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In situ high-resolution synchrotron x-ray diffraction reveals a local minimum in rhombohedral distortion angle a R (associated with an inflection in the lattice constant a R) near 400 and 350 C in BiFeO 3 (BFO) and (BiFeO 3) 0.95 (BaTiO 3) 0.05 (BFO-5%BT), respectively. It suggests a coupling between ferroelectric and magnetic parameters near the antiferromagnetic-paramagnetic transition, which is responsible for the broad frequency-dependent dielectric maxima. A rhombohedral (R)-orthorhombic (O)-cubic (C) transition sequence takes place near 820 and 850 C in BFO upon heating. BFO-5%BT exhibits a R-C transition near 830 C. The BaTiO 3 substitution can enhance dielectric and ferromagnetic responses and reduce electric leakage. The dielectric loss of BFO-5%BT remains less than 0.04 below 150 C. V