A new layered carbide, [Zr1.97Y0.03]Al4C5, has been synthesized and characterized by X-ray powder diffraction (XRPD), transmission electron microscopy, and energy-dispersive X-ray spectroscopy (EDX). The atom ratios [Zr:Y] were determined by EDX, and the crystal structure was refined from laboratory XRPD data (CuK alpha(1)) using the Rietveld method. The crystal is trigonal (space group R3m, Z=3) with lattice dimensions of a=0.331934(4) nm, c=4.09459(3) nm, and V=0.390701(7) nm(3). The final reliability indices were R-wp=10.29% (S=1.31), R-p=7.45%, R-B=1.63%, and R-F=1.04%. The compound shows an intergrowth structure with NaCl-type [Zr1.97Y0.03C3] thin slabs separated by Al4C3-type [AlC] layers. This material is isostructural with Zr-2[Al3.56Si0.44]C-5.