During SANS measurements, 5c1 block copolymers and the corresponding cross-linked nanogels were subjected to a temperature ramp from 25 to 45 °C and from 32 to 42 °C, respectively (Figure , Table and Table ). Gaussian chains to a more entangled polymer network (Rg of 52.0 ± 0.6 nm) indicating the start of the coil-to-globule transition. At higher temperatures (36 and 45 °C) data were fitted using a triaxial ellipsoid model, which suggests the formation of non-perfect spherical nanogels, with an observable trend of ellipse transitioning to more sphere shape with increasing temperature (Table ). From these experiments a Tcp of 35-36 °C was obtained, which was similar to the value found by DLS (37 °C). Multiplying the scattering intensity by Q 2 allowed us to obtain the Kratky plot with linear x-and y-axes (Figure ). This plot is useful for studying nanogel degree of globularity, flexibility and compactness. The peak appearing in the Kratky plot at higher temperatures suggests the formation of globular particles above 35 °C. As the temperature further increases, the peak becomes more defined suggesting an increase in globularity.