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Contents; 1 SHELXL; 1.1 The SHELX program suite; 1.1.1 SHELXTL and other programs; 1.2 SHELXL; 1.2.1 Program organization; 1.2.2 The instruction file name.ins; 1.2.3 The reflection data file name.hkl; 1.2.4 Merging data in SHELXL; 1.2.5 The connectivity table; 2 Crystal structure refinement; 2.1 Least-squares refinement; 2.1.1 Refinement against F or F[sup(2)]-is that a question?; 2.2 Weak data and high-resolution cut-off; 2.3 Residual factors; 2.4 Parameters; 2.5 Constraints; 2.5.1 Site occupancy factors; 2.5.2 Special position constraints; 2.5.3 Rigid group constraints |
2.5.4 Floating origin constraints2.5.5 Hydrogen atoms; 2.5.6 Constraints in SHELXL; 2.6 Restraints; 2.6.1 Geometrical restraints; 2.6.2 Restraints on displacement parameters; 2.6.3 Other restraints; 2.7 Free variables in SHELXL; 2.8 Results; 2.8.1 Bond lengths and angles; 2.8.2 Torsion angles; 2.8.3 Atoms on common planes; 2.8.4 Hydrogen bonds; 2.8.5 The RTAB command; 2.8.6 The MORE command; 2.8.7 The .cif file; 2.9 Refinement problems; 3 Hydrogen atoms; 3.1 X--H bond lengths and U[sub(eq)] values of H atoms; 3.2 Hydrogen bound to different atom types; 3.2.1 Hydrogen bound to carbon atoms |
3.2.2 Hydrogen bound to nitrogen and oxygen3.2.3 Hydrogen bound to metals; 3.3 Placing hydrogen atoms in SHELXL; 3.3.1 List of most common m and n values in HFIX commands; 3.3.2 Semi-free refinement of acidic hydrogen atoms; 3.4 Hydrogen bonds in SHELXL; 3.5 Examples; 3.5.1 Routine hydrogen atom placement: C[sub(31)]H[sub(54)]MoN[sub(2)]O[sub(2)]; 3.5.2 Hydrogen atoms in a Zr-hydride; 3.5.3 Acidic hydrogen atoms and hydrogen bonds; 4 Atom type assignment; 4.1 All electrons are blue; 4.2 Chemical knowledge; 4.3 Crystallographic knowledge; 4.4 Examples |
4.4.1 Tetrameric InCl[sub(3)]-the N or O question4.4.2 A cobalt salt; 4.4.3 Unclear central metal atom; 5 Disorder; 5.1 Types of disorder; 5.1.1 Substitutional disorder; 5.1.2 Positional disorder; 5.1.3 Mess-a special case of disorder; 5.2 Refinement of disorder; 5.2.1 Refinement of disorder with SHELXL; 5.3 Examples; 5.3.1 Gallium-iminosilicate-Disorder of two ethyl groups; 5.3.2 Disorder of a Ti(III) compound; 5.3.3 A mixed crystal treated as occupancy disorder; 5.3.4 Disorder of solvent molecules; 5.3.5 Three types of disorder in one structure: cycloikositetraphenylene; 6 Pseudo-Symmetry |
6.1 Global pseudo-symmetry6.2 True NCS; 6.3 Examples; 6.3.1 Pn or P2[sub(1)]/n; 6.3.2 [Si(NH[sub(2)])[sub(2)]CH(SiMe[sub(3)])[sub(2)]][sub(2)]: P1 with Z = 12; 7 Twinning; 7.1 Definition of a Twin; 7.2 Classification of twins; 7.2.1 Twinning by merohedry; 7.2.2 Twinning by pseudo-merohedry; 7.2.3 Twinning by reticular merohedry; 7.2.4 Non-merohedral twins; 7.3 Tests for twinning; 7.4 Structure solution; 7.5 Twin refinement; 7.6 Determination of the absolute structure; 7.7 Warning signs of twinning; 7.8 Examples; 7.8.1 Twinning by merohedry; 7.8.2 An example of pseudo-merohedral twinning |
7.8.3 First example of twinning by reticular merohedry |