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This invention belongs to the field of catalyst preparation and application technology, and discloses a method for preparing sulfur-bridged bimetallic alkyne complexes and their application in the dehydrogenation coupling synthesis of 1,4-diyne. The method uses thiols or thiophenol salts as bridging ligands, with each metal center coordinated with a cyclopentadienyl group or a substituted cyclopentadienyl group. This invention achieves coordination activation of the terminal alkyne by controlling the oxidation state of the metal center and altering the bonding mode of the terminal alkyne at the metal center. In this system, the sulfur-bridged ligand not only assists the metal center in activating the terminal alkyne but also stabilizes a key intermediate in the catalytic process. Subsequently, the coordinated-activated terminal alkyne undergoes a reductive elimination process to generate 1,4-diyne. This reaction can be carried out in a temperature range of -100℃ to 25℃, with a reaction time of 0.5 to 48 hours. This method can synthesize a series of novel sulfur-bridged bimetallic alkyne complexes with high yield and high selectivity, providing a novel catalytic system for the activation of C-H bonds in terminal alkynes mediated by inexpensive metals and the further synthesis of 1,4-diyne.