Process of structure determination of liquid-crystalline superstructures formed in a mesogenic series, bis(
n-alkoxybenzoyl)hydrazine[BABH(
n) ;
n, the number of carbon atoms in the alkoxy group], is described. The chain-length (
n) dependence of relative diffraction intensities from the
Ia3d phase resolves the phase problem, leading to the structural description that the molecular centers are on the rods forming two interpenetrating jungle gyms. Theoretical consideration on the stability of superstructures and systematic MEM analysis reveal the coexistence of two aggregation modes (rods forming an extending jungle gym and closed sheets forming spherical shells) for the
Im3m phase.
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