NMR for polymorphism

Gihane attended the "Formation pratique RMN liquide et solide" organized by the Pole RMN of the Institut Chevreul in Villeneuve d'Ascq, a great way to learn from the best 🙂

Giulia and Johanna attended the France-Benelux joint conference organized in Lille. Bravo Johanna for the excellent talk "DNP NMR for probing crystallization of organic pharmaceutical compounds in confinement: the case of nicotinamide"! Thank you to the GERM for a wonderful organization.

Dr Elodie Salager from the CEMHTI in Orléans visited the lab after giving an excellent talk "Devices for electrochemical energy storage" as a part of the seminar series organized by the FSCM. Thank you Elodie 🙂

Johanna attended the Journée Grand Sud RMN in Bordeaux, where she gave the talk: "Hydrophilic polymer-based polarizing matrices for trapping and characterizing metastable pharmaceutical species by DNP NMR". She was awarded the best talk prize!! Bravo!

During the Symposium "SynergizingCrystallography andSpectroscopy: From Orderto Dynamics" organized by the Professors Pance Naumov, Asif Equbal and Brijit Yhomas of the NYU in Abu Dhabi, Giulia gave an invited talk "Crystallization of polymorphic solids in confinement studied by hyperpolarized solid-state NMR and microfluidics" at the ACS Virtual Spring Meeting, and Johanna gave a short talk "Hydrophilic polymer-based polarizing matrices: A new system for investigating the crystallization of pharmaceutical compounds by DNP NMR".

Pr. Marco Geppi from the University of Pisa visited the lab and was our invited speaker at the annual MoMa meeting organized between our group and the group of Danielle Laurencin at the Institut Charles Gerhardt in Montpellier. He gave an excellent talk on "NMR and NQR of functional materials for environmental, energy, and optoelectronic technologies". We had a very exciting couple of days!

New paper out on Crystal Growth & Des. where we discuss the structural properties of calcium carbonate hemihydrate, a very difficult polymorph to observe, using a combination of DFT calculations and solid-state NMR spectroscopic methods. The paper was chosen to be featured on the journal cover!

Céline gave a talk at the Chino-French Symposium on solid-state NMR for materials chemistry in Wuhan, and could visit the University NMR labs. A great experience!

Arianna Ghelardi, PhD candidate in the group of prof. Marco Geppi at the University of Pisa will join our group for 3 months. She will use MAS DNP to characterize cocrystalline pharmaceutical formulations. Welcome!

Giulia and Céline attended the Alpine Conference, where they gave two round tables on the investigation of crystallization in confinement using MAS DNP. They also attended the preconference tutorials on Sunday morning. It was a wonderful week of exciting science in a magnificent environment. So inspiring! This was also the first edition of the conference with Giulia as a chair of the organizing committee.

New article in collaboration with the group of Thierry Azaïs in Paris: we show how 43Ca MAS DNP spectroscopy can help reveal the formation of transient phases of calcium phosphate along the pathway to the formation of hydroxyapatite.

Giulia gave a talk "Hyperpolarising porous polymer matrices for MAS DNP" and Pierre presented a poster. A very vibrant scientific week in a wonderful location.

Bravo Céline for an excellent talk on her PhD thesis results! And thank you to the ICR for organizing this beautiful and fun day at the Iles du Frioul.

From left to right : Johanna Guazzelli, Samuel Cousin, Giulia Mollica, Céline Huart, Pierre Thureau, Romane Canovas, Gihane El Khiri, Minh Tu Ly, Fabio Ziarelli and Léa.

Congratulations to Gihane, who has been awarded a highly competitive InterED PhD fellowship. She will join our group in October 2025 to work on a PhD project investigating the effects of electric fields on crystallization under confinement by combining microfluidics and DNP-enhanced NMR. This project will be carried out under the joint supervision of Dr Giulia Mollica (ICR) and Dr. Stéphane Veesler (CINaM lab, Marseille).

New paper in collaboration with the group of Dennis Kurzbach at the University of Vienna: we show how, using a combination of magnetic resonance approaches including EPR, liquid NMR and MAS DNP, we reveal the existence of R5 peptides domains with different dynamic properties in biomimetic silica-peptides nanocapsules.

In the framework of a recently funded PHC ULYSSES exchange project, Prof. Stan Von Euw visited the lab and gave an excellent talk "Formation of Biominerals: What is Biological and what is Physicochemical?". Thank you Stan!

We recently published a new book chapter on Applications of MAS DNP to NMR Crystallography of Bulk Molecular Materials. The chapter is part of the book Modern NMR Crystallography, edited by D. L. Bryce. This volume is the second edition of the landmark book originally published in 2009 and edited by R. K. Harris.

In the framework of a recently funded PHC ULYSSES exchange project, Giulia and Céline visited Prof. Stan Von Euw's lab at the University of Galway. Giulia gave a talk to the department, Céline learned some lab work on corals to produce biomimetic materials, and they visited the magnificent Connemara. Thank you Stan, Sudeshna and Roisin for a wonderful week!

Gihane will join the group for 6 months on a M2 internship to work on the investigation of crystallization processes in pharmaceutical compounds using a combination of MAS DNP and microfluidics. In collaboration with the group of S. Veesler at the CINaM lab in Marseille.

Giulia was awarded a PHC ULYSSES grant to support a collaborative research project with Prof. Stanislas Von Euw (University of Galway) on the synthesis and characterization of bone-mimetic composite materials.

Giulia attended the SMARTER conference in Aveiro where she gave a talk "Crystallization in confinement studied by solid-state NMR and MAS DNP". She also gave an invited talk during the PANACEA meeting to provide her perspective as a spectroscopist on the use of solid-state NMR for pharmaceutical research.

At the 45th Annual Discussion Meeting and Joint Conference of the German, Danish, Polish, and Swedish Magnetic Resonance Communities 2024 Giulia gave the invited talk: "Crystallization in confinement studied by solid-state NMR and MAS DNP". A wonderful conference for a wonderful 4 days of science.

We show that confinement can stabilise metastable polymorphs of Aspirin that can be revealed with the help of solid state NMR.

The PRC project MICRONMR (PI: Giulia Mollica) was selected by ANR for funding! This will support the group research on the investigation of the mechanisms of crystallization of polymorphc organic solids from solution in confined environments constituted by microfluidics droplets or porous matrices. Coordinated by Giulia (ICR), the project involves three other partners from ICR, CINaM and FSCM labs in Marseille.

Bravo to Johanna, who brilliantly passed the examination to access the Chemical Science Doctoral School of Aix Marseille University (ED250). She will start her project on the study of confined crystallization in porous matrices in October 2024.

Céline and Minh Tu attended the PANACEA school on Solid State NMR in Venice. A wonderful location and organization, and very intense learning for a week full of NMR. Best way to set strong NMR foundations for the rest of their PhD.

Giulia gave an invited oral presentation to the ENC 2024, where she presented recent approaches to investigate metastable forms using solid state NMR and DNP

After almost two years of preparation by the CNRS and the association Femmes et Sciences, the photographic exhibition of "la Science Taille XXElles" finally opened to the public. The fantastic pictures taken by Vincent Moncorgé for this beautiful project are exposed in Marseille city center for a month. A beautiful and funny way to celebrate and promote the role of women in science, hoping this will be of inspiration to the young generation.

Giulia was invited by Prof. Brijith Thomas to give a seminar to the Chemistry department of the New York University in Adu Dhabi. A day full of discussion, but we managed to find a little time to visit a little bit. Thank you Brijith for this fantastic hospitality!

New paper out! Nice example of how DNP can help investigating frozen solution of Ca ions. Nice collaboration with the group of T. Azais at Sorbonne University.

Congratulations to Nghia for his new paper!

Giulia was invited by Prof. Dennis Kurzbach to give a seminar at the University of Vienna's Chemistry department. A day full of science in the magnificent Vienna. Thank you Dennis for your hospitality!

Welcome to the group to our PhD students Céline and Minh Tu!

We describe a new sample formulation for MAS DNP, showing that good sensitivity enhancements be obtained in water without glycerol (or other glass forming agents) simply by dissolving
high concentrations of electrolytes (such as NaCl or LiCl), which perturb the otherwise
unavoidable ice crystallization observed upon cooling, thereby reducing PA phase separation
and restoring DNP efficiency.

Giulia and Sam contributed to the European Researcher's Night in Marseille for the ICR through Speed Searching and Tabou de la Recherche...and met lots of young and old people interested in science.

Giulia was in Chamonix attending the Alpine Conference in solids where she gave tutorial on Sunday morning on solid state NMR of small molecules, and later during the week a round table presentation of polymorphic transformation in solids detected by MAS DNP. She also officially joined the organizing committee of the Alpine Conference!

Since the 2023 edition, Giulia is officially a member of the organizing committee of the Alpine Conference! Thank you to Jean-Nicolas and the other members for this exciting opportunity.

Giulia attended the ISMAR conference in Brisbane (AUS) where she gave an invited lecture on the study of polymorphic phase formation and transformation using hyperpolarized NMR. Stunning city and location, and excellent conference!

Giulia gave an invited talk to the IUCr conference in Melbourne. Fantastic meeting and location.

Pierre was at the Euromar 2023 in Glasgow where he gave a presentation on the use of MAS DNP for the early detection of polymorphic transformations in organic solids.

Prof Raffaella Demichelis from Curtin University in Australia visited the lab. She gave a beautiful talk on "Chemistry at the mineral-fluid interface: an atomic-scale perspective", very interesting topic and results. Thanks Raffaella!

Romain successfully defended his PhD! Congratulations to him and many thanks to the committee members Marco Geppi, Loriane Lecoq (rapporteurs), Christian Bonhomme and Danielle Laurencin for the nice discussion.

Céline Huart is the recipient of a PhD fellowship funded by the University of Aix-Marseille. Her interdisciplinary project will be carried out between the ICR and the CINaM laboratories in Marseille. She will combine hyperpolarized NMR and microfluidics for studying crystallization in confined environements. Stay tuned for exciting discoveries!

Congratulations to Samuel for his first publication with us! Great collaboration with Arthur Pinon (Gothenburg), Kenneth D.M. Harris and Colan E. Hughes (Cardiff) to show how far DNP can go to reveal the nanoscale morphology of mixtures of organic polymorphs.

Giulia and Sam attended the GERM conference on NMR in extreme conditions in Murol. Sam gave a beautiful talk on the study of morphology of organic particles by MAS DNP. We had very lively discussions and lot of fun in a beautiful environment by the lake, surrounded by ancient volcanos.

Giulia gave an invited talk to the spin hyperpolarization symposium organized by the University of Nottingham. Lots of interesting talks and discussions, food for the mind!

Congratulations Marie for this new pedagogical review presenting nuclear magnetic resonance strategies for time-resolved atomic-level investigation of crystallization from solution. There is an interesting section on perspectives and future directions in the field. Non specialists are welcome!

Another good news! Giulia has been appointed Distinguished Junior Member (Membre Distingué Junior) by the French Chemical Society.

Great news! Giulia has been nominated for the Grand Prix Départemental pour la Recherche en Provence. The ceremony for the prize attribution will take place on the 2nd of December.

We show that additives that serve crystallization can also enhance the sensitivity of DNP.

Congrats to Sam for successfully passing his CNRS audition. He is now permanent CNRS Researcher!
All the group wishes him lots of success!

Giulia, Sam and Romain were in Chamonix to attend the Alpine Conference on Magnetic Resonance. Giulia gave a talk on the use of MAS DNP to investigate cristallisation and achieving polymorph selection. Romain and Sam gave two round tables showing recent results on the study of crystallization in inorganic systems and spin diffusion. Awesome conference with very lively formal and informal discussions.

The overall aim of the project is to develop and apply an emerging NMR hyperpolarization technique, namely magic-angle spinning nuclear dynamic polarization (MAS-DNP), to characterize the process of formation of polymorphic organic solids. To apply: https://emploi.cnrs.fr/Offres/CDD/UMR7273-GIUMOL-019/Default.aspx

We showed how supercritical CO2 impregnation can be efficiently used to disperse radicals used as polarizing agents for DNP into polymeric materials, enhancing the sensitivity of NMR towards the structural analysis of challenging materials.

Giulia and Romain participated to the PANACEA workshop on ssNMR methods for pharmaceutical formulations hosted by the group of Prof. L. Emsley in EPFL Lausanne. We had a fantastic week of lively discussions between coaches and students in front of the spectrometer and off!

We welcomed the MISOTOP group from the Institut Charles Gerhardt of Montpellier for the third MoMa meeting, where Marie, Samuel and Nghia gave a talk. We had a lot of fun discussing NMR, DNP, isotopic enrichment through mechanochemistry, recoupling methods, spin diffusion and crystallization.

Giulia presented our recent results on the use of MAS DNP for the study of crystallization and selection of polymorph at the online conference HyMar, organized by the Italian discussion group on Magnetic Resonance, GIDRM.

Dr Arthur Pinon from University of Gothenburg will stay with us for two weeks to work on spin diffusion. Welcome Arthur!

Nghia is going to work on methodological development in ssNMR and DNP.

Marie successfully defended her PhD on the 4th of March.
Bravo Marie for your hard work, resilience and perseverance, and for a brilliant and living discussion with the jury. Thank you to Anne Lesage and Christian Bonhomme for accepting to review Marie's PhD manuscript and for sharing with us this very happy moment. And thank you to Kenneth Harris and Paul Hogkinson for accepting to be part of the committee.

We are always looking for motivated candidates to join our group. Please contact Giulia Mollica at giulia.mollica@univ-amu.fr for information about currently available positions and projects.

Congratulations to Marie for this very nice review article on NMR and DNP methods for investigating crystallization from solution.