Triethylamine-promoted polycondensations of 5,5',6,6'-tetrahydroxy-3,3, 3',3'-tetramethyl spirobisindane (TTSBI) and alpha,omega-alkane dicarboxylic acid dichlorides were performed with equimolar feed ratios. Three different procedures were compared. At a TTSBI concentration of 0.05 mol/L, gelation was avoided, and soluble cyclic polyesters having two 011 groups per repeat unit were isolated. These polyesters were characterized with H-1 NMR spectroscopy, MALDI-TOF mass spectrometry, and SEC and DSC measurements. All polycondensations with sebacoyl chloride resulted in gelation, regardless of the procedure. (c) 2007 Wiley Periodicals, Inc.