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The neutral dinuclear complexes [(η⁵-C₅Me₅)₂Rh₂(μ-dhnq)Cl₂] ( 1 ) and [(η⁵-C₅Me₅)₂Ir₂(μ-dhnq)Cl₂] ( 2 ) (dhnqH₂ = 5,8-dihydroxy-1,4-naphthoquinone) were obtained from the reaction of [(η⁵-C₅Me₅)M(μ-Cl)Cl]₂ (M = Rh, Ir) with dhnqH₂ in the presence of CH₃COONa. Treatment of 1 or 2 in methanol with linear ditopic ligands L (L = pyrazine, 4,4'-bipyridine or 1,2-bis(4-pyridyl)ethylene), in the presence of AgCF₃SO₃, affords the corresponding tetranuclear metalla-rectangles [(η⁵-C₅Me₅)₄M₄(μ-dhnq)₂(μ-L)₂] 4+ (L = pyrazine, M = Rh, 3 ; M = Ir, 4 ; L = 4,4'-bipyridine, M = Rh, 5 ; M = Ir, 6 ; L = 1,2-bis(4-pyridyl)ethylene, M = Rh, 7 ; M = Ir, 8 ). All complexes were isolated as their triflate salts and were fully characterized by infrared, ¹H and 13 C NMR spectroscopy, and some representative complexes by single-crystal X-ray structure analysis. The X-ray structures of 3 , 5 and 6 confirm the formation of the tetranuclear metalla-cycles, and suggest that complexes 5 and 6 possess a cavity of sufficient size to encapsulate small guest molecules. In addition, the antiproliferative activity of the metalla-cycles 3 - 8 was evaluated against the human ovarian A2780 (cisplatin sensitive) and A2780cisR (cisplatin resistant) cancer cell lines and on non-tumorigenic human embryonic kidney HEK293 cells. All cationic tetranuclear metalla-rectangles were found to be highly cytotoxic, with IC 50 values in the low micromolar range.

materials

Synthesis, Molecular Structure and Cytotoxicity of Molecular Materials Based on Water Soluble Half-Sandwich Rh(III) and Ir(III) Tetranuclear Metalla-Cycles