Mechanical alloying (MA) by planetary type ball mill of pure iron powders was carried out under the ammonia gas atmosphere. The powders of metastable iron nitrides was synthesized up to the nitrogen content of 23 at% N. The observed phases are identified as the super-saturated bcc solid solution for the nitrogen concentration below 14.5 at% N and the non-equilibrium hcp phase stable at high temperature for 20.8 at.% N. Magnetization of Fe-N powders gradually decreases with increasing the N concentration on contrast to the enhancement reported for the bct iron nitrides. Neutron diffraction experiments also provide detailed information concerning the local atomic structure surrounding the nitrogen atoms. The coordination number of Fe atom around a nitrogen atom for the iron nitride containing 9.5 at% N turns out to be 3.9 atoms. This suggests that a nitrogen atom is situated at a center of the tetrahedron formed by iron atoms.