ACS Publications. Most Trusted. Most Cited. Most Read
Site-Isolated Main-Group Tris(2-pyridyl)borate Complexes by Pyridine Substitution and Their Ring-Opening Polymerization Catalysis
My Activity

Figure 1Loading Img
    Article

    Site-Isolated Main-Group Tris(2-pyridyl)borate Complexes by Pyridine Substitution and Their Ring-Opening Polymerization Catalysis
    Click to copy article linkArticle link copied!

    Other Access OptionsSupporting Information (1)

    Inorganic Chemistry

    Cite this: Inorg. Chem. 2022, 61, 28, 10852–10862
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.inorgchem.2c01289
    Published July 1, 2022
    Copyright © 2022 American Chemical Society

    Abstract

    Click to copy section linkSection link copied!
    Abstract Image

    Tris(2-pyridyl)borates are an emerging class of scorpionate ligands, distinguished as exceptionally robust and electron-donating. However, the rapid formation of inert homoleptic complexes with divalent metals has so far limited their catalytic utility. We report site-isolating tris(2-pyridyl)borate ligands, bearing isopropyl, tert-butyl, and mesityl substituents at the pyridine 6-position to suppress the formation of inert homoleptic complexes. These ligands form the first 1:1 complexes between tris(2-pyridyl)borates and Mg2+, Zn2+, or Ca2+, with isopropyl-substituted TpyiPrH showing the most generality. Single-crystal X-ray diffraction analysis of the resulting complexes and comparison to density functional theory (DFT) models showed geometric distortions driven by steric repulsion between the pyridine 6-substituents and the hexamethyldisilazide (HMDS, N(SiMe3)2) anion. We show that this steric profile is a feature of the six-membered pyridine ring and contrasts with more established tris(pyrazolyl)borate and tris(imidazoline)borate scorpionate complexes. TpyiPrMg(HMDS) (1) and its zinc analogue are moderately active for the controlled polymerization of l-lactide, ε-caprolactone, and trimethylene carbonate. Furthermore, 1 gives controlled polymerization under more demanding melt-phase polymerization conditions at 100 °C, and block copolymerization of ε-caprolactone and trimethylene carbonate. These results will enable useful catalysis and coordination chemistry studies with tris(2-pyridyl)borates, and characterizes their structural complementarity to more familiar scorpionate ligands.

    Copyright © 2022 American Chemical Society

    Read this article

    To access this article, please review the available access options below.

    Get instant access

    Purchase Access

    Read this article for 48 hours. Check out below using your ACS ID or as a guest.

    Recommended

    Access through Your Institution

    You may have access to this article through your institution.

    Your institution does not have access to this content. Add or change your institution or let them know you’d like them to include access.

    Supporting Information

    Click to copy section linkSection link copied!

    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.inorgchem.2c01289.

    • Synthetic procedures, characterization data, and X-ray crystallographic analysis data (PDF)

    Accession Codes

    CCDC 20948142094817 and 2094819 contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, or by emailing [email protected], or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44 1223 336033.

    Terms & Conditions

    Electronic Supporting Information files are available without a subscription to ACS Web Editions. The American Chemical Society holds a copyright ownership interest in any copyrightable Supporting Information. Files available from the ACS website may be downloaded for personal use only. Users are not otherwise permitted to reproduce, republish, redistribute, or sell any Supporting Information from the ACS website, either in whole or in part, in either machine-readable form or any other form without permission from the American Chemical Society. For permission to reproduce, republish and redistribute this material, requesters must process their own requests via the RightsLink permission system. Information about how to use the RightsLink permission system can be found at http://pubs.acs.org/page/copyright/permissions.html.

    Cited By

    Click to copy section linkSection link copied!

    This article is cited by 9 publications.

    1. Mukundam Vanga, Vo Quang Huy Phan, Jiang Wu, Alvaro Muñoz-Castro, H. V. Rasika Dias. Thallium(I) Complexes of Tris(pyridyl)borates and a Comparison to Their Pyrazolyl Analogues. Inorganic Chemistry 2023, 62 (45) , 18563-18572. https://doi.org/10.1021/acs.inorgchem.3c02805
    2. Jin Qian, Robert J. Comito. Ethylene Polymerization with Thermally Robust Vanadium(III) Tris(2-pyridyl)borate Complexes. Organometallics 2023, 42 (12) , 1254-1258. https://doi.org/10.1021/acs.organomet.2c00568
    3. Brandon T. Watson, Mukundam Vanga, Anurag Noonikara-Poyil, Alvaro Muñoz-Castro, H. V. Rasika Dias. Copper(I), Silver(I), and Gold(I) Ethylene Complexes of Fluorinated and Boron-Methylated Bis- and Tris(pyridyl)borate Chelators. Inorganic Chemistry 2023, 62 (4) , 1636-1648. https://doi.org/10.1021/acs.inorgchem.2c04009
    4. Luis F. Sánchez-Barba, Andrés Garcés, Agustín Lara-Sánchez, Marta Navarro, David González-Lizana. Main advances in the application of scorpionate-based catalytic systems for the preparation of sustainable polymers. Chemical Communications 2025, 88 https://doi.org/10.1039/D4CC05014B
    5. Oscar F. González-Belman, J. Oscar C. Jiménez-Halla, Gerardo González, José E. Báez. Comparison of three elements (In, Sn, and Sb) in the same period as catalysts in the ring-opening polymerization of l -lactide: from amorphous to semicrystalline polyesters. RSC Advances 2024, 14 (47) , 34733-34745. https://doi.org/10.1039/D4RA06783E
    6. Enrique Francés-Poveda, Marc Martínez de Sarasa Buchaca, Carmen Moya-López, Iñigo J. Vitorica-Yrezabal, Isabel López-Solera, José A. Castro-Osma, Felipe de la Cruz-Martínez, Agustín Lara-Sánchez. Calcium-catalysed ring-opening copolymerisation of epoxides and cyclic anhydrides. Polymer Chemistry 2024, 15 (32) , 3238-3245. https://doi.org/10.1039/D4PY00379A
    7. Hong-Li An, Yuan Duan, Tian-Tian Chen, Lan-Qin Chai. Experimental and theoretical studies of trinuclear cadmium(II) complex containing pyridine ring: Synthesis, crystallographic, spectroscopic, TD/DFT calculations and Hirshfeld surface analysis. Journal of Molecular Structure 2024, 1310 , 138320. https://doi.org/10.1016/j.molstruc.2024.138320
    8. Jin Qian, Simran Simran, Robert J. Comito. Aluminum Tris(2-pyridyl)borates: Structure, reactivity and catalysis. Polyhedron 2024, 254 , 116931. https://doi.org/10.1016/j.poly.2024.116931
    9. James McQuade, Frieder Jäkle. Tris(pyridyl)borates: an emergent class of versatile and robust polydentate ligands for catalysis and materials applications. Dalton Transactions 2023, 52 (30) , 10278-10285. https://doi.org/10.1039/D3DT01665J

    Inorganic Chemistry

    Cite this: Inorg. Chem. 2022, 61, 28, 10852–10862
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.inorgchem.2c01289
    Published July 1, 2022
    Copyright © 2022 American Chemical Society

    Article Views

    1826

    Altmetric

    -

    Citations

    Learn about these metrics

    Article Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.

    Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.

    The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated.