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Abstract π‐d Conjugated coordination polymers (CCPs) have attracted much attention for various applications, although the chemical states and structures of many CCPs are still blurry. Now, a one‐dimensional (1D) π‐d conjugated coordination polymer for high performance sodium‐ion batteries is presented. The chemical states of the obtained coordination polymer are clearly revealed. The electrochemical process undergoes a three‐electron reaction and the structure transforms from C=N double bonds and Ni II to C−N single bonds and Ni I , respectively. Our unintentional experiments provided visual confirmation of Ni I . The existence of Ni I was further corroborated by its X‐ray absorption near‐edge structure (XANES) and its catalytic activity in Negishi cross‐coupling.
Chen et al. (Mon,) studied this question.