Abstract. Two aliphatic dicarboxy1ic acid ligands, iminodiacetic acid (H2L1) and 3,3‐thiodipropionic acid (H2L2), were used to construct two novel lead(II) frameworks, namely, [Pb(μ4‐L1)Br]n (1) and [Pb3(μ9‐L2)(μ2‐Br)2Br2]n (2), under hydrothermal conditions. It has to be noted that for 1 the central PbII ions are bridged by L2– ligands resulting in infinite right‐ and left‐handed helical Pb–(O–C–O)–Pb linkage. Compound 2 represents a novel 3D hybrid luminescent lead(II) framework with I3O0 type connectivity. For 2 infinite 2D Pb–O–Pb inorganic layers and trinuclear Pb3Br4 clusters are inter‐linked forming a 3D inorganic connectivity. In 1 the five‐coordinate central PbII ions adopt a hemi‐directed coordination arrangement, whereas in 2 six‐coordinate Pb1, six‐coordinate Pb2, and four‐coordinate Pb3 atoms adopt hemi‐directed coordination arrangements. The variable lead(II) coordination environment and flexible coordination modes of carboxy1ic acid ligands such as H2L1 and H2L2 also reveal great potential for constructing novel inorganic‐organic hybrid materials. Furthermore TGA, FT‐IR, PXRD, elemental analysis, and photo‐luminescent properties of 1 and 2 were investigated.