The possibility to synthesize M_1x M₂(OH) _y F _z nanolayers by the ionic layering method with the use of soluble anionic complexes of metal fluorides was demonstrated. The influence of the concentration and pH of reagent solutions and of the number of ionic layering cycles on the kinetics of layer growth was studied using the example of Cu _x Zr(OH) _y F _z layers. The composition of the synthesized layers was studied by X-ray photoelectron (XPE) spectroscopy, ellipsometry, and electronic and Fourier transform IR (FT-IR) transmission spectroscopy.