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Arenediazonium substitution reactions occur when the diazonium group is substituted by various functional groups such as halides, hydroxyl, nitrile, etc. For instance, arenediazonium salts react with copper(I) salts of chloride, bromide, or cyanide to form corresponding aryl chlorides, bromides, and nitriles. These reactions are named Sandmeyer reactions. Although the mechanism of this reaction is complicated, as illustrated in Figure 1, they are believed to progress via an aryl copper...
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The hybridized nitrogen atom in amines possesses a lone pair of electrons and is bound to three substituents with a bond angle of around 108°, which is less than the tetrahedral angle of 109.5°. However, the C–N–H bond angle is slightly larger at 112°, with a carbon–nitrogen bond length of 147 pm. This carbon–nitrogen bond length of of amines is longer than the carbon–oxygen bond of alcohols (143 pm) but shorter than alkanes’...
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Different monodentate and polydentate ligands are used as complexing agents in complexometric titration reactions. The formation of complexes by mono- and bidentate ligands involves two or more intermediate steps, limiting their use as complexing agents. In comparison, polydentate ligands can form complexes with metal ions in a single-step process, facilitating sharper end points. This means polydentate ligands, such as amino carboxylic acid derivatives, are most commonly employed in...
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In complexation reactions, metal atoms or cations interact with ligands to form donor-acceptor adducts called metal complexes. Ligands that bind through one donor site are monodentate, ligands with two donor sites are bidentate, and those with more than two donor sites are polydentate ligands. For example, ethylene diamine is a bidentate ligand that binds through two nitrogen donor atoms, forming a five-membered ring. EDTA is a polydentate ligand that binds through four oxygen and two nitrogen...
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Nitrous acid, a weak acid, is prepared in situ via the reaction of sodium nitrite with a strong acid under cold conditions. This nitrous acid prepared in situ reacts with primary arylamines to form arenediazonium salts. Such reactions are known as diazotization reactions. As shown in Figure 1, the formation of arenediazonium salts begins with the decomposition of nitrous acid in an acidic solution to give nitrosonium ions.
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Lanthanide(III) complexation with an amide derived pyridinophane.

Goretti Castro1, Rufina Bastida, Alejandro Macías

  • 1Departamento de Química Inorgánica, Facultad de Ciencias, Universidade de Vigo , As Lagoas, Marcosende, 36310, Pontevedra, Spain.

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This study details lanthanide(III) complexes with a pyridinophane ligand, revealing their solid-state and solution structures. The complexes show consistent coordination and structural similarity across the lanthanide series, with varying flexibility.

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Area of Science:

  • Coordination Chemistry
  • Lanthanide Chemistry
  • Supramolecular Chemistry

Background:

  • Lanthanide(III) complexes are crucial in various applications.
  • Understanding their structural dynamics in solution is key for designing new materials.
  • Pyridinophane ligands offer unique coordination environments for metal ions.

Purpose of the Study:

  • To investigate the solid-state and solution structures of lanthanide(III) complexes with the TPPTAM ligand.
  • To determine the coordination number and structural behavior across the lanthanide series.
  • To elucidate the dynamic processes in solution using spectroscopic methods.

Main Methods:

  • X-ray crystallography for solid-state structure determination.
  • Luminescence lifetime measurements in H2O and D2O.
  • Lanthanide-induced paramagnetic NMR shift analysis.
  • Variable-temperature (VT) 1H NMR spectroscopy.

Main Results:

  • Crystal structures of 13 Ln(3+) complexes and one La(3+) complex determined.
  • Ligand consistently provides 9-fold coordination, completed to 10-fold by solvent or anion.
  • Structural similarity observed between solid-state and solution structures across the lanthanide series.
  • Luminescence data indicate coordinated water in solution for Eu(3+) and Tb(3+) complexes.
  • Complexes exhibit fluxional behavior for lighter lanthanides and increased rigidity for heavier ones.

Conclusions:

  • The TPPTAM ligand forms stable 10-coordinate lanthanide(III) complexes.
  • Solution structures closely mimic solid-state arrangements.
  • Dynamic properties of the complexes vary significantly with lanthanide ion size.
  • These findings provide insights into lanthanide coordination chemistry and structural dynamics.