Abstract

Hybrid copper molybdates containing the long‐spanning bis(4‐pyridylmethyl) piperazine (bpmp) ligand were prepared via hydrothermal synthesis and structurally characterized by single‐crystal X‐ray diffraction. The reduced copper phase and major product [Cu4(MoO4)2(bpmp)4]n (1) shows 1D ribbon motifs with embedded {CuI2O2} dimeric units, built from the bpmp pillaring of [Cu4(MoO4)2] linear clusters. The oxidized copper phase and minor product {[Cu2(MoO4)2(bpmp)4]·24H2O}n (2) displays [Cu(bpmp)2]n2n+ mutually inclined interpenetrated cationic layers cross‐pillared by molybdate tetrahedra into an unprecedented 6‐connected self‐penetrated network with 485265 topology.

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