Data associated with “One-step Preparation of Biocompatible Gold Nanoplates with Controlled Thickness and Adjustable Optical Properties for Plasmon-based Applications”: https://doi.org/10.1002/adfm.202003512 UV-vis spectra and XRD data of gold nanoplates: Ye, Sunjie and Connell, Simon D. and McLaughlan, James R. and Roach, Lucien and Aslam, Zabeada and Chankhunthod, Navadecho and Brown, Andy P. and Brydson, Rik and Bushby, Richard J. and Critchley, Kevin and Coletta, P. Louise and Markham, Alexander F. and Evans, Stephen D. (2020) Data associated with 'One-step Preparation of Biocompatible Gold Nanoplates with Controlled Thickness and Adjustable Optical Properties for Plasmon-based Applications'. University of Leeds. [Dataset] https://doi.org/10.5518/790 Dataset description: The ability to synthesize plasmonic nanomaterials with well-defined structures and tailorable size is crucial for exploring their potential applications. Gold nanoplates (AuNPLs) exhibit appealing structural and optical properties, yet their applications are limited by difficulties in thickness control. Other challenges include a narrow range of tunability in size and surface plasmon resonance (SPR), combined with a synthesis conventionally involving cytotoxic cetyltrimethylammonium (CTA) halide surfactant. Here, a one-step, high-yield synthesis of single-crystalline AuNPLs has been developed, based on the combined use of two structure-directing agents, methyl orange and FeBr3, which undergo preferential adsorption onto different crystalline facets of gold. The obtained AuNPLs feature high shape homogeneity that enables mesoscopic self-assembly, broad-range tunability of dimensions (controlled thickness from ∼7 to ∼20 nm, accompanied by modulation of the edge length from ~150 nm to ~2 μm) and plasmonic properties. These merits, coupled with a preparation free of CTA-halide surfactants, have facilitated the exploration of various uses especially in bio-related areas. For example, they have been demonstrated as biocompatible photothermal agents for cell ablation in NIR-I and II windows. This work paves the way to the innovative fabrication of anisotropic plasmonic nanomaterials with desired attributes for wide-ranging practical applications. Files: Figure_2d-XRD_curve.xlsx Figure_5a-UV-vis_spectra.xlsx Figure_5e-UV-vis_spectra.xlsx