three NH-indazoles (3-methyl, 3-trifluoromethyl and 3-trifluoromethyl-4,5,6,7-tetrafluoroindazoles) have been determined by X-ray crystallography. These three compounds, together with 3-methyl-4,5,6,7- tetrafluoroindazole, whose X-ray structure could not be determined, have been studied using multinuclear magnetic resonance spectroscopy, including solid-state CPMAS. They all are 1H-tautomers. In the crystal, 3-methyl-1H-indazole forms hydrogen bonded dimers, whereas 3-trifluoromethyl-1H- indazole and 3-trifluoromethyl-4,5,6,7-tetrafluoro-1H-indazole crystallize as catemers. These catemers are chiral space group P32. They are the first examples of indazoles crystallizing in the form of helices of three-fold screw axis. Attempts at rationalizing this behavior on the basis of supramolecular interactions (hydrogen bonds and aromatic interactions) and GIAO calculations are discussed. © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.
Published: 2007

44. Electrical Conductivity and Spin Crossover: A New Achievement with a Metal Bis Dithiolene Complex

Author: Stéphane Dorbes, Christophe Faulmann, Lydie Valade, Isabelle Malfant, Stéphane Lampert, José A. Real, Kane Jacob, Marie-Liesse Doublet, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), and Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC)
Subjects: Condensed matter physics, 010405 organic chemistry, Chemistry, Cationic polymerization, 010402 general chemistry, 01 natural sciences, 0104 chemical sciences, 3. Good health, Inorganic Chemistry, Spin crossover, Electrical resistivity and conductivity, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Physical chemistry, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS
Abstract: Three new compounds based on the cationic complex [Fe(III)(3-R-salEen)(2)]+ (salEen stands for N-(2-ethylamino)ethyl)-salicylaldimine, R = H, CH(3)O) with the electroactive Ni(dmit)(2) species as a counterion (dmit stands for 1,3-dithia-2-thione-4,5-dithiolato) have been synthesized and structurally and magnetically characterized. Compound 1 ([Ni(dmit)(2)][Fe(3-OMe-salEen)(2)]. CH(3)OH) shows an apparent hysteresis loop, due to an irreversible desolvatation process. Compound 2 ([Ni(dmit)(2)](NO(3))[Fe(salEen)(2)](2)) exhibits a gradual and incomplete spin transition. Compound 3 ([Ni(dmit)(2)](5)[Fe(salEen)(2)](2), 6CH(3)CN) is a fractional oxidation state complex, which behaves like a semiconductor and exhibits a gradual but complete spin transition between 300 and 4 K.
Published: 2007
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45. Vibrational and Optical Studies of Organic Conductor Nanoparticles

Author: Dominique de Caro, Kane Jacob, Matthieu Souque, Lydie Valade, Dominique de Caro, Kane Jacob, Matthieu Souque, and Lydie Valade
Published: 2012
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46. Synthesis, X-ray crystal structures, optical properties and modelling data of neutral bis(1,2-dithiolene) nickel complexes of the “non-cyclic SR” family

Author: Bui, Thanh-Tuan, primary, Vuong, Minh Ha, additional, Bonneval, Bénédicte Garreau-de, additional, Alary, Fabienne, additional, Kane, Jacob, additional, Duhayon, Carine, additional, Sournia-Saquet, Alix, additional, and Moineau-Chane-Ching, Kathleen I., additional
Published: 2012
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47. Polymorphism and its effects on the magnetic behaviour of the [Fe(sal2-trien)][Ni(dmit)2] spin-crossover complex

Author: Christophe Faulmann, Joe Chahine, Kane Jacob, Lydie Valade, and Petra Ágota Szilágyi
Subjects: Crystallography, Polymorphism (materials science), Chemistry, Spin crossover, Intermolecular force, Materials Chemistry, General Chemistry, Crystal structure, equipment and supplies, human activities, Catalysis
Abstract: The syntheses, structural characterisation, and magnetic and spectroscopic properties of three new polymorphs of the spin-crossover complex [Fe(sal2-trien)][Ni(dmit)2] are reported. The results are discussed as a function of their intra- and intermolecular arrangement. Correlation of their crystal structures and magnetic properties suggest that some torsion angles play a significant role in the magnetic properties of this class of compounds. Intermolecular contacts are also of importance, and the nature of the short contacts between molecular species seems to be more crucial than their number in the allowance of spin-crossover.
Published: 2009
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48. Charge injection from organic charge-transfer salts to organic semiconductorsElectronic supplementary information (ESI) available: Experimental details of preparation of CT-salt dispersions and the device fabrication, output characteristics and table of transistor characteristics, and energy level estimation. See DOI: 10.1039/c1jm12783g

Author: Tomofumi Kadoya, Dominique de Caro, Kane Jacob, Christophe Faulmann, Lydie Valade, and Takehiko Mori
Abstract: Highly conducting films of organic charge-transfer (CT) salts are fabricated by a solution process from the dispersions stabilized by poly(vinylpyrrolidone). This method provides a general way to obtain conducting films of nonvolatile organic cation- and anion-radical salts with inorganic counter ions. Carrier injection from organic CT salts to organic semiconductors is investigated by using these films as electrodes in organic field-effect transistors. Efficient hole injection is observed not only from organic cation-radical salts but also from anion-radical salts to pentacene and sexithiophene. Electron injection is dominant from both types of CT salts to C60, but hole injection and ambipolar characteristics are observed for cation-radical salts. The Fermi levels of the CT salts are discussed on the basis of these observations. [ABSTRACT FROM AUTHOR]
Published: 2011
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49. A New Perfluorinated F21-Tp Scorpionate Ligand: Enhanced Alkane Functionalization by Carbene Insertion with (F21-Tp)M Catalysts (M = Cu, Ag).

Author: Emmanuelle Despagnet-Ayoub, Kane Jacob, Laure Vendier, Eleuterio Álvarez, Ana Caballero, Michel Etienne, M. Mar Díaz-Requejo, and Pedro J. Pérez
Subjects: *MATHEMATICAL complexes, *CHEMICAL inhibitors, *LINE geometry, *ALKANES
Abstract: The new tris(indazolyl)borate ligand [F 21-Tp 4Bo,3CF3]Tl ( 1) has been prepared and structurally characterized. The reaction of its thalium salt with copper iodide or silver triflate afforded the complexes [F 21-Tp 4Bo,3CF3]ML (M = Cu, L = NCMe, 2; M = Ag, L = Me 2CO, 4), from which the carbonyl adducts [F 21-Tp 4Bo,3CF3]M(CO) (M = Cu, 3; M = Ag, 5) have also been obtained. Complexes 2− 5have been characterized by spectroscopic and X-ray studies, from which the existence of electron-deficient metal centers could be envisaged. Complexes 2and 4have been employed as catalysts for the reaction of alkanes and cycloalkanes with ethyl diazoacetate. The silver complex displays excellent catalytic activity for the insertion of the carbene into the alkane CH bonds. Functionalized products are obtained in high yield (>90%) with low catalyst loadings (0.5%). TON values of 200 have been reached, 10 times higher than any other group 11 metal-based catalyst already reported for this transformation. [ABSTRACT FROM AUTHOR]
Published: 2008
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50. The structure of fluorinated indazoles: the effect of the replacement of a H by a F atom on the supramolecular structure of NH-indazoles.

Author: Johannes Teichert, Pascal Oulié, Kane Jacob, Laure Vendier, Michel Etienne, Rosa M. Claramunt, Concepción López, Carlos Pérez Medina, Ibon Alkorta, and José Elguero
Subjects: X-ray crystallography, MAGNETIC resonance, SPECTRUM analysis, MAGNETIC fields
Abstract: The structures of three NH-indazoles (3-methyl, 3-trifluoromethyl and 3-trifluoromethyl-4,5,6,7-tetrafluoroindazoles) have been determined by X-ray crystallography. These three compounds, together with 3-methyl-4,5,6,7-tetrafluoroindazole, whose X-ray structure could not be determined, have been studied using multinuclear magnetic resonance spectroscopy, including solid-state CPMAS. They all are 1H-tautomers. In the crystal, 3-methyl-1H-indazole forms hydrogen bonded dimers, whereas 3-trifluoromethyl-1H-indazole and 3-trifluoromethyl-4,5,6,7-tetrafluoro-1H-indazole crystallize as catemers. These catemers are chiral space group P32. They are the first examples of indazoles crystallizing in the form of helices of three-fold screw axis. Attempts at rationalizing this behavior on the basis of supramolecular interactions (hydrogen bonds and aromatic interactions) and GIAO calculations are discussed. [ABSTRACT FROM AUTHOR]
Published: 2007
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