Applying a combination of melt synthesis followed by long-term annealing a fluorohectorite is obtained which is unique with respect to homogeneity, purity, and particle size. Counterintuitively, the hectorite undergoes a disorder-to-order transition upon swelling to the level of the bilayer hydrate. Alkylammonium-exchanged samples show at any chain length only a single basal spacing corroborating a nicely homogeneous layer charge density. Its intracrystalline reactivity improves greatly upon annealing, making it capable to spontaneously and completely disintegrate into single clay lamellae of 1 nm thickness. Realizing exceptional aspect ratios of around 20,000 upon delamination, this synthetic clay will offer unprecedented potential as functional filler in highly transparent nanocomposites with superior gas barrier and mechanical properties.

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 to exclude 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 pseudohexagonal 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.

Using (13)C double quantum solid-state NMR spectroscopy, we were able to observe nuclei of a supramolecular BTA based additive on the nanoscale in a matrix of i-PP at a concentration of only 0.09 wt%. These nuclei exhibit the analogous structural features as the crystalline phase of the neat additive.

The crystal structure of 1,3,5-tris(2-fluoro-2-methylpropionylamino)benzene was solved by combining powder X-ray diffraction, solid-state NMR spectroscopy and quantum chemical calculations.

Using a combined approach based on scanning electron microscopy, powder X-ray diffraction as well as 1D and 2D multinuclear solid-state NMR spectroscopy, we were able to determine the morphology and the crystal structures for a set of three supramolecular compounds with different hydrogen bonding motifs, namely N,N′-(cyclohexane-trans-1,4-diyl)bis(2,2-dimethylpropanamide) 1, 1,1′-(cyclohexane-trans-1,4-diyl)bis(3-tert-butylurea) 2 and N 1 ,N 4-bis(tert-butylcarbamoyl)cyclohexane-trans-1,4-dicarboxamide 3. Based on a complete signal assignment of the 1D solid-state MAS NMR spectra (1 H, 13 C, 15 N) employing 2D HETCOR experiments and a quantitative evaluation of the corresponding resonances, the content of the asymmetric unit was determined to one half of a molecule. Probing the molecular configuration with 1 H-1 H double-quantum experiments revealed an intramolecular hydrogen bond for compound 3 while 1 and 2 form exclusively intermolecular H-bonds. Ab initio structure solutions applying real space methods with an included close-contact penalty were carried out for all compounds. The following Rietveld refinements led to excellent wR p-values between 2.5% and 4.1%. Compounds 1 and 2 crystallise isostructurally in the monoclinic space group P2 1 /c exhibiting a pseudo-biaxial hydrogen bond motif. 3 crystallises in the triclinic space group P1 with intermolecular head-to-tail hydrogen bonds connecting the molecules to one-dimensional ribbons. Nevertheless, all compounds grow in a sheet-like morphology with lateral dimensions of several hundred micrometres indicating a fast growth in two dimensions along two of the crystal axes. Since all three molecules possess inversion symmetry cancelling the molecular dipole moment the growth mechanism itself has to be dominantly driven by the formation of hydrogen bond networks.