The most prominent factors determining the properties and applications of metal–organic frameworks (MOFs) are their structural, morphological, and stability features under harsh conditions. Therefore, it is important to design the new methods to synthesize MOFs with modified structure and morphology and as a result more stability for the expansion of well-organized MOFs. Herein, we reported the new synthetic strategy for the preparation of copperaurin tricarboxylate metal–organic framework (CuATC-MOF) using a mixed solvent system. Comprehensive monitoring of the new synthetic strategy revealed the mixed solvent system (DMF/EtOH) is a key factor on particle size, morphology, and chemical stability of CuATC-MOF. Then, the as-prepared CuATC-MOF with an acceptable specific surface area (62.655 m2/g), the particle size of 40–90 nm, and mesoporous structure exhibited superior catalytic activity and stability for the catalytic formation of a C-C bond through a Suzuki-Miyaura cross-coupling reaction (SMCR). FT-IR, PXRD, BET, FE-SEM, TEM, EDX, EDX-mapping, TGA, and ICP-OES are impressive techniques that assisted us to well identified the structure of CuATC-MOF. Additionally, CuATC-MOF displayed excellent recyclability, during the six consecutive cycles, without significant reduction in its catalytic efficiency.

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