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Abstract We present chemostratigraphy, biostratigraphy, and geochronology from a succession that spans the Ediacaran-Cambrian boundary in Sonora, Mexico. A sandy hematite-rich dolostone bed, which occurs 20 m above carbonates that record the nadir of the basal Cambrian carbon isotope excursion within the La Ciénega Formation, yielded a maximum depositional age of 539.40 ± 0.23 Ma using U-Pb chemical abrasion–isotope dilution–thermal ionization mass spectrometry on a population of sharply faceted volcanic zircon crystals. This bed, interpreted to contain reworked tuffaceous material, is above the last occurrences of late Ediacaran body fossils and below the first occurrence of the Cambrian trace fossil Treptichnus pedum, and so the age calibrates key markers of the Ediacaran-Cambrian boundary. The temporal coincidence of rift-related flood basalt volcanism in southern Laurentia (>250,000 km3 of basalt), a negative carbon isotope excursion, and biological turnover is consistent with a mechanistic link between the eruption of a large igneous province and end-Ediacaran extinction.