Abstract

Consecutive base-catalysed reactions of calix[4]arene with the ditosylates of two different polyetherdiols result in the relatively efficient production of an unsymmetrical calix biscrown-6 which, after reduction of an ethoxycarbonyl substituent to an hydroxymethyl group, has been characterised structurally by a room-temperature, single crystal X-ray study of its chloroform solvate. Crystals of ( 4), C53H62O13... ∼0.57CHCl3, are triclinic, P¯1, a 18.95(3), b 12.394(9), c 11.756(7) A α 106.93(5), β 101.77(8), γ 94.63(8)°, Z = 2; R was 0.088 for 2231 ’observed' (I > 3σ(I)) diffractometer data.

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