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The theoretically observable limit of electron density distribution by single-crystal X-ray diffraction is discussed. When F_{orb} and {\delta}F are defined as, respectively, the partial structure factor for an orbital and the deviation of the observed F from the true F, the accuracy of electron density attributable to F_{orb} is chiefly determined by the number of reflections satisfying the condition F_{orb}/F > {\delta}F/F. Since F_{orb}/F, which is generally small for crystals with large F(0,0,0), is constant under a given set of experimental conditions, {\delta}F/F must be reduced to increase the number of reflections satisfying F_{orb}/F > {\delta}F/F. The present paper demonstrates how to reduce {\delta}F mathematically and experimentally, and the following topics are covered: the Poisson statistics, accumulation of errors in the data collection and reduction procedure, multiple diffraction, conversion error from F^2 to F in refinement programs, which is unavoidable when the input quantities have different dimension from F, weighting of reflections, and tips. For demonstration, observation of the electron density of the Ti-3d^1 orbital in YTiO_3 by synchrotron single-crystal X-ray diffraction is presented., Comment: 68 pages, 20 figures

Single crystals of K$_x$Fe$_{2-y}$Se$_2$ are prepared by quenching at various temperatures. The crystals obtained at higher quenching temperatures have a surface morphology with mesh-like texture. They show a sharp superconducting transition at $T_\rm{c}$ ~32 K with a large shielding volume fraction. On the other hand, the crystals prepared without quenching show an onset superconducting transition at ~44 K and a zero resistivity around ~33 K, and they possess island-like regions on the surface with a larger amount of Fe incorporation. In-situ high-temperature single crystal X-ray diffraction measurements tell us the Fe-vacancy ordered phase is generated at a temperature region around 270 {\deg}C via iron diffusion. The creation of this Fe-vacancy ordered phase may become a driving force of the growth of the higher $T_\rm{c}$ phase. The superconductivity at ~44 K is attributed to a metallic phase with no Fe-vacancy., Comment: 14 pages, 6 figures