No abstract

The structure of the new medium-pore aluminophosphate molecular sieve PST-6 is determined by the combined use of rotation electron diffraction tomography, synchrotron X-ray powder diffraction, and computer modeling. PST-6 was prepared by calcination of another new aluminophosphate material with an unknown structure synthesized using diethylamine as a structure-directing agent, which is thought to contain bridging hydroxy groups. PST-6 has 36 crystallographically distinct tetrahedral sites in the asymmetric unit and is thus crystallographically the most complex zeolitic structure ever solved.

1,5-(1,4-diazabicyclo[2.2.2]octane)pentyl dibromide (diDABCO-C5)13.0 g (0.06 mol) of 1,5-dibromopentane was dissolved in 50 mL ethanol and added droop-wise to a solution under stirring at 50 °C of 33.6 g (0.30 mol) of 1,4-diazabicyclo[2.2.2]octane (DABCO) dissolved in 100 mL ethanol. The mixture was refluxed for 24 hours. Once cold, the excess of ethanol was removed on a rotary evaporator leaving yellow oil. Subsequently cold

Organic structure-directing agents (OSDAs), such as quaternary ammonium cations and amines, used in the synthesis of zeolites and related crystalline microporous oxides usually end up entrapped inside the void spaces of the crystallized inorganic host lattice. But none of them is known to form direct chemical bonds to the framework of these industrially important catalysts and adsorbents. We demonstrate that ECR-40, currently regarded as a typical silicoaluminophosphate molecular sieve, constitutes instead a new family of inorganic-organic hybrid networks in which the OSDAs are covalently bonded to the inorganic framework. ECR-40 crystallization begins with the formation of an Al-OSDA complex in the liquid phase in which the Al is octahedrally coordinated. This unit is incorporated in the crystallizing ECR-40. Subsequent removal of framework-bound OSDAs generates Al-O-Al linkages in a fully tetrahedrally coordinated framework.

A microporous silicoaluminophosphate with a novel topology type, STA-20, has been prepared via a dual templating method using hexamethylene bisdiazabicyclooctane (diDABCO-C6) and trimethylamine as co-templates. Its structure has been solved and 2 confirmed using a multi-technique approach that included the use of a hypothetical zeolite database to obtain a candidate starting structure, followed by scanning transmission electron microscopy with annular dark field imaging and Rietveld refinement. STA-20 is a member of the ABC-6 family of zeotype structures. The structure has trigonal symmetry, P-31c, with a = 13.15497(18) Å and c = 30.5833(4) Å in the calcined form. It has a 12-layer stacking sequence of 6-rings (6Rs), AABAABAACAAC(A), which contains single and double 6R units. As well as d6r, can and gme cages, STA-20 possesses the longest cage observed in an ordered ABC-6 material, giving a 3D-connected pore system limited by 8R windows. Models for the location of the templates within cages of the framework were obtained by combining elemental analysis, 13 C MAS NMR, computer modelling and Rietveld refinement.