Intramolecular Quadridentate Synthesis: X-Ray Crystallographic Analysis of [(NH₂CH₂CH₂NH₂)Co(NH₂(CH₂)₂N = C(NH₂)CH₂S(CH₂)₂NH₂)](CF₃SO₃)₃.H₂O

Abstract

Meridional forms of N₃S quadridentate complexes of the type

[(en)Co(NH₂(CH₂)₂ N=C(R′)CH₂S(CH₂)₂NH₂)]³⁺ with R′ = CH₃ and NH₂) are readily prepared from [(en)₂Co(S(R)CH₂CH₂ NH₂)]³⁺ (with R = CH₂COCH₃ and CH₂CN, respectively; en = ethane-1,2-diamine) in basic solution. The X-ray crystallographic analysis of the complex with R1= NH₂ was determined as the monohydrate of its triflate salt and shown to have a β-type configuration of the quadridentate. Crystals are monoclinic, space group C2/c with a 23.337(1), b 11.973(1), c 20.015(1) Å , β 95.12(1)º, and Z 8. 3183 data with 1 ≥ 3 σ (1) were refined to conventional R factors of 0.056 and 0.072.