Cobalt nanocrystals, recently synthesized with narrow size distributions and controlled shapes, organize in a wide range of arrays as a function of shape, size and interparticle interactions. The nanocrystals (NCs) consist of a cobalt metal core with a nominal diameter of 11 nm, and an organic surfactant surface layer with a chain length of ∼1.7 nm. For the simplest case (ε-Co nanospheres, super-paramagnetic at room temperature) a hexagonal arrangement of NCs is observed in transmission electron microscope (TEM) images when precipitated from solution onto carbon films. For practical applications and for further understanding of the self-assembly process, long range order of the super lattice must be probed over regions that are greater in extent than may be examined by TEM. Hence, small angle x-ray scattering (SAXS) measurements were performed on cobalt nanospheres randomly dispersed in solution and assembled on glass substrates. Least squares fit to the intensity distribution as a function of the scattering vector q gave an average particle diameter of 11.0 ± 0.8 nm. Structure factor contribution to the intensity profile agrees well with a quasi-random model for scattering from a face centered cubic (FCC) superlattice composed of uniform radius cobalt spheres. The measured nearest neighbor interparticle spacing, 14.1 nm, agrees to within 2% of the predicted value of 14.4 nm based on a free energy model that governs the self-assembly of the nanoparticle system.