Ni200/Fe16 (angstrom) multilayers were prepared by thermal evaporation in high vacuum onto mylar substrates at room temperature (RT). CEMS spectra at RT show the coexistence of several magnetic phases and out-of-plane magnetic anisotropy of the iron layers. SQUID measurements in the 4.2-350 K temperature range show in-plane magnetization of the Ni layers and a magnetic phase transition near 300 K.