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Phosphorus pentachloride reacts with p-tert.butylcalix[4]arene to give the P-bridged calix[4]-arene derivative 3, which has three differently coordinated phosphorus atoms ([sgrave]4λ5-, [sgrave]5λ5-[sgrave]6λ5-phosphorus). 3 reacts with antimony pentachloride to give the unsymmetrical calix[4]arene bisphosphonium salt 4, and 3 reacts with ethanol to give the unsymmetrical calix[4]arene diphosphate 6.
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