This dataset contains raw micro-X-ray diffraction (μ-XRD) patterns of 8 yellow-skinned Nanhong Agate samples collected from Northeastern Yunnan, China. Data acquisition was performed using a Malvern PANalytical EMPYREAN diffractometer(Malvern-Panalytical, UK) with Cu-Kα radiation (λ = 1.54056 Å), operating at 40 kV and 40 mA. The measurements were performed on a defined microarea using a 0.5-mm X-ray beam collimator. The sample was scanned over a 2θ range of 5° to 90° with a step size of 0.02°. The data acquisition time for each step was 140.25 s, and the scan speed was 0.048°/s. The total time spent at each test site was 30 min and 53 s, ensuring adequate counting statistics. The obtained diffraction patterns were analyzed using Rietveld refinement. The analyses were performed at the Kunming University of Science and Technology Analysis and Testing Research Center on June 25, 2024.

Laboratory Instruments：The X-ray diffraction measurements were performed using an EMPYREAN multifunctional X-ray diffractometer (Malvern-Panalytical, UK) equipped with a PIXCEL 3D detector and copper target. The instrument configuration included advanced optical path control modules: a BBHD filter, parallel beam mirror, and double cross slit system. This setup enabled flexible switching between focused and parallel beam modes, with precise control of micro-focused beam spot size (adjustable down to 0.1 mm minimum dimension through slit optimization). The parallel beam configuration achieved an ultra-low grazing incidence angle of 0.1°, while the double cross slit assembly maintained a minimum effective aperture of ≥0.1 mm during measurements.2θ (degrees): Diffraction angle range (5° to 90°).Intensity (counts): Measured intensity of the diffracted X-rays.Step size (degrees): 0.02°.Acquisition time per step (seconds): 140.25 s.Scan speed (degrees/second): 0.048°/s.Total measurement time per site (minutes:seconds): 30:53.Additional Notes:The dataset includes raw μ-XRD patterns for eight samples.The data files contain columns for 2θ (degrees) and corresponding intensity (counts).Non-common abbreviations (e.g., μ-XRD, Cu-Kα) are explained in the metadata.