Electron spin transient nutation method based on pulsed EPR spectroscopy was for the first time exploited for the identification of effective molecular spin multiplicities of a quasi one-dimensional organic high-spin polymer, showing the effective molecular high, spins with the spin quantum number S>2 featured in the nutation spectra of the polymer. It was concluded that the polymer was characterized as the mixture of molecular high-spin assemblages, supporting that the results from the susceptibility measurements of the same polymer suggested the existence of high-spin assemblages with an average S=2. The pulsed EPR nutation spectroscopy was also applied to high-spin systems of Mn
2+ (S=5/2) and Cr
3+ (S=3/2) in MgO powder, demonstrating the inherent advantages of the nutation spectroscopy. Particularly, the nutation method showed that Cr
3+ in MgO is located in lower symmetric environments distorted from octahedral symmetry. The nutation spectra for the Cr
3+-doped MgO powder indicated the occurrence of multiple quantum transitions for S=3/2.
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