Synthesis and Characterization of a Tetrapodal NO44– Ligand and Its Transition Metal Complexes

Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R.; Chang, Christopher J.; Long, Jeffrey R.

doi:10.1021/acs.inorgchem.6b00908

Title: Synthesis and Characterization of a Tetrapodal NO₄^4– Ligand and Its Transition Metal Complexes

Journal Article · Tue Jul 12 00:00:00 EDT 2016 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.6b00908· OSTI ID:1480729

Axelson, Jordan C. ^[1]; Gonzalez, Miguel I. ^[1]; Meihaus, Katie R. ^[1]; Chang, Christopher J. ^[2]; Long, Jeffrey R. ^[3]

Univ. of California, Berkeley, CA (United States). Departments of Chemistry
Univ. of California, Berkeley, CA (United States). Departments of Chemistry, Molecular and Cell Biology and Howard Hughes Medical Institute; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
Univ. of California, Berkeley, CA (United States). Departments of Chemistry and Chemical and Biomolecular Engineering; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division

In this paper, we present the synthesis and characterization of alkali metal salts of the new tetraanionic, tetrapodal ligand 2,2'-(pyridine-2,6-diyl)bis(2-methylmalonate) (A4[PY(CO₂)₄], A = Li⁺, Na⁺, K⁺, and Cs⁺), via deprotection of the neutral tetrapodal ligand tetraethyl 2,2'-(pyridine-2,6-diyl)bis(2-methylmalonate) (PY(CO2Et)₄). The [PY(CO₂)₄]^4- ligand is composed of an axial pyridine and four equatorial carboxylate groups and must be kept at or below 0 °C to prevent decomposition. Exposing it to a number of divalent first-row transition metals cleanly forms complexes to give the series K₂[(PY(CO₂)₄)M(H₂O)] (M = Mn²⁺, Fe²⁺, Co²⁺, Ni²⁺, Zn²⁺). The metal complexes were comprehensively characterized via single-crystal X-ray diffraction,1H NMR and UV-vis absorption spectroscopy, and cyclic voltammetry. Crystal structures reveal that [PY(CO₂)₄]^4- coordinates in a pentadentate fashion to allow for a nearly ideal octahedral coordination geometry upon binding an exogenous water ligand. Additionally, depending on the nature of the charge-balancing countercation (Li⁺, Na⁺, or K⁺), the [(PY(CO₂)₄)M(H₂O)]^2- complexes can assemble in the solid state to form one-dimensional channels filled with water molecules. Aqueous electrochemistry performed on [(PY(CO₂)₄)M(H₂O)]^2- suggested accessible trivalent oxidation states for the Fe, Co, and Ni complexes, and the trivalent Co³⁺ species [(PY(CO₂)₄)Co(OH)]^2- could be isolated via chemical oxidation. Finally, the successful synthesis of the [PY(CO₂)₄]^4- ligand and its transition metal complexes illustrates the still-untapped versatility within the tetrapodal ligand family, which may yet hold promise for the isolation of more reactive and higher-valent metal complexes.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences, and Biosciences Division

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1480729

Journal Information:: Inorganic Chemistry, Vol. 55, Issue 15; ISSN 0020-1669

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

CCDC 1500123: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc022 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500124: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc033 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500125: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc044 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500126: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc055 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500127: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc066 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500128: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc077 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500129: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc088 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500130: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc099 The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500131: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0bb The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500132: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0cc The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500133: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0dd The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500134: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0ff The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500135: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0gg The current record is supplemented by this dataset	dataset	January 2016
CCDC 1500136: Experimental Crystal Structure Determination Axelson, Jordan C.; Gonzalez, Miguel I.; Meihaus, Katie R. https://doi.org/10.5517/ccdc.csd.cc1mc0hh The current record is supplemented by this dataset	dataset	January 2016

Title: Synthesis and Characterization of a Tetrapodal NO44– Ligand and Its Transition Metal Complexes

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Title: Synthesis and Characterization of a Tetrapodal NO₄^4– Ligand and Its Transition Metal Complexes