第十二章 结构的表达及CIF.ppt

第十二章 结构的表达与CIF 12.1 Crystallographic Data and Structure Refinement Parameters Empirical formula：与Z关联 Formula weight Crystal system Space group (No.) Unit cell parameters：等长列一，特角不列 V Z Dc和Dm F(000) Crystal size Absorption coefficient Temperature：K Color λ (Mo Kα) Limiting indices：h, k, l的上下限 θ range All/unique reflections/Rint Completeness Data/restraints/parameters Observed relections [I 2σ(I)] GOF on F2 [I 2σ(I)] GOF on F2 (all data) R indices [I 2σ(I)]: R1, wR2 R indices (all data): R1, wR2 Largest difference peak/hole Residual electron density Item Data Item Parameter empirical formula Al12Br24H108O60 limiting indices -28 ≤ h ≤ +19 fw 3310.46 -28 ≤ k ≤ +27 temp (K) 100(2) -27 ≤ l ≤ +28 cryst syst cubic ? range (°) 1.68-28.32 space group Fd-3m (No. 227) all/unique reflns/Rint 16411/600/0.0447 a (?) 21.015(2) completeness (%) 99.8 volume (?3) 9281(3) data/restraints/param 600/0/48 Z 4 obsd reflns [I ? 2?(I)] 576 Dc (g/cm3) 2.369 GOF on F2 [I ? 2?(I)] 1.074 F(000) 6336 GOF on F2 (all data) 1.074 crystal size (mm3) 0.20×0.20×0.10 R indices [I ? 2?(I)] R1 = 0.0328, wR2 = 0.0878 abs coeff (mm-1) 10.549 R indices (all data) R1 = 0.0342, wR2 = 0.0885 color Colorless largest difference peak/hole (e/?3) 0.938/-1.669 ? (Mo K?) (?) 0.71073 residual electron density (e/?3) 0.121 Table 1. Crystallographic data and structure refinement parameters 12.2 Molecular Structure Molecular structure and symmetry Atomic coordinates and thermal parameters Bond lengths and bond angles Torsion angle Dihedral angle Structural graphics ellipsoid-stick ball-stick (lines) polyhedron (space filling) Ionic structures of [Al4(OH)6(H2O)12]6+ (Al4) and [Al(H2O)6]3+ (Al1): (A and B) Ellipsoid-stick representations with a probability of 80%, (C and D) Polyhedral representations. B A C D 12.3 Crystal Structure Packing diagram Polyhedra and linking Three-dimensional perspective H bonds and intermolecular interaction Simulated powder XRD pattern Electron-density map C a b c a b c B