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Concerns about the toxicity of lead-based perovskites have aroused great interest for the development of alternative lead-free perovskite-type materials. Recently, theoretical calculations predict that Pb²⁺ cations can be substituted by a combination of Cu²⁺ and Sb³⁺ cations to form a vacancy-ordered layered double perovskite structure with superior optoelectronic properties. However, accessibilities to this class of perovskite-type materials remain inadequate, hindering their practical implementations in various applications. Here, we report the first colloidal synthesis of Cs₄CuSb₂Cl₁₂ perovskite-type nanocrystals (NCs). The resulting NCs exhibit a layered double perovskite structure with ordered vacancies and a direct band gap of 1.79 eV. A composition–structure–property relationship has been established by investigating a series of Cs₄Cu_xAg_2–2xSb₂Cl₁₂ perovskite-type NCs (0 ≤ x ≤ 1). The composition …