第十二章 结构的表达与CIF.ppt

第十二章结构的表达与 CIF 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?D c和D m?F (000) ? Crystal size ? Absorption coefficient M DVZNV ZMD c A c6606 .1 or ?????? Temperature :K ? Color ?λ (Mo K α)? Limiting indices :h, k, l的上下限?θ range ? All/unique reflections/ R int ? Completeness ? Data/restraints/parameters ? Observed relections [ I > 2 σ(I )] ? GOF on F 2 [I > 2 σ(I )] ? GOF on F 2 (all data) ?R indices [ I > 2 σ(I )]: R 1, wR 2?R indices (all data): R 1, wR 2? Largest difference peak/hole ? Residual electron density Item Data Item Parameter empirical formula Al 12 Br 24H 108O 60 limiting indices -28 ≤ h ≤+19 -28 ≤k ≤+27 temp (K) 100(2) -27 ≤ l ≤+28 cryst syst cubic ? range ( °) - space group Fd-3m (No. 227) all/unique reflns/ R int 16411/600/ a (?) (2) completeness (%) volume (? 3) 9281(3) data/restraints/param 600/0/48 Z4 obsd reflns [ I ? 2?(I )] 576 D c (g/cm 3) GOF on F 2 [ I ? 2?(I )] F (000) 6336 GOF on F 2 (all data) crystal size (mm 3) × × R indices [ I ? 2?(I )] R 1 = , wR 2 = abs coeff (mm -1 ) R indices (all data) R 1 = , wR 2 = color Colorless largest difference peak/hole (e/ ? 3) /- ?(Mo K ?) (?) residual electron density (e/ ? 3) Table 1. Crystallographic data and structure refinement parameters 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 [Al 4 (OH) 6 (H 2 O) 12] 6+ (Al 4 ) and [Al(H 2 O) 6] 3+ (Al 1 ): (A and B) Ellipsoid-stick representations with a probability of 80%, (C and D) Polyhedral representations. B AC D Crystal Stru