13C and 1H NMR characterization of the sodium perchlorafe complex of a new tetraoxatetraaza lipophilic cage ligand (1) derived from 1,7-dioxa-4,10-diazacyclododecane has been performed. 1H homonuclear correlated and 1H J-resolved two-dimensional experiments allowed the recognition of resonances due to different types of OCH2CH2N fragments, and of those of the hydrogens of the bridging chains. 13C resonances have been assigned on the basis of a 13C1H heteronuclear correlated two-dimensional experiment, together with the 13C NMR spectra of the synthetic precursors of 1. 13C spin-lattice relaxation times and NOE measurements established that the unique relaxation mechanism is dipole-dipole; the calculated rotational correlation times indicated that molecular reorientation is isotropic. 13C spectra and relaxation times obtained in different solvents showed that specific solute-solvent interactions are absent.
13C and 1H Two-dimensional NMR Characterization of the Sodium Perchlorate Complex of a New Tetraoxatetraaza Lipophilic Cage Ligand
MOLINARI, Henriette;
1986-01-01
Abstract
13C and 1H NMR characterization of the sodium perchlorafe complex of a new tetraoxatetraaza lipophilic cage ligand (1) derived from 1,7-dioxa-4,10-diazacyclododecane has been performed. 1H homonuclear correlated and 1H J-resolved two-dimensional experiments allowed the recognition of resonances due to different types of OCH2CH2N fragments, and of those of the hydrogens of the bridging chains. 13C resonances have been assigned on the basis of a 13C1H heteronuclear correlated two-dimensional experiment, together with the 13C NMR spectra of the synthetic precursors of 1. 13C spin-lattice relaxation times and NOE measurements established that the unique relaxation mechanism is dipole-dipole; the calculated rotational correlation times indicated that molecular reorientation is isotropic. 13C spectra and relaxation times obtained in different solvents showed that specific solute-solvent interactions are absent.
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