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Treatment of [Ph3EMe][I] with [NaN(SiMe3)2] affords the ylides [Ph3E=CH2] (E = As, 1As; P, 1P). For 1As this overcomes prior difficulties in the synthesis of this classical arsonium-ylide that have historically impeded its wider study. The structure of 1As has now been determined, 45 years after it was first convincingly isolated, and compared to 1P, confirming the long-proposed hypothesis of increasing pyramidalisation of the ylide-carbon, highlighting the increasing dominance of E+-C- dipolar resonance form (sp3-C) over the E=C ene p-
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