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Under identical conditions, CuI reacts with PhS(CH2)8SPh and p‐TolS(CH2)8STol‐p affording, respectively, a luminescent 1D coordination polymer [Cu4I4{μ2‐PhS(CH2)8SPh}2]n (1) and an unprecedented 2D network [Cu8I8{μ2‐p‐TolS(CH2)8STol‐p}3(MeCN)2]n (2), which incorporate closed‐cubane Cu4I4 and octanuclear Cu8I8 clusters of as connecting nodes. Their thermal and photophysical properties exhibit notable...
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