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The present work provides a simple, low-cost and prospective strategy for the synthesis of defective Cd-Zn-S solid solutions, and it also delivers guidance to design and develop the advanced visible-light photocatalyst in the future.Coordination polymers are highly desirable for various applications due to their functionality control of crystal structures. In this work, an unique class of amorphous Co coordination polymer spheres anchored onto 3D macroporous carbon (MPC) support (denoted as Co CPSs/MPC) was prepared via a facile hydrot