Isolation and crystal and molecular structures of [(C5H2Br3)2Fe], [(C5HBr4)2Fe] and [(C5Br5)(C5Br4HgBr)Fe]

The reaction of [(C5H3Br2)2Fe] with lithium tetramethylpiperidinide (LiTMP) in a 1:10 molar ratio in tetrahydrofuran yields, after quenching with C2H2Br4, a mixture of the polybromoferrocenes [C10H10 – nBrnFe] with n   = 4 – 9, from which single crystals of bis(1,2,3-tribromocyclopentadienyl)iron(II), [Fe(C5H2Br3)2], and bis(1,2,3,4-tetrabromocyclopentadienyl)iron(II), [Fe(C5HBr4)2Fe], were obtained by a combination of chromatography and fractional crystallization. Treatment of `[C10(HgOAc)10Fe]' with KBr3 yields a mixture of polybromoferrocenes [C10H10 – nBrnFe] with n   = 8 – 10 and bromomercurioferrocenes [C10H9 – nBrn(HgBr)Fe] with n   = 7 – 9, from which single crystals of (1-bromomercurio-2,3,4,5-tetrabromocyclopentadienyl)(1,2,3,4,5-pentabromocyclopentadienyl)iron(II), [FeHgBr(C5Br4)(C5Br5)], were obtained by fractional crystallization. The crystal structures of all the compounds show Br...Br, Br...H and sometimes Br...Cp... π (Cp is a ring centroid) interactions, as well as π – π interactions. The findings are supported by Hirshfeld analyses.

Source: Acta Crystallographica Section C - October 13, 2022 Category: Chemistry Authors: Blockhaus, T. S ü nkel, K. Tags: noncovalent interactions halogen bonding Hirshfeld analysis crystal structure bromoferrocene research papers Source Type: research