Table 2. Experimental details.
| Phase 1 | Phase 2 | |
|---|---|---|
| Crystal data | ||
| Chemical formula | Na+·C6H7O7 − | Si |
| M r | 214.10 | 28.09 |
| Crystal system, space group | Orthorhombic, P212121 | Cubic, F
d
m
|
| Temperature (K) | 300 | 300 |
| a, b, c (Å) | 7.4527 (3), 7.7032 (3), 13.4551 (4) | 5.43105, 5.43105, 5.43105 |
| α, β, γ (°) | 90, 90, 90 | 90, 90, 90 |
| V (Å3) | 772.45 (5) | 160.20 |
| Z | 4 | 8 |
| Radiation type | Kα1, Kα2, λ = 1.540629, 1.544451 Å | Kα1, Kα2, λ = 1.540629, 1.544451 Å |
| Specimen shape, size (mm) | Flat sheet, 25 × 25 | Flat sheet, 25 × 25 |
| Data collection | ||
| Diffractometer | Bruker D2 Phaser | Bruker D2 Phaser |
| Specimen mounting | Bruker PMMA holder | Bruker PMMA holder |
| Data collection mode | Reflection | Reflection |
| Scan method | Step | Step |
| 2θ values (°) | 2θmin = 5.042 2θmax = 100.048 2θstep = 0.020 | 2θmin = 5.042 2θmax = 100.048 2θstep = 0.020 |
| Refinement | ||
| R factors and goodness of fit | R p = 0.063, R wp = 0.084, R exp = 0.024, R(F 2) = 0.0780, χ2 = 12.180 | R p = 0.063, R wp = 0.084, R exp = 0.024, R(F 2) = 0.0780, χ2 = 12.180 |
| No. of parameters | 76 | 76 |
| No. of restraints | 29 | 29 |
The same symmetry and lattice parameters were used for the DFT calculation. Computer programs: DIFFRAC.Measurement (Bruker, 2009 ▸), Powder4 (Dragoe, 2001 ▸), DASH (David et al., 2006 ▸), GSAS (Larson & Von Dreele, 2004 ▸), EXPGUI (Toby, 2001 ▸), DIAMOND (Crystal Impact, 2015 ▸) and publCIF (Westrip, 2010 ▸).