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Abstract
Compounds of composition [Co(picam)3]I3·H2O(I) and [Co(picam)3](ClO4)3·2H2O(II) were unexpectedly obtained while attempting to synthesize [cis-Co(picam)2(NO2)2]± derivatives, using procedures expected to suceed in producing the cis-dinitro cation. The structure of the title compound was determined, at which point we realized the nature of the product obtained. (I) crystallizes in the monoclinic system, P21 lc (No. 14), Z = 4, a = 14.521(7), b = 15.003(4), c = 11.347(4) Å, β = 95.01(4)°, V = 2462.60 Å3 and d = 2.107 g-cm−3. F(000) = 1480, R(F) = 0.037 and Rw(F) = 0.044 for 3095 reflections. Data were corrected for absorption obtained from Psi-scans (μ = 44.397 cm−1) and the transmission coefficients ranged from 0.2615 to 0.3878. The cations exist in the lattice as enantiomeric pairs with chiroptical descriptors Δ(δδΛ)[fac-Co(picam)3]± and Λ(ΛΛδ)[fac-Co(picam)3]±. The analogous perchlorate was obtained also and identified only by its elemental analysis.