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Crystals of bis-(tetra-butyl-ammonium) di-μ 3 -chlorido--tris-(μ 2 -4-iodo-pyrazolato-κ 2  N : N ')tris-[chlorido-cuprate(II)] 1,4-dioxane hemisolvate, (C 16 H 36 N) 2 [Cu 3 (C 3 H 2 IN 2 ) 3 Cl 5 ]·0.5C 4 H 8 O or (Bu 4 N) 2 [Cu II  3 ( μ  3 -Cl) 2 ( μ -4-I-pz) 3 Cl 3 ]·0.5C 4 H 8 O, were obtained by evaporating a solution of (Bu 4 N) 2 [{Cu II ( μ -OH)( μ -4-I-pz)}  n  CO 3 ] ( n = 27-31) nanojars in chloro-form/1,4-dioxane. The decomposition of chloro-form in the presence of oxygen and moisture provides HCl, which leads to the breakdown of nanojars to the title trinuclear copper(II) pyrazolate complex, and possibly Cu II ions and free 4-iodo-pyrazole. Cu II ions, in turn, act as catalyst for the accelerated decomposition of chloro-form, ultimately leading to the complete breakdown of nanojars. The crystal structure presented here provides the first structural description of a trinuclear copper(II) pyrazolate complex with iodine-substituted pyrazoles. In contrast to related trinuclear complexes based on differently substituted 4- R -pyrazoles ( R = H, Cl, Br, Me), the [Cu 3 ( μ -4-I-pz) 3 Cl 3 ] core in the title complex is nearly planar. This difference is likely a result of the presence of the iodine substituent, which provides a unique, novel feature in copper pyrazolate chemistry. Thus, the iodine atoms form halogen bonds with the terminal chlorido ligands of the surrounding complexes [mean length of I⋯Cl contacts = 3.48 (1) Å], leading to an extended two-dimensional, halogen-bonded network along (-110). The cavities within this framework are filled by centrosymmetric 1,4-dioxane solvent mol-ecules, which create further bridges via C-H⋯Cl hydrogen bonds with terminal chlorido ligands of the trinuclear complex not involved in halogen bonding.

Halogen-bonded network of trinuclear copper(II) 4-iodopyrazolate complexes formed by mutual breakdown of chloroform and nanojars