Here, using the case of a novel flux-grown layered semiconductor crystal, we show how a combination of high resolution X-ray absorption contrast tomography and diffraction contrast tomography can be applied to identify previously-undiscovered materials while simultaneously viewing the crystal morphology and growth habit. Since the Laue pattern indexation can be quickly checked against known crystal structures, a set of "unmatched" crystals was quickly identified, and the material was determined to be a new layered semiconductor KBiS 2 , still embedded in the flux. Conducting the entire analysis non-destructively enables investigation of the crystals in their native environment while preserving the samples for further subsequent correlative characterization.