Table 1. Crystal Data and Structure Refinement Parameters for Zr(OH)2(C2O4) (ZrOx) and (H11O5)2[Zr2(C2O4)5(H2O)4] (H2Zr2Ox5).
| ZrOx Zr(OH)2(C2O4) | H2Zr2Ox5 (H11O5)2[Zr2(C2O4)5(H2O)4] | |
|---|---|---|
| CCDC number | 2011396 | 2011397 |
| empirical formula | C2O6H2Zr1 | C10O34H30Zr2 |
| formula weight | 213.3 | 876.78 |
| temperature/K | 293 | 296 |
| crystal system | Monoclinic | triclinic |
| space group | C2/c | P1̅ |
| a/Å | 12.813(4) | 6.9269(3) |
| b/Å | 5.8882(14) | 10.4427(6) |
| c/Å | 6.7088(13) | 10.6447(6) |
| α/deg | 90 | 78.421(2) |
| β/deg | 118.25(2) | 86.155(2) |
| γ/deg | 90 | 89.945(2) |
| volume/Å3 | 445.9(2) | 752.56(7) |
| Z | 4 | 1 |
| ρcalc g/cm3 | 3.177 | 1.935 |
| μ/mm–1 | 20.01 | 0.821 |
| F(000) | 408 | 442 |
| radiation | Cu Kα | Mo Kα |
| 2Θ range for data collection/deg | 5–110 (stepsize 0.02) | 3.90–51.88 |
| index ranges | –8 ≤ h ≤ 8 | |
| –12 ≤ k ≤ 12 | ||
| –13 ≤ l ≤ 13 | ||
| reflections collected | 19,393 | |
| independent reflections | 2914 [Rint = 0.0389, Rsigma = 0.0581] | |
| data/restraints/parameters | 5614/39/9 | 2914/15/253 |
| goodness-of-fit on F2 | 4.45 | 1.045 |
| final R indexes [I ≥ 2σ (I)] | R1 = 0.0417 wR2 = 0.0600 | R1 = 0.0282 wR2 = 0.0529 |
| final R indexes [all data] | R1 = 0.0417 wR2 = 0.0600 | R1 = 0.0378 wR2 = 0.0566 |
| largest diff. peak/hole/e·Å–3 | 1.01/–1.82 | 0.55/–0.40 |