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3. Exploring the crystallisation of aspirin in a confined porous material using solid-state nuclear magnetic resonance.

Author

Juramy, Marie, Besson, Eric, Gastaldi, Stéphane, Ziarelli, Fabio, Viel, Stéphane, Mollica, Giulia, and Thureau, Pierre

Abstract

In this study, nuclear magnetic resonance (NMR) is used to investigate the crystallisation behaviour of aspirin within a mesoporous SBA-15 silica material. The potential of dynamic nuclear polarisation (DNP) experiments is also investigated using specifically designed porous materials that incorporate polarising agents within their walls. The formation of the metastable crystalline form II is observed when crystallisation occurs within the pores of the mesoporous structure. Conversely, bulk crystallisation yields the most stable form, namely form I, of aspirin. Remarkably, the metastable form II remains trapped within the pores of mesoporous SBA-15 silica material even 30 days after impregnation, underscoring its persistent stability within this confined environment. [ABSTRACT FROM AUTHOR]

Published
2025
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20. Supercritical CO2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid‐state NMR.

Author

Le, Dao, Frison, Amélie, Masmoudi, Yasmine, Bouledjouidja, Abir, Thureau, Pierre, Mollica, Giulia, Badens, Elisabeth, Ziarelli, Fabio, and Viel, Stéphane

Subjects
POLARIZATION (Nuclear physics), MAGIC angle spinning, NUCLEAR magnetic resonance spectroscopy, PROOF of concept, CARBON dioxide, POLYSTYRENE, POLYMERS
Abstract

In this study, supercritical CO2 (scCO2) was used to impregnate polymers with paramagnetic polarizing agents to prepare samples for dynamic nuclear polarization (DNP) solid‐state NMR (ssNMR) experiments. As a proof of concept, we impregnated polystyrene samples with bTbK, which stands for bis‐TEMPO‐bisketal where TEMPO is 2,2,6,6‐tetra‐methylpiperindin‐1‐oxyl. Substantial DNP signal enhancements could be measured on DNP‐enhanced 1H → 13C cross‐polarization (CP) magic‐angle spinning (MAS) spectra recorded at 9.4 T and ~100 K, reaching a maximum value of 8 in the most favorable case, which appeared comparable or even higher than what is typically obtained on similar systems for former sample preparation methods. These results highlight the potential of scCO2 impregnation as an efficient and possibly versatile methodology to prepare polymer samples for DNP ssNMR investigations. [ABSTRACT FROM AUTHOR]

Published
2022
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21. Stressing the differences in alizarin and purpurin dyes through UV-visible light absorption and 1H-NMR spectroscopies.

Author

Tissier, Roger-Charles, Rigaud, Baptiste, Thureau, Pierre, Huix-Rotllant, Miquel, Jaber, Maguy, and Ferré, Nicolas

Abstract

Three anthraquinone-based chromophores (9,10-anthraquinone, alizarin, purpurin) are compared from the point of view of their experimental and computed NMR and UV-visible light absorption spectra. Using a hybrid (explicit/implicit) solvent model, each proton chemical shift can be reproduced with an error of less than 7%, even when such protons are engaged in inter-molecular hydrogen bonds with the solvent or when the analyzed sample contains a significant amount of impurities, for instance, 9,10-anthraquinone in purpurin. All the steady-state UV-visible absorption spectra feature a significant vibrational progression in the first absorption band. The shape of the corresponding computed spectra, including vibronic couplings obtained with the adiabatic Hessian approach and the Franck–Condon and Herzberg–Teller approximation of the transition dipole, are in excellent agreement with the experimental ones. The importance and the nature of the vibronic couplings are different for the three molecules, even if they only differ by the number of hydroxyl groups. [ABSTRACT FROM AUTHOR]

Published
2022
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22. MRI assessment of multiple dipolar relaxation time ( T 1 D ) components in biological tissues interpreted with a generalized inhomogeneous magnetization transfer (ihMT) model

Author

Carvalho, Victor N.D., Hertanu, Andreea, Grélard, Axelle, Mchinda, Samira, Soustelle, Lucas, Loquet, Antoine, Dufourc, Erick J., Varma, Gopal, Alsop, David C., Thureau, Pierre, Girard, Olivier M., Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Chimie et Biologie des Membranes et des Nanoobjets (CBMN), Université de Bordeaux (UB)-École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Beth Israel Deaconess - Harvard Medical School, ANR-11-IDEX-0001,Amidex,INITIATIVE D'EXCELLENCE AIX MARSEILLE UNIVERSITE(2011), ANR-17-CE18-0030,verISMO,IRM du transfert d'aimantation inhomogène : vers un nouveau biomarqueur in vivo spécifique et sensible de la myéline(2017), European Project: 713750,H2020,H2020-MSCA-COFUND-2015,DOC2AMU(2016), Assistance Publique - Hôpitaux de Marseille (APHM)-Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS), and École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS)

Subjects
T 1D, MRI contrast, Myelin, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, Jeener-Broekaert, Dipolar relaxation time, Inhomogeneous magnetization transfer, Myelin Imaging, ihMT
Abstract

International audience; T 1D , the relaxation time of dipolar order, is sensitive to slow motional processes. Thus T 1D is a probe for membrane dynamics and organization that could be used to characterize myelin, the lipid-rich membrane of axonal fibers. A mono-component T 1D model associated with a modified ihMT sequence was previously proposed for in vivo evaluation of T 1D with MRI. However, experiments have suggested that myelinated tissues exhibit multiple T 1D components probably due to a heterogeneous molecular mobility. A bi-component T 1D model is proposed and implemented. ihMT images of ex-vivo, fixed rat spinal cord were acquired with multiple frequency alternation rate. Fits to data yielded two T 1D s of about 500 µs and 10 ms. The proposed model seems to further explore the complexity of myelin organization compared to the previously reported mono-component T 1D model.

Published
2020
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26. MRI assessment of multiple dipolar relaxation time (T1D) components in biological tissues interpreted with a generalized inhomogeneous magnetization transfer (ihMT) model

Author

Carvalho, Victor N.D., primary, Hertanu, Andreea, additional, Grélard, Axelle, additional, Mchinda, Samira, additional, Soustelle, Lucas, additional, Loquet, Antoine, additional, Dufourc, Erick J., additional, Varma, Gopal, additional, Alsop, David C., additional, Thureau, Pierre, additional, Girard, Olivier M., additional, and Duhamel, Guillaume, additional

Published
2020
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27. Structural investigations of polymer materials by DNP solid-state NMR

Author

Mollica, Giulia, Ziarelli, Fabio, Thureau, Pierre, Viel, Stéphane, Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Fédération des Sciences Chimiques de Marseille (FRSCM), Aix Marseille Université (AMU)-École Centrale de Marseille (ECM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Universitaire de France (IUF), Ministère de l'Education nationale, de l’Enseignement supérieur et de la Recherche (M.E.N.E.S.R.), ANR-11-IDEX-0001,Amidex,INITIATIVE D'EXCELLENCE AIX MARSEILLE UNIVERSITE(2011), European Project: 758498,ERC-2017-STG,STRUCTURE(2018), and École Centrale de Marseille (ECM)-Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[CHIM.POLY]Chemical Sciences/Polymers, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry
Abstract

International audience; Solid-state nuclear magnetic resonance (SSNMR) has established itself as an essential structural elucidation technique in polymer science because it can non-destructively provide unique molecular-level information with atomic resolution on complex macromolecular materials, especially when combined with complementary techniques such as scattering and computer simulation. The Achilles’ heel of NMR, however, is its low sensitivity due to the weak nuclear spin polarisation at thermal equilibrium, even at very high magnetic fields. One intriguing way to enhance NMR sensitivity is dynamic nuclear polarisation (DNP), which relies on the microwave-driven transfer of thermal electron spin polarisation to nuclei. DNP is attracting scientific attention owing to the availability of both high-power/high-frequency microwave sources and efficient DNP polarising agents (i.e., paramagnetic species used for doping diamagnetic samples to provide the source of electron polarisation for DNP). At moderately high magnetic fields (∼10 T), large DNP signal enhancements can now be readily obtained, which has led to unprecedented SSNMR applications. In this review, we describe the requirements for high-field DNP SSNMR and provide examples of its use for the structural analysis of organic polymer materials, so as to highlight its advantages and (current) limitations for the field.

Published
2019
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28. Multicomponent dipolar relaxation time (T1D) assessment in myelin using inhmogeneous magnetization transfer (ihMT) MRI

Author

Carvalho, Victor, Girard, Olivier M., Hertanu, Andreea, Soustelle, Lucas, Grélard, Axelle, Loquet, Antoine, Dufourc, Erick J., Varma, Gopal, Alsop, David C., Thureau, Pierre, Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), Chimie et Biologie des Membranes et des Nanoobjets (CBMN), Université de Bordeaux (UB)-École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Beth Israel Deaconess - Harvard Medical School, Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Duhamel, Guillaume, Assistance Publique - Hôpitaux de Marseille (APHM)-Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS), and École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [INFO.INFO-IM] Computer Science [cs]/Medical Imaging, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2019

29. On the dipolar order underlying broad macromolecular lines

Author

Girard, Olivier M., Carvalho, Victor, De Rochefort, Ludovic, Hertanu, Andreea, Thureau, Pierre, Varma, Gopal, Alsop, David C., Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Beth Israel Deaconess - Harvard Medical School, Assistance Publique - Hôpitaux de Marseille (APHM)-Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS), and Duhamel, Guillaume

Subjects
[SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [INFO.INFO-IM] Computer Science [cs]/Medical Imaging, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging
Abstract

International audience; Dipolar order has recently regained attention in MRI to analyze dipolar broadened lines in CEST and inhomogeneous Magnetization Transfer (ihMT), leading to new frequency irradiation patterns for enhanced saturation and access to an unexplored degree of freedom. A better understanding of dipolar order is of great interest to guide intuition and may lead to fundamental optimization of the ihMT technique, which is a promising tool providing new tissue contrasts. In this contribution we propose to review this concept, considering a simplified model of isolated proton pairs and the general Provotorov theory of RF saturation which applies to an ensemble of coupled spin.

Published
2019

30. Assessment of two T1D components within myelinated tissue with ihMT MRI

Author

Carvalho, Victor, Girard, Olivier M., Hertanu, Andreea, Mchinda, Samira, Soustelle, Lucas, Grélard, Axelle, Loquet, Antoine, Dufourc, Erick J., Varma, Gopal, Alsop, David C., Thureau, Pierre, Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), Chimie et Biologie des Membranes et des Nanoobjets (CBMN), Université de Bordeaux (UB)-École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Beth Israel Deaconess - Harvard Medical School, Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Assistance Publique - Hôpitaux de Marseille (APHM)-Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS), École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS), and Duhamel, Guillaume

Subjects
endocrine system, [SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, endocrine system diseases, immune system diseases, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [INFO.INFO-IM] Computer Science [cs]/Medical Imaging, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging, nutritional and metabolic diseases
Abstract

International audience; T1D, the relaxation time of the dipolar order, is a probe for membrane dynamics and organization that could be used to assess myelin integrity. A single-component T1D model associated with a modified ihMT sequence had been proposed for in vivo evaluation of T1D with MRI. However, experiments and simulations revealed that myelinated tissues exhibit multiple T1D components. A bi-component T1D model is proposed and validated. Fits in a rat spinal cord yield two T1Ds of about 10 ms and 400 μs. The results suggest that myelin has a dynamically heterogeneous organization.

Published
2019

31. Mesure de deux composantes T1D dans les tissus myélinisés par IRM ihMT

Author

Carvalho, Victor, Girard, Olivier M., Hertanu, Andreea, Mchinda, Samira, Soustelle, Lucas, Grélard, Axelle, Loquet, Antoine, Dufourc, Erick J., Varma, Gopal, Alsop, David C., Thureau, Pierre, Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Assistance Publique - Hôpitaux de Marseille (APHM)-Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS), Chimie et Biologie des Membranes et des Nanoobjets (CBMN), École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS), Beth Israel Deaconess - Harvard Medical School, Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Duhamel, Guillaume, Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), and Université de Bordeaux (UB)-École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [INFO.INFO-IM] Computer Science [cs]/Medical Imaging, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging, ComputingMilieux_MISCELLANEOUS
Abstract

National audience

Published
2019

32. MRI assessment of multiple dipolar relaxation time (T1D) components in biological tissues interpreted with a generalized inhomogeneous magnetization transfer (ihMT) model

Author

Carvalho, Victor N. D., Hertanu, Andreea, Grelard, Axelle, Mchinda, Samira, Soustelle, Lucas, Loquet, Antoine, Dufourc, Erick J., Varma, Gopal, Alsop, David C., Thureau, Pierre, Girard, Olivier M., Duhamel, Guillaume, Chimie et Biologie des Membranes et des Nanoobjets (CBMN), École Nationale d'Ingénieurs des Travaux Agricoles - Bordeaux (ENITAB)-Institut de Chimie du CNRS (INC)-Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS), and Admin, Oskar

Subjects
[CHIM.MATE] Chemical Sciences/Material chemistry, endocrine system, MRI contrast, endocrine system diseases, immune system diseases, Myelin, Jeener-Broekaert, Inhomogeneous magnetization transfer, Dipolar relaxation time, nutritional and metabolic diseases, [CHIM.MATE]Chemical Sciences/Material chemistry, Myelin Imaging, ihMT
Abstract

T1D, the relaxation time of dipolar order, is sensitive to slow motional processes. Thus T1D is a probe for membrane dynamics and organization that could be used to characterize myelin, the lipid-rich membrane of axonal fibers. A mono-component T1D model associated with a modified ihMT sequence was previously proposed for in vivo evaluation of T1D with MRI. However, experiments have suggested that myelinated tissues exhibit multiple T1D components probably due to a heterogeneous molecular mobility. A bi-component T1D model is proposed and implemented. ihMT images of ex-vivo, fixed rat spinal cord were acquired with multiple frequency alternation rate. Fits to data yielded two T1Ds of about 500mus and 10ms. The proposed model seems to further explore the complexity of myelin organization compared to the previously reported mono-component T1D model.

Published
2019

39. High Resolution Magic Angle Spinning (HR-MAS) NMR characterization of inhomogeneous magnetization transfer (ihMT) responsive samples

Author

Girard, Olivier M., Carvalho, Victor, Thureau, Pierre, Prevost, Valentin H., Mchinda, Samira, Varma, Gopal, Alsop, David C., Duhamel, Guillaume, Centre de résonance magnétique biologique et médicale (CRMBM), Aix Marseille Université (AMU)-Assistance Publique - Hôpitaux de Marseille (APHM)-Centre National de la Recherche Scientifique (CNRS), and BERNARD, Monique

Subjects
[SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [INFO.INFO-IM] Computer Science [cs]/Medical Imaging, [INFO.INFO-IM]Computer Science [cs]/Medical Imaging
Abstract

International audience; Inhomogeneous magnetization transfer (ihMT) is a promising technique for central nervous system imaging. Although ihMT signal is mostly observed in myelinated tissues, weaker ihMT signal may be revealed in other biological tissue. The fundamental relationship between the underlying NMR lineshape and the ihMT signal is still an open question. Here we investigate high resolution magic-angle spinning (HR-MAS) NMR to provide insight into the mechanisms underpinning line broadening of ihMT responsive samples. The resulting spectra evidence different dipolar Hamiltonian components contributing to line broadening and support ihMT as being dominated by inhomogeneous interaction in myelinated tissues.

Published
2017

40. Reducing the computational cost of NMR crystallography of organic powders at natural isotopic abundance with the help of 13C‐13C dipolar couplings.

Author

Thureau, Pierre, Sturniolo, Simone, Zilka, Miri, Ziarelli, Fabio, Viel, Stéphane, Yates, Jonathan R., and Mollica, Giulia

Subjects
*CHEMICAL shift (Nuclear magnetic resonance), *POLARIZATION (Nuclear physics), *CRYSTALLOGRAPHY, *NUCLEAR magnetic resonance, *POWDERS, *DENSITY functional theory
Abstract

Structure determination of functional organic compounds remains a formidable challenge when the sample exists as a powder. Nuclear magnetic resonance crystallography approaches based on the comparison of experimental and Density Functional Theory (DFT)‐computed 1H chemical shifts have already demonstrated great potential for structure determination of organic powders, but limitations still persist. In this study, we discuss the possibility of using 13C‐13C dipolar couplings quantified on powdered theophylline at natural isotopic abundance with the help of dynamic nuclear polarization, to realize a DFT‐free, rapid screening of a pool of structures predicted by ab initio random structure search. We show that although 13C‐13C dipolar couplings can identify structures possessing long range structural motifs and unit cell parameters close to those of the true structure, it must be complemented with other data to recover information about the presence and the chemical nature of the supramolecular interactions. [ABSTRACT FROM AUTHOR]

Published
2019
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42. Solid-State H-1 NMR Studies of Homonuclear Dipolar Couplings

Author

Thureau, Pierre, Mollica, Giulia, Ziarelli, Fabio, Viel, Stéphane, Institut de Chimie Radicalaire (ICR), Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Spectropôle - Aix Marseille Université (AMU SPEC), and Aix Marseille Université (AMU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[CHIM]Chemical Sciences
Abstract

International audience; We review here the different methodologies used to study H-1 homonuclear dipolar couplings in solid-state NMR. Because most protonated powder samples contain clusters of strongly coupled H-1 nuclei, structural studies based on the measurement of individual H-1 homonuclear dipolar couplings have long been severely restricted. Driven by faster MAS frequencies, higher magnetic fields, pulse sequence and computing developments, major improvements have been achieved in this field over the last decade. We describe here the solid-state NMR techniques that have been developed recently, with special attention to the experiments based on H-1 spin diffusion and double-quantum recoupling. For these experiments, a comprehensive description of the spin dynamics involved is provided. Finally, an overview of the most promising emerging techniques is also given.

Published
2014
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48. Corrigendum: Supercritical CO2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid‐state NMR.

Author

Le, Dao, Frison, Amélie, Masmoudi, Yasmine, Bouledjouidja, Abir, Thureau, Pierre, Mollica, Giulia, Badens, Elisabeth, Ziarelli, Fabio, and Viel, Stéphane

Subjects
POLARIZATION (Nuclear physics), MOLECULAR structure, MOLECULES, METHYL groups
Abstract

Each of the two carbons in alpha to the two nitroxide functions should bear two methyl groups, leading to the following corrected Scheme 1. In the published article SP [ sp [1] SP ] sp above: An error has been made in Scheme 1 on the molecular structure of bTbK (Scheme 1b). Corrigendum: Supercritical CO2 impregnation process applied to polymer samples preparation for dynamic nuclear polarization solid-state NMR. [Extracted from the article]

Published
2023
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