Journal
DALTON TRANSACTIONS
Volume -, Issue 32, Pages 3516-3525Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/b703660d
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- ICREA Funding Source: Custom
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The reactions between [Pd(P-P)(OTf)(2)] (where P-P = dppp or dppf) and two different bipyridyl ligands (L-1 = 1,3-bis(4-pyridylmethyl) urea and L-2 = 1,3-bis(pyridinylmethyl) benzenedicarboxamide) containing hydrogen-bonding units have been studied. The X-ray crystal structures of three of these assemblies have been solved showing them to be the [2 + 2] metallo-macrocycles [Pd(P-P)(L-n)](2)(OTf)(4) [P-P = dppp, n = 1, (1); P-P = dppp, n = 2, (2); P-P = dppf, n = 1, (3)]. To confirm whether the dimeric assembly of one of these species (1) is retained in solution, several investigations have been carried out. H-1 NMR studies in DMSO and high resolution ESI mass spectrometry have shown that 1 is in equilibrium with a larger [3 + 3] metallo-macrocycle. The equilibrium between these two species can be modified by changing the temperature, concentration or solvent. Also, addition of certain anions (e. g. [H2PO4](-)) to the mixture shifts the equilibrium favoring the formation of the [2 + 2] metallo-macrocycle over the [3 + 3] (initially present in a larger proportion).
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