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Synthesis and crystal structure determination of iridium(III) acetylacetonate and its Br-and I-substituted analogs

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Abstract

γ-Halogen-substituted iridium(III) acetylacetonates of general formula Ir(acacX)3,where acacX = CH3 -CO-CX-CO- CH3,X =Br, I, were synthesized. The compounds are characterized by melting points and chemical analysis data for C, H, Br, and I. An X-ray diffraction analysis was performed for iridium(III) acetylacetonate and its y-substituted analogs, crystal data were obtained, and crystal structures were determined. The crystals are monoclinic;the structures are molecular. Crystal data: Ir(acac)3 - IrO6C15H21,a = 13.900(2), b = 16.440(3), c = 7.494(2) å, γ =98.63(2)‡, V= 1693.2 å3,space group P21/b,Z = 4, dcalc =1.92 g/cm3,sin θ/λmax = 0.703, Fhkl = 2841, R = 0.044. Ir(acacBr)3- IrBr3O6C15H18,a = 12.794(2), b = 15.753(2), c = 9.990(2) å Β = 105.76(2)‡, V= 1937.6 å3,space group P21/n,Z =4, dcalc =2.49 g/cm3, sinθ/λmax = 0.702, Fhkl = 1748, R = 0.048. Ir(acacI)3- M3O6C15H18,a = 12.855(2), b = 10.136(2), c =16.338(3)å, Β = 104.6(2)‡, V=2059.8å3,space group P21/n, Z =4, dcalc = 2.79g/cm3, θmax =25‡, Fhkl = 2817, R =0.032. The Ir..Ir distances were estimated to be > 7.49 å for Ir(acac)3 and > 8.10 å for Ir(acacBr)3 and Ir(acacl)3.If the estimate is limited to 10 å, the intermolecular coordination number (ICN) in the structures is 10.

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Authors and Affiliations

  1. Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Russia

    V. G. Isakova, I. A. Baidina, N. B. Morozova, I. K. Igumenov & V. B. Rybakov

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  1. V. G. Isakova
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  2. I. A. Baidina
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  3. N. B. Morozova
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  4. I. K. Igumenov
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  5. V. B. Rybakov
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Translated fromZhurnal Struktumoi Khimii, Vol. 40, No. 2, pp. 331–339, March–April, 1999

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Isakova, V.G., Baidina, I.A., Morozova, N.B. et al. Synthesis and crystal structure determination of iridium(III) acetylacetonate and its Br-and I-substituted analogs. J Struct Chem 40, 276–283 (1999). https://doi.org/10.1007/BF02903657

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