Oxidation of alkali metal derivatives of the dianions [E((t)BuN)P(μ-N(t)Bu)(2)P(N(t)Bu)E](2-) (E = S, Se) with I(2) produces 15-membered macrocycles in which a planar P(6)E(6) motif is stabilised by perpendicular P(2)N(2) scaffolds.

DEDICATION: Dedicated to Wolf-Walther du Mont on the occasion of his 70 th birthday.KEYWORDS: peri-substitution, phosphorus-tellurium, through-space spin-spin coupling, acenaphthene 2 ABSTRACT: A series of peri-substituted phosphorus-tellurium systems R'Te-Acenap-PR 2 (R' = Ph, pAn, Nap, Mes, Tip; R = i Pr, Ph) exhibiting large "through space" spin-spin coupling constants and the "onset" of three-centre four-electron type interactions are presented. The influence of the substituents at the phosphorus and tellurium atoms as well as their behavior upon oxidation (with S, Se) or metalcoordination (Pt, Au) is discussed using NMR spectroscopy, single crystal X-ray diffraction, and advanced DFT studies including NBO, AIM and ELI-D analyses.

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