Zeolite Rho Loaded with Methylamines. III. Trimethylamine Loadings
Samples of two differently prepared zeolites rho loaded with different amounts of trimethylamine (TMA) were studied in their hydrated and dehydrated forms by X-ray and neutron diffraction experiments. Both zeolites are partially dealuminated, as indicated by nonframework Al, which is assumed to be Al2O3 or AlOOH. Series I was prepared from dry-calcined NHn-rho at 873 K, series II from steam-calcined NHn-rho at 773 K. The samples were loaded with different amounts of deuterated TMA. Rietveld refinements yielded the following results for series I: (1) H3.8(H-TMA)5Cs0.2Al9 Si39O96.Al2O3.22H2O, X-ray data collection at room temperature, Im\overline 3m, a = 15.0542 (2) Å, R wp = 0.094; (2) composition as in (1) (anhydrous), neutron data collection at 5 K of dehydrated and deuterated sample, Im3m, a = 15.0467 (4) Å, R wp = 0.034. Series II: (3) H0.3(H-TMA)5Cs0.7Al6Si42O96.2.5Al2O3.22H2O, X-ray data collection at room temperature, Im\overline 3m, a = 15.0574 (2) Å, R wp = 0.118; (4) composition as in (3) (anhydrous), neutron data collection at 5 K of dehydrated and deuterated sample, lm\overline 3m, a = 15.0761 (5) Å, R wp = 0.037. In all determinations the TMA molecules reside with the N and H (D in neutron diffraction analysis) atoms on the central axes (x, 0, 0) pointing towards the center of the single eight-ring, whilst the three methyl groups point away to the center of the \alpha-cage.