The study investigates co-substitutions of Fe3+ and Ni2+ at the beta-Ca-3(PO4)(2) structure for applications in hyperthermia. A detailed structural analysis, magnetic properties and the consequential hyperthermia effect due to the Fe3+ and Ni2+ co-substitutions at the beta-Ca-3(PO4)(2) structure are studied. The structural analysis affirms the ability of beta-Ca-3(PO4)(2) to host 12.55 mol. % Ni2+ and an equal share of similar to 6.25 mol. % of Ni2+ and Fe3+ co-substitutions without significant structural distortions. Both the Ni2+ and Fe3+ prefer to occupy the six-fold co-ordinated Ca2+(5) site of beta-Ca-3(PO4)(2) structure. Fe3+/Ni2+ co-substitutions in beta-Ca-3(PO4)(2) display superior magnetic features and also show pronounced hyperthermia effect than Ni2+ only substitutions. Ni2+ presence at higher concentration elicit cytotoxic effects while its existence at lower concentration in Fe3+/Ni2+ co-substitutions display negligible toxicity. (C) 2017 Elsevier B.V. All rights reserved.