Ligands containing P–CH2–CH2–P elements have been shown to form double-stranded helicates whose axis consists of gold atoms with Au⋯Au contacts; the interconversion of the P and M forms of the helicate [Au3(μ-pp2)2](OTf)3 (pp2 = PhP(CH2CH2PPh2)2) is monitored via 31P NMR.