Sterically crowded stilbene-containing alternating polyanions were prepared via an indirect strategy of synthesizing protected monomers followed by deprotection and neutralization of the polyanion precursors. The solution properties of these new sterically crowded polyelectrolytes were studied. Steady-state solution shear rheology showed a pronounced polyelectrolyte effect. The persistence lengths of these polyelectrolytes were determined. The dissociation behavior of the polyanions was investigated by pH titration with HCl, and multistep dissociation behavior was observed. Chain size and aggregation were studied by using DLS at varying ionic strengths. Polyelectrolytes behaved like rigid-rods and formed concentrated solutions at the polymer concentration of 1.0 mg mL-1. (c) 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2013, 51, 1565-1570