The complexes [M2(p-XBP)3(N03)6] [M = Pr, Nd, Sm, Er; p-XBP = N,N'-xylene-l,4-diylbis(pyridin-2-one)] are shown by X-ray diffraction methods to contain the first example of an O-bonded triple helical bridge.
In the polyamides 4.12, 10.6, 8.8 and 6.10 three fractions are present. The WAXD crystallinity is comparable to that of DSC and amounts to 40% in all samples. The rigid fraction obtained by solid state NMR is, however, close to 60%, pointing at 20% rigid amorphous material. A combination of the NMR, WAXD and SAXS results reveals that the latter fraction is situated inside the crystalline phase and not at the crystalline -'mobile amorphous' interface. Accordingly, one third of the crystalline layers with a thickness between 50 and 56 Å is not truly crystalline. From the width of the WAXD 100 reflections it can be deduced that crystalline grains exist with lateral dimensions of approximately 100 Å . Hence a picture emerges of alternating solid and liquid-like layers with the former consisting of crystalline grains separated by rigid amorphous matter.
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