Research data supporting "A Self-Assembly Toolbox for Thiophene-Based Conjugated Polyelectrolytes: Surfactants, Solvent and Copolymerisation"

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.

"Figure 2"文件夹包含P3HTPMe3(SDS)x与P3HT-b-P3HTPMe3(SDS)x在室温下的归一化紫外-可见（UV/Vis）吸收光谱（2a、2b）与稳态发射光谱（2c、2d）。两组样品的总浓度均为10 mg mL−1，溶剂为重水（D2O），激发波长λex = 450 nm。

"Figure 3"文件夹包含未添加表面活性剂、以及以1:1电荷比添加十二烷基硫酸钠（SDS）或全氟辛烷磺酸（PFOS）时，P3HTPMe3（3a、3c）与P3HT-b-P3HTPMe3（3b、3d）的归一化紫外-可见吸收光谱与发射光谱。样品总浓度为10 mg mL−1，溶剂为D2O，激发波长λex = 450 nm。

"Figure 4"文件夹包含P3HTPMe3、P3HT-b-P3HTPMe3，以及二者与1:1比例的SDS和PFOS形成的静电复合物在氘代甲醇-d4（d4-MeOD）中的紫外-可见吸收光谱（4a）与发射光谱（4b），样品浓度均为10 mg mL−1。

"Figure S1"文件夹包含P3HTPMe3(SDS)x（S1a）与P3HT-b-P3HTPMe3(SDS)x（S1b）在室温下随组分x变化的归一化紫外-可见吸收光谱。样品总浓度为0.1 mg mL−1，溶剂为D2O。

"Figure S2"文件夹包含P3HTPMe3(PFOS)x（S2a）与P3HT-b-P3HTPMe3(PFOS)x（S2b）在室温下随全氟辛烷磺酸（PFOS）组分x变化的归一化稳态发射光谱。样品总浓度为10 mg mL−1，溶剂为D2O，激发波长λex = 450 nm。

上述文件夹中的原始文件包含单独的测量文件（及仪器元数据）与整合后的图谱（即稿件中的最终插图）。小角中子散射（Small-Angle Neutron Scattering, SANS）实验在英国迪德科特的ISIS脉冲中子源（STFC卢瑟福阿普尔顿实验室）的LOQ小角衍射仪上完成。散射函数采用SasView程序（版本3.1.2），通过非线性最小二乘法拟合为刚性圆柱模型、层状薄板模型或核壳圆柱模型。

"Figure 6"文件夹包含P3HTPMe3与P3HT-b-P3HTPMe3在D2O中，以选定电荷比添加SDS（6a、6b）及氘代十二烷基硫酸钠（d25-SDS）（6d、6e）的SANS数据。各体系总浓度为10 mg mL−1，测试温度T = 25 °C。文件名包含各共轭聚合物的标识、浓度，以及SDS或氘代SDS（若存在）的比例/浓度。同时提供了对照样品与参考样品（文件名为"缩写化合物_D2O"）。SANS数据以散射矢量q（X轴）、散射强度I(q)（Y轴）及散射强度的误差（y误差）形式给出。

"Figure S4"文件夹包含P3HTPMe3在D2O中（浓度10 mg mL−1）、T = 25 °C条件下的吉尼耶（Guinier）图数据（q, I(q), y误差）。

"Figure S5"文件夹包含SDS与PFOS在D2O和d4-MeOD中的SANS数据（q, I(q), y误差）。各样品浓度为10 mg mL−1，T = 25 °C。

"Figure S6"文件夹包含P3HTPMe3(SDS)5在D2O中的SANS数据（q, I(q), y误差）。总浓度为10 mg mL−1，T = 25 °C。

"Figure S7"文件夹包含（a）P3HTPMe3与（b）P3HT-b-P3HTPMe3在D2O中以选定电荷比添加PFOS的SANS数据（q, I(q), y误差）。总浓度为10 mg mL−1，T = 25 °C。

冷冻透射电子显微镜（Cryo-transmission Electron Microscopy, Cryo-TEM）测试使用浓度为10 mg mL−1的D2O溶液样品，可观测的长度尺度范围为5~500 nm。"Figure 7"文件夹包含P3HTPMe3（7a）、P3HTPMe3(SDS)1（7b）、P3HT-b-P3HTPMe3（7c）与P3HT-b-P3HTPMe3(SDS)（7d）的冷冻透射电子显微镜显微图像，格式为.tif文件。各样品总浓度均为10 mg mL−1。"Figure S8"文件夹包含更多冷冻透射电子显微镜图像，所有文件名均标注了相关标识。

原子力显微镜（Atomic Force Microscopy, AFM）测试使用安装于防振平台的Asylum Research MFP-3D™仪器，在室温环境下采用轻敲模式完成。高分辨率原子力显微镜测试使用硅悬臂梁搭配金刚石针尖。"Figure 8"文件夹包含电荷比为1:1的纯共轭聚电解质（Conjugated Polyelectrolytes, CPEs）与共轭聚电解质-表面活性剂复合物的原子力显微镜轻敲模式高度图像（样品浓度为10 mg mL−1，溶剂为水或甲醇）。"Figure S9"与"Figure S10"文件夹包含更多辅助性原子力显微镜图像，所有文件名均标注了相关标识。