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Controlling the morphology and crystallographic coherence of assemblies of magnetic nanoparticles is a promising route to functional materials. Time-resolved small-angle X-ray scattering (SAXS) was combined with microscopy and scaling analysis to probe and analyze evaporation-induced assembly in levitating drops and thin films of superparamagnetic iron oxide nanocubes in weak magnetic fields. We show that assembly of micrometer-sized mesocrystals with a cubic shape preceded the formation ofdoi:10.1021/acs.nanolett.0c02770.s002 fatcat:guy3cmqtxjh7fckp4fjc7rkova