Gold nanocrystals passivated by self‐assembled monolayers of straightchain alkylhiolate molecules have been obtained as highly purified molecular materials of high intrinsic stability. Evidence is presented for a predicted discrete sequence of energetically optimal fcc structures of a truncated octahedral morphological motif (see cover). The nanocrystal materials have a propensity to form extended superlattics, such as that in the Figure.

Anisotropic line-shape broadening (peak width which is not a smooth function of d-spacing) is frequently observed in powder diffraction patterns, and can be a source of considerable dif®culty for whole-pattern ®tting or Rietveld analysis. A model of the multi-dimensional distribution of lattice metrics within a powder sample is developed, leading naturally to a few parameters which can be varied to achieve optimal line-shape ®ts. Conditions on these parameters are derived for all crystal systems, and the method is illustrated with two examples: sodium p-hydroxybenzoate and rubidium fulleride.