Crystal Structure of a Highly Efficient Clarifying Agent for Isotactic Polypropylene

Titelangaben

Schmidt, Marko ; Wittmann, Johannes J. ; Kress, Roman ; Schneider, Denis ; Steuernagel, Stefan ; Schmidt, Hans-Werner ; Senker, Jürgen:
Crystal Structure of a Highly Efficient Clarifying Agent for Isotactic Polypropylene.
In: Crystal Growth & Design. Bd. 12 (2012) Heft 5 . - S. 2543-2551.
ISSN 1528-7505
DOI: https://doi.org/10.1021/cg300151s

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Abstract

Using a combined approach based on X-ray powder diffraction and solid-state NMR spectroscopy we were able to determine the crystal structure of 1,3,5-tris(2,2-dimethylpropionylamino)benzene, an efficient clarifying agent for isotactic polypropylene. The XPRD data and 1D solid-state NMR experiments allowed excluding most of the possible primitive orthorhombic space groups with the exception of 11. The structure solution was carried out using real space methods including a close-contact penalty. Four space groups lead to reasonable wRp values below 10 %. 13C13C double quantum (DQ) experiments of the labeled carbonyl group were measured with a supercycled symmetry based dipolar recoupling sequence. Taking into account the wRp values after Rietveld refinement as well as simulations of DQ build-up curves based on nine spin systems, the space group P212121 is clearly favored. The largest dipolar coupling within these spin systems was about 60 Hz corresponding to a distance of 5 Å. 1,3,5-tris(2,2-dimethylpropionylamino)benzene crystallizes in an orthorhombic metric (a = 14.91(5) Å, b = 24.05(8) Å, c = 6.80(2) Å). The molecules are arranged in a pseudo hexagonal rod packing with medium-strong hydrogen bonds and π-stacking. The antiferroelectric arrangement of neighbored rods leads to an averaging of the net dipolar moment in the whole crystal.