Single crystals of the Y5Cu5Mg8, Y5Cu5Mg13, Y5Cu5Mg16 and YCuMg4 compounds were synthesized by heating in a resistance furnace evacuated quartz vials containing Ta-crucibles with element pieces. SEM-EDXS analyses were performed to check phases composition. The structures were refined from X-ray single crystal diffraction data. Y5Cu5Mg8, Y5Cu5Mg13 and Y5Cu5Mg16 represent new structure types: Y5Cu5Mg8 – orthorhombic, Pmma, oP36, a = 2.63723(15), b = 0.40066(2), c = 0.74115(6) nm, Z = 2, wR2 = 0.0597, 939 F2 values, 60 variables; Y5Cu5Mg13 – orthorhombic, Cmcm, oS92, a = 0.40973(2), b = 1.92794(8), c = 2.57907(11) nm, Z = 4, wR2 = 0.1134, 1208 F2 values, 75 variables; Y5Cu5Mg16 – orthorhombic, Cmcm, oS104, a = 0.41360(8), b = 1.9239(4), c = 2.9086(6) nm, Z = 4, wR2 = 0.0760, 1383 F2 values, 84 variables. YCuMg4 crystallizes in the TbCuMg4 structure type (Cmmm, oS48, a = 1.35754(4), b = 2.03153(6), c = 0.39060(1) nm, Z = 8, wR2 = 0.0401, 661 F2 values, 45 variables). The crystal chemistry of these two-layer structures is comparatively discussed. Majority of novel compounds were characterized as members of inhomogeneous 2D intergrowth structure series of R5M5X5, X4 (Mg4) and empty Mg octahedra building blocks of general formula R5kM5kX5k + 4l + m. The common pentagonal prism derivative structural fragments around the most electropositive yttrium atoms were outlined in all these intermetallics.Graphical abstract