A series of new 1D chain and 2D coordination polymers with cyclotriguaiacylene-type ligands are reported. A zig-zag 1D coordination chain is found in complex [Cd2(4ph4py)(NO3)3(H2O)2(DMA)2]·(NO3)·(DMA)4, where 4ph4py = tris[4-(4-pyridyl)benzoyl]-cyclotriguaiacylene and DMA = dimethylacetamide, while complex [Zn(4ph4py)2(CF3COO)(H2O)]·(CF3COO)(NMP)7, where NMP = N-methylpyrrolidone, has a doubly bridged coordination chain structure. Complexes [M(3ph3py)(NO3)2]·(NMP)4 where M = Co or Zn, 3ph3py = tris[3-(3-pyridyl)benzoyl]cyclotriguaiacylene, are isostructural and feature 1D ladder coordination chains. Complexes [Cd2(4ph4py)2(NO3)4(NMP)]·(NMP)9(H2O)4 and [Co(4ph4py)(H2O)2]·(NO3)2·(DMF)2, where DMF = dimethylformamide, both have (3,4)-connected 2D coordination polymers with a rare (42.62)(4.62)2 topology. A 2D coordination polymer with this topology is also found in complex [Co2(3ph4py)2(NO3)(H2O)5]·(NO3)3·(DMF)9 where 3ph4py = tris[3-(4-pyridyl)benzoyl]cyclotriguaiacylene. All 2D coordination polymer complexes are interpenetrating or polycatenating. [Co2(3ph4py)2(NO3)(H2O)5]3+ polymers form a 2D→3D polycatenation showing self-complementary “hand-shake” interactions between the host-type ligands.
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