Description:
<jats:title>Abstract</jats:title><jats:p>The <jats:sup>1</jats:sup>H and <jats:sup>13</jats:sup>C NMR spectra of phenanthro[9,10‐<jats:italic>b</jats:italic>]thiophene were totally assigned using a combination of twodimensional NMR techniques. Direct hetcronuclear correlations were established using heteronuclear chemical shift correlation with semi‐selective proton decoupling. Two methods were employed to establish the identity of vicinal neighboring protons: heteronuclear relayed coherence transfer and low‐pass <jats:italic>J</jats:italic>‐filtered heteronuclear relayed coherence transfer. The versatilities of the two techniques were compared. Quaternary carbon resonance assignments and the orientations of individual spin systems relative to one another were accomplished using the proton‐detected long‐range heteronuclear multiple quantum coherence experiment (HMBC). Key long‐range inter‐ring proton homonuclear spin couplings served to confirm the orientations of the proton spin systems.</jats:p>