Table 3. Experimental details.
| [NaRb(C6H6O7)] | [NaCs(C6H6O7)] | |
|---|---|---|
| Crystal data | ||
| M r | 298.57 | 346.00 |
| Crystal system, space group | Triclinic, P
|
Monoclinic, I2 |
| Temperature (K) | 300 | 300 |
| a, b, c (Å) | 5.9864 (2), 8.4104 (3), 10.2903 (3) | 10.8913 (5), 5.5168 (2), 17.7908 (8) |
| α, β, γ (°) | 74.798 (3), 76.756 (3), 72.878 (2) | 90, 97.014 (4), 90 |
| V (Å3) | 471.28 (3) | 1060.96 (6) |
| Z | 2 | 4 |
| Radiation type | Kα1, Kα2, λ = 1.540593, 1.544451 Å | Kα1, Kα2, λ = 0.709319, 0.713609 Å |
| μ (mm−1) | – | 2.09 |
| Specimen shape, size (mm) | Flat sheet, 24 × 24 | Cylinder, 12 × 0.3 |
| Data collection | ||
| Diffractometer | Bruker D2 Phaser | PANalytical Empyrean |
| Specimen mounting | Standard holder | Glass capillary |
| Data collection mode | Reflection | Transmission |
| Scan method | Step | Step |
| 2θ values (°) | 2θmin = 5.001 2θmax = 100.007 2θstep = 0.020 | 2θmin = 1.011 2θmax = 49.991 2θstep = 0.017 |
| Refinement | ||
| R factors and goodness of fit | R p = 0.028, R wp = 0.038, R exp = 0.022, R(F 2) = 0.13613, χ2 = 3.028 | R p = 0.045, R wp = 0.059, R exp = 0.026, R(F 2) = 0.08622, χ2 = 5.570 |
| No. of parameters | 84 | 80 |
| No. of restraints | 29 | 29 |
| H-atom treatment | Only H-atom displacement parameters refined | Only H-atom displacement parameters refined |
The same symmetry and lattice parameters were used for the DFT calculations as for each powder diffraction study. Computer programs: DIFFRAC.Measurement (Bruker, 2009 ▸), FOX (Favre-Nicolin & Černý, 2002 ▸), GSAS (Larson & Von Dreele, 2004 ▸), Mercury (Macrae et al., 2008 ▸), DIAMOND (Crystal Impact, 2015 ▸) and publCIF (Westrip, 2010 ▸).