RESUMEN
A boron-rich sodium boride, formerly known as NaB15, has been subjected to a comprehensive structural reinvestigation using X-ray single-crystal and powder diffraction, low-temperature neutron and electron diffraction, high-resolution transmission electron microscopy, and 23Na solid-state NMR spectroscopy. The results indicate that the previously published orthorhombic space group is incorrect. Consistent with all of the experimental results a modified structural description is developed in the monoclinic space group Ilml (a = 585.92(3), b= 1039.92(6), c = 833.17(5) pin, beta = 90.373(5) from powder data). Because one of the interstitial boron atom positions remains unoccupied, the accurate compositional formula is NaB145 or Na2B29.
RESUMEN
Chemical transport experiments are a valuable aid of great potential in the synthesis and thermochemical characterization of solids. Compounds of interest can often only be crystallized by this method. The use of a transport balance allows very detailed observations, particularly of the course of the experiment over time (simultaneous or sequential deposition of multiple-phase solids). The computer program CVTRANS enables a quantitative thermochemical description of the experiment based on the cooperative transport model. A compilation of recent results illustrates the development and efficiency of the method. The transport of phosphides, anhydrous phosphates and sulfates, and rare-earth oxide and oxohalide compounds are treated in detail.