Abstract. Aim of this work were experiments on growing new materials based on fluoride crystals with the colquiriite structure LiSr 0,8 Ca 0,2 F 6 , as well as the study of their phase composition. It is shown that for a series of crystals LiSr 0,8 Ca 0,2 F 6 distribution of reflections observed corresponds to the colquiriite structure, and the dependence of the lattice constant in the transition from LiCaAlF 6 crystal to LiSrAlF 6 crystal is linear. Also it found that absorption coefficient in mixed samples is much larger than in not mixed.