Table 2. Crystal Data and Structure Refinement Parameters for Na2[Zr(C2O4)3]·2H2O (Na2ZrOx3), K(H7O3)[Zr(C2O4)3]·H2O (KHZrOx3), (NH4) (H7O3)[Zr(C2O4)3]·H2O ((NH4HZrOx3)), Rb(H5O2)0.5(H9O4)0.5[Zr(C2O4)3] (RbHZrOx3), and Cs(H5O2)0.5(H9O4)0.5[Zr(C2O4)3] (CsHZrOx3).
| NaZrOx3 Na2[Zr(C2O4)3]·2H2O | KHZrOx3 K(H7O3)[Zr(C2O4)3]·H2O | NH4HZrOx3 (NH4)(H7O3)[Zr(C2O4)3]·H2O | RbHZrOx3 Rb(H5O2)0.5(H9O4)0.5[Zr(C2O4)3] | CsHZrOx3 Cs(H5O2)0.5(H9O4)0.5[Zr(C2O4)3] | |
|---|---|---|---|---|---|
| CCDC number | 2011398 | 2011399 | 2011400 | 2011401 | 2011402 |
| empirical formula | Na2ZrC6O14H4 | KZrC6O16H9 | ZrC6O16NH13 | RbZrC6O15H7 | CsZrC6O15H7 |
| formula weight | 437.29 | 467.45 | 446.39 | 495.81 | 540.73 |
| temperature/K | 296 | 296 | 296 | 296 | 296 |
| crystal system | monoclinic | monoclinic | monoclinic | triclinic | triclinic |
| space group | C2/c | P21/c | P21/c | P1̅ | P1̅ |
| a/Å | 13.8646(9) | 9.2166(9) | 9.3411(7) | 7.7027(5) | 7.7318(4) |
| b/Å | 10.4241(6) | 11.169(1) | 11.1701(8) | 8.9788(6) | 9.1847(5) |
| c/Å | 8.9290(5) | 14.094(2) | 14.2537(9) | 10.6518(7) | 10.6352(5) |
| α/deg | 90 | 90 | 90 | 79.179(3) | 78.861(2) |
| β/deg | 95.743(3) | 107.718(5) | 107.699(2) | 72.476(4) | 72.333(2) |
| γ/deg | 90 | 90 | 90 | 76.975(3) | 77.713(2) |
| volume/Å3 | 1284.00(13) | 1382.0(2) | 1416.85(17) | 678.70(8) | 696.41(6) |
| Z | 4 | 4 | 4 | 2 | 2 |
| ρcalc g/cm3 | 2.262 | 2.247 | 2.093 | 2.426 | 2.579 |
| μ/mm–1 | 1.006 | 1.191 | 0.871 | 4.459 | 3.449 |
| F(000) | 856 | 928 | 896 | 480 | 511 |
| radiation | Mo Kα (λ = 0.71073) | ||||
| 2Θ range for data collection/deg | 4.90–59.36 | 4.64–53.06 | 4.72–67.34 | 4.69–46.00 | 5.60–68.52 |
| index ranges | –17 ≤ h ≤ 18 | –11 ≤ h ≤ 11 | –14 ≤ h ≤ 14 | –8 ≤ h ≤ 8 | –12 ≤ h ≤ 12 |
| –14 ≤ k ≤ 14 | –13 ≤ k ≤ 14 | –17 ≤ k ≤ 17 | –9 ≤ k ≤ 9 | –14 ≤ k ≤ 14 | |
| –11 ≤ l ≤ 12 | –16 ≤ l ≤ 17 | –21 ≤ l ≤ 22 | –11 ≤ l ≤ 11 | –16 ≤ l ≤ 16 | |
| reflections collected | 11,377 | 21,953 | 58,123 | 14,524 | 37,161 |
| independent reflections | 1722 [Rint = 0.0385, Rsigma = 0.0440] | 2868 [Rint = 0.0389, Rsigma = 0057] | 5638 [Rint = 0.0219, Rsigma = 0.0446] | 1886 [Rint = 0.0411, Rsigma = 0.0655] | 5777 [Rint = 0.0322, Rsigma = 0.0463] |
| data/restraints/parameters | 1722/2/111 | 2868/9/244 | 5638/13/256 | 1886/2/214 | 5777/2/214 |
| goodness-of-fit on F2 | 1.068 | 1.060 | 1.043 | 1.026 | 0.973 |
| final R indexes [I ≥ 2σ (I)] | R1 = 0.0286 | R1 = 0.0291 | R1 = 0.0248 | R1 = 0.0367 | R1 = 0.0377 |
| wR2 = 0.0534 | wR2 = 0.0593 | wR2 = 0.0583 | wR2 = 0.0900 | wR2 = 0.0900 | |
| final R indexes [all data] | R1 = 0.0368 | R1 = 0.0422 | R1 = 0.0340 | R1 = 0.0524 | R1 = 0.0486 |
| wR2 = 0.0572 | wR2 = 0.0640 | wR2 = 0.0624 | wR2 = 0.0986 | wR2 = 0.1020 | |
| largest diff. peak/hole/e Å–3 | 0.77/–0.38 | 0.42/–0.50 | 0.70/–0.43 | 0.90/–0.99 | 2.34/–3.59 |