Taylor-Couette reactors allow short reaction times and enable the synthesis of powders with uniform particle size, and thus are suitable for preparing secondary battery cathode materials. Herein, cubic, monoclinic, and rhombohedral NaxMnFe(CN)(6)center dot zH(2)O samples were prepared in a Taylor-Couette reactor at various drying conditions/temperature and were shown to exhibit structure-dependent electro-chemical properties. When cycled at 0.1 C in a potential range of 2.0-4.0 V, cubic-, monoclinic-, and rhombohedral-structured samples exhibited reversible discharge capacities of 89.5, 91.4, and 150.1 mAhh g(-1), respectively. Importantly, the rhombohedral-structured sample not only showed the highest reversible discharge capacity but also exhibited excellent capacity retention (88.03%) after 50 cycles at 0.5 C (300 mA g(-1)), which was ascribed to its extremely low interstitial water content. (C) 2017 Elsevier B.V. All rights reserved.