The folder "Figure 2" contains normalised UV/Vis absorption spectra (2a, 2b) and steady-state emission spectra (2c, 2d) for P3HTPMe3(SDS)x and P3HT-b-P3HTPMe3(SDS)x at room temperature. For both, total sample concentrations were 10 mg mL−1 in D2O. λex = 450 nm.

The folder "Figure 3" contains normalised UV/Vis absorption and emission spectra for P3HTPMe3 (3a, 3c) and P3HT-bP3HTPMe3 (3b, 3d) with no surfactant and 1:1 charge ratio of SDS or PFOS at room temperature. Total sample concentrations were 10 mg mL−1 in D2O. λex = 450 nm.

The folder "Figure 4" contains UV/Vis absorption (4a) and emission (4b) spectra of P3HTPMe3 and P3HT-b-P3HTPMe3 and the corresponding 1:1 SDS nd PFOS electrostatic complexes in d4-MeOD (10 mg mL−1).

The folder "Figure S1 contains normalised UV/Vis absorption spectra for P3HTPMe3(SDS)x (S1a) and P3HT-bP3HTPMe3(SDS)x (S1b) as a function of composition, x, at room temperature. Total sample concentration = 0.1 mg mL-1 in D2O.

The folder "Figure S2" contains normalised steady-state emission spectra for P3HTPMe3(PFOS)x (S2a) and P3HT-bP3HTPMe3(PFOS)x (s2b) as a function of PFOS composition, x, at room temperature. Total sample concentration = 10 mg mL-1 in D2O. λex = 450 nm.

The origin files in the above folders contain the individual measurement files (and instrument meta data) as well as consolidated graphs (final figures in manuscript).

SANS was carried out on the LOQ small-angle diffractometer at the ISIS Pulsed Neutron Source (STFC Rutherford Appleton Laboratory, Didcot, UK). The scattering functions were fit using non-linear leastsquares analysis to a Rigid Cylinder modelLamellar Sheet model or a Core–Shell Cylinder model using the SasView program (version 3.1.2).

The folder "Figure 6" contains SANS data of P3HTPMe3 and P3HT-b-P3HTPMe3 in D2O with selected charge ratios of SDS (6a, 6b) and d25-SDS (6d, 6e),. The overall concentration of each system was 10 mg mL−1. T = 25 °C. The file names contain the identiy of each conjugated polymer, the concentration and ratio/concentration of SDS or dSDS, if present. References and control samples are also provided (filename is "abbreviated compound_D2O" only)

The SANS data are reported in terms of q (X), scattering intensity (Y) and error on scattering intensity (y error).

The folder "Figure S4" contains data (q, I(q), y error) for the Guinier plot of P3HTPMe3 in D2O (10 mg mL-1) at T = 25 °C.

The folder "Figure S5" contains SANS data (q, I(q), y error) of SDS and PFOS in D2O and d4-MeOD. The concentration of each sample was 10 mg mL-1. T = 25

The folder "Figure S6" contains SANS data (q, I(q), y error) of P3HTPMe3(SDS)5 in D2O. The overall concentration was 10 mg mL-1. T = 25 °C.

The folder "Figure S7" contains SANS data (q, I(q), y error) of (a) P3HTPMe3 and (b) P3HT-b-P3HTPMe3 with selected charge ratios of PFOS in D2O. The overall concentration was 10 mg mL-1. T = 25 °C.

Cryo-TEM measurements were carried out on concentrated samples (10 mg mL−1 in D2O). The observable length scale range was between 5 and 500 nm.

The folder "Figure 7" contains Cryo-TEM micrographs as .tif files of P3HTPMe3 (7a), P3HTPMe3(SDS)1 (7b), P3HT-b-P3HTPMe3 (7c) and P3HT-b-P3HTPMe3(SDS) (7d). Total concentration for each was 10 mg mL−1.

The folder "Figure S8" contains further cryo-TEM images, all filenames labelled with relevant designation.

Atomic force microscopy (AFM) measurements were performed using an Asylum Research MFP-3D™ instrument mounted on an anti-vibration plinth, in the tapping mode at room temperature under ambient conditions. Higher resolution AFM measurements were performed using diamond tips on silicon cantilevers.

The folder "Figure 8" contains AFM tapping-mode height images of pure CPEs and CPE–surfactant complexes at 1:1 charge ratio. (10 mg mL−1 in either water or methanol).

The folders "Figure S9" and Figure "S10" contain further supporting AFM images, all filenames labelled with relevant designation.