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Low-dimensional (LD) lead-halide perovskites have emerged as highly promising materials for optoelectronic applications due to their tunable bandgaps, strong light absorption, and improved environmental stability compared to their three-dimensional (3D) counterparts. However, precise control over their structural arrangement and optical response remains a major challenge. This thesis presents a comprehensive investigation into the combined effects of organic cation engineering using amino(methyl)pyridine isomers (x-AMP; x = 2, 3, and 4) and halide variation on the chemical and optical properties of LD lead-halide perovskites. All samples were synthesized via a reflux method under ambient conditions, eliminating the need for a glove-box system and enabling a cost-effective and scalable synthesis route. Fourier Transform Infrared (FTIR) spectroscopy was employed to elucidate chemical interactions between the organic cations and inorganic frameworks, while UV–Visible (UV–Vis) spectroscopy was used to evaluate optical absorption behavior and determine optical bandgaps. The results demonstrate that positional isomerism of x-AMP significantly affects hydrogen bonding, lattice distortion, and quantum confinement, while halide substitution further modulates absorption edge positions and bandgap energies. This study establishes a dual-parameter strategy—organic cation position and halide composition—as an effective approach for tailoring LD perovskites toward stable and tunable optoelectronic materials.