MnAPO-11 samples were synthesized from aqueous (MnAPO-11(A)) and ethylene glycol (MnAPO-11(NA)) media. The crystallinity of the samples was more when the synthesis was carried out in ethylene glycol. Chemical and thermogravimetric analyses reveal greater incorporation of Mn in the framework of MnAPO-11(NA) than in MnAPO-11(A). At least five different types of Mn(II) species are detected in the samples by ESR. The studies suggest that Mn is more homogeneously distributed in MnAPO-11(NA) than in MnAPO-11(A).