Table 2. Experimental details.
| Co2(O2CC6H4C6H4CO2)(OH)2 | Ni2(O2CC6H4C6H4CO2)(OH)2 | (NH4)2BPDC | |
|---|---|---|---|
| Crystal data | |||
| Chemical formula | [Co(C14H8O4)0.5(OH)] | [Ni(C14H8O4)0.5(OH)] | 2NH4 +·C14H8O4 2− |
| M r | 392.09 | 391.63 | 276.29 |
| Crystal system, space group | Triclinic, P
|
Triclinic, P
|
Triclinic, P1 |
| Temperature (K) | 300 | 300 | 300 |
| a, b, c (Å) | 14.16 (5), 6.269 (3), 3.323 (4) | 15.0 (11), 6.04 (12), 4.04 (9) | 4.6770 (6), 5.2306 (14), 14.387 (6) |
| α, β, γ (°) | 91.43 (2), 98.46 (7), 90.0 (3) | 82.7 (2), 72.3 (8), 82 (2) | 90.57 (7), 91.41 (4), 92.775 (11) |
| V (Å3) | 291.6 (2) | 345 (2) | 351.43 (17) |
| Z | 1 | 1 | 1 |
| Radiation type | Kα1,2, λ = 0.70932, 0.71361 Å | Kα1,2, λ = 1.54059, 1.54445 Å | Kα1,2, λ = 0.70932, 0.71361 Å |
| Specimen shape, size (mm) | Cylinder, 12 × 0.7 | Flat sheet, 16 × 16 | Cylinder, 12 × 0.7 |
| Data collection | |||
| Diffractometer | PANalytical Empyrean | PANalytical X’Pert | PANalytical Empyrean |
| Specimen mounting | Glass capillary | Si zero-background cell with well | Glass capillary |
| Data collection mode | Transmission | Reflection | Transmission |
| Scan method | Step | Step | Step |
| 2θ values (°) | 2θmin = 1.002 2θmax = 49.991, 2θstep = 0.008 | 2θmin = 4.008 2θmax = 99.998, 2θstep = 0.017 | 2θmin = 1.008 2θmax = 49.982, 2θstep = 0.008 |
| Refinement | |||
| R factors and goodness of fit | R p = 0.065, R wp = 0.092, R exp = 0.022, R(F 2) = 0.11340, χ2 = 21.977 | R p = 0.042, R wp = 0.059, R exp = 0.011, R(F 2) = 0.09176, χ2 = 30.426 | R p = 0.033, R wp = 0.043, R exp = 0.015, R(F 2) = 0.09394, χ2 = 14.055 |
| No. of parameters | 49 | 47 | 93 |
| No. of restraints | 64 | 30 | 55 |
| (Δ/σ)max | 2.587 | 4.433 | 0.723 |
The same symmetry and lattice parameters were used for the DFT calculations as for each powder diffraction study. Computer program: GSAS-II (Toby & Von Dreele, 2013 ▸).