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All 1 H and 13 C NMR signals of the four poly(phenylenephthalides): polydiphenylenephthalide (P(DPh)-1), polyterphenylenephthalide (P(TPh)-2) and two sequentially ordered polymers with different ratios of alternating diphenylenephthalide and terphenylenephthalide units (P(DTPh)-3, P(DDTPh)-4) were assigned unequivocally with two-dimensional NMR techniques ( 1 H- 1 H COSY and NOESY; 1 H- 13 C HSQC and HMBC). There are four types of polyphenylene fragments: not symmetrical end, symmetrical inner, symmetrical pre-end and formally symmetric pre-end. The equivalent carbon atoms in these fragments have different chemical shifts. A full additivity of the chemical shifts for the side phthalide and polyphenylene carbon atoms was revealed. A new structure of diads with a mirror symmetry plane, passing through the middle of aromatic moieties, is proposed. Copyright © 2017 John Wiley & Sons, Ltd., (Copyright © 2017 John Wiley & Sons, Ltd.)

(1) H and (13) С NMR spectral assignments have been provided for low-molecular reference monomers, poly(diphenyleneoxidephthalide) and periodic copoly(arylenephthalide) derivatives such as AB, ABB, and ABBB (where A = terphenylenephthalide and B = diphenyleneoxidephthalide) using (1) H-(1) H COSY, (1) H-(13) C HSQC and HMBC NMR techniques. Distinctive (13) C NMR chemical shifts of a main chain have been observed containing fragments of similar structures and lateral phthalate groups being part of various diads., (Copyright © 2013 John Wiley & Sons, Ltd.)