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Synthesis of a tube-like tetra-bipyridyl, tetra-ethylacetato-calix[4]arene in 1,3-alternate conformation and the unexpected crystal structure of its [bpy(CoCl2)]3-[bpy(CoCl2)(H2O)] complex.

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Title: Synthesis of a tube-like tetra-bipyridyl, tetra-ethylacetato-calix[4]arene in 1,3-alternate conformation and the unexpected crystal structure of its [bpy(CoCl2)]3-[bpy(CoCl2)(H2O)] complex.
Authors: Mourer, Maxime, Bouizi, Younes, Leclerc, Sébastien, Malaman, Bernard, Regnouf de Vains, Jean-Bernard
Source: New Journal of Chemistry; 9/21/2024, Vol. 48 Issue 35, p15577-15589, 13p
Subject Terms: BIPYRIDINE, LIGANDS (Chemistry), CRYSTAL structure, X-ray diffraction, COBALT
Abstract: Treating conic tetra-para-ethylacetato-calix[4]arene (1) with 2.2 equivalents of K2CO3 and 4 equivalents of 6-bromomethyl-6′-methyl-2,2′-bipyridine affords the expected fully substituted podand, mainly in its 1,3-alternate conformation (2). This tube-like bipyridyl derivative 2 was subjected to complexation studies with CoCl2·6H2O to give a blue tetra cobalt(II) complex species (3). This complex displays a unique group of 6 aromatic bipyridyl 1H-NMR resonance signals demonstrating its high symmetry, while X-ray diffraction studies showed the presence of 3 expected tetrahedral bpy(CoCl2) units and 1 original trigonal bipyramidal unit involving the adjunction of a fifth ligand assumed to be H2O that could participate in the crystal scaffold. [ABSTRACT FROM AUTHOR]
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Database: Complementary Index
Description
Abstract:Treating conic tetra-para-ethylacetato-calix[4]arene (1) with 2.2 equivalents of K<subscript>2</subscript>CO<subscript>3</subscript> and 4 equivalents of 6-bromomethyl-6′-methyl-2,2′-bipyridine affords the expected fully substituted podand, mainly in its 1,3-alternate conformation (2). This tube-like bipyridyl derivative 2 was subjected to complexation studies with CoCl<subscript>2</subscript>·6H<subscript>2</subscript>O to give a blue tetra cobalt(II) complex species (3). This complex displays a unique group of 6 aromatic bipyridyl <sup>1</sup>H-NMR resonance signals demonstrating its high symmetry, while X-ray diffraction studies showed the presence of 3 expected tetrahedral bpy(CoCl<subscript>2</subscript>) units and 1 original trigonal bipyramidal unit involving the adjunction of a fifth ligand assumed to be H<subscript>2</subscript>O that could participate in the crystal scaffold. [ABSTRACT FROM AUTHOR]
ISSN:11440546
DOI:10.1039/d4nj02476a