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The first examples of layered hybrid iron fluorides are reported. In the reactions carried out, the chain compound (H₂<i>pipz</i>)FeF₅·H₂O always occurs as the major phase, with the layered compounds, (H₂<i>pipz</i>)₃Fe₄F1₈·2H₂O and (H₂<i>pipz</i>)₂Fe₃F₁₃·H₂O, being isolated from some reactions as major impurities. The latter two compounds feature two-dimensional sheets of corner-and edge-shared FeIIIF₆ octahedra, resulting in two distinct layer architectures. The compound (H₂<i>pipz</i>)FeF₅·H₂O, isolated as the major phase, crystallises with a one-dimensional structure exhibiting zig-zag [FeF₅]_∞ chains. This work opens up the potential for a much wider family of layered hybrid transition-metal fluorides.