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A set of samples with different textures from the sedimentary Fe–Ni deposits of Central Euboea, Greece, were studied with XRD and SEM-EDS to investigate the relationships between phyllosilicates present. The deposits are characterized by the coexistence of smectite, corrensite, R0 mixed-layer chlorite-smectite and discrete chlorite, which indicates disequilibrium conditions. It is suggested that chlorite, the main Ni-host in the deposits, formed by conversion of smectite (nontronite and possibly stevensite), via corrensite and R0 Chl-Sme during diagenesis. This is the first report for chloritization of Fe-rich dioctahedral smectite during diagenesis.