Table 1.
Crystal data for lanthanide complexes (La-Gd) with TREN-1,2-HOIQO (1).
| [La(1)(H2O)] • H2O | [Pr(1)(H2O)] • H2O | [Nd(1)(H2O)] • H2O | [Sm(1)(H2O)] • H2O | [Eu(1)(H2O)] • H2O | [Gd(1)(H2O)] • H2O | |
|---|---|---|---|---|---|---|
| formula | C36H34LaN7O11 | C36H34N7O11Pr | C36H34N7NdO11 | C36H34N7O11Sm | C36H34EuN7O11 | C36H34GdN7O11 |
| mol. weight | 879.61 | 881.61 | 884.94 | 891.05 | 892.66 | 897.95 |
| crystal app. | colorless plate | red plate | red plate | red plate | colorless plate | colorless plate |
| crystal system | monoclinic | monoclinic | monoclinic | monoclinic | monoclinic | monoclinic |
| space group | P21/c | P21/c | P21/c | P21/c | P21/c | P21/c |
| a [Å] | 12.3545(11) | 12.3482(14) | 12.355(5) | 12.3528(13) | 12.380(3) | 12.3590(18) |
| b [Å] | 26.745(2) | 26.594(3) | 26.521(5) | 26.371(3) | 26.314(5) | 26.307(4) |
| c [Å] | 10.6674(9) | 10.6089(12) | 10.605(5) | 10.6066(11) | 10.612(2) | 10.5933(15) |
| α [°] | 90 | 90 | 90 | 90 | 90 | 90 |
| β [°] | 97.018(2) | 96.581(2) | 96.512(5) | 96.441(2) | 96.470(4) | 96.343(3) |
| γ [°] | 90 | 90 | 90 | 90 | 90 | 90 |
| volume [Å3] | 3498.3 (5) | 3460.9(7) | 3452(2) | 3433.3(6) | 3435.0(12) | 3423.1(9) |
| Z | 4 | 4 | 4 | 4 | 4 | 4 |
| ρ [g cm−1] | 1.67 | 1.69 | 1.70 | 1.72 | 1.73 | 1.74 |
| μ [mm−1] | 1.30 | 1.48 | 1.58 | 1.79 | 1.90 | 2.01 |
| crystal size [mm3] | 0.24×0.22×0.09 | 0.27×0.13×0.09 | 0.30×0.15×0.08 | 0.28×0.13×0.06 | 0.15×0.07×0.04 | 0.19×0.13×0.06 |
| temperature [K] | 160(2) | 157(2) | 156(2) | 159(2) | 158(2) | 164(2) |
| radiation [Å] | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) |
| θ max [°] | 26.40 | 26.37 | 26.39 | 26.40 | 26.37 | 26.42 |
| meas. refls. | 19871 | 19631 | 19552 | 19446 | 19433 | 19276 |
| indep. refls. | 7071 | 7016 | 6951 | 6953 | 6936 | 6861 |
| refls. in ref. | 5080 (I ≥ 2σ(I)) | 4840 (I ≥ 2σ(I)) | 4620 (I ≥ 2σ(I)) | 4741 (I ≥ 2σ(I)) | 4280 (I ≥ 2σ(I)) | 4343 (I ≥ 2σ(I)) |
| parameters | 496 | 496 | 496 | 496 | 496 | 496 |
| R[a] | 0.0610 | 0.0507 | 0.0530 | 0.0483 | 0.0584 | 0.0564 |
| wR[b] | 0.1474 | 0.1086 | 0.1130 | 0.1042 | 0.1183 | 0.1138 |
| R[a] (all data) | 0.0897 | 0.0860 | 0.0951 | 0.0849 | 0.1120 | 0.1054 |
| wR (all data) | 0.1598 | 0.1194 | 0.1264 | 0.1148 | 0.1345 | 0.1285 |
| GoF | 1.050 | 1.035 | 1.030 | 1.026 | 1.008 | 1.003 |
| Δρmax [e/Å3] | 4.39 (near La) | 1.01 | 1.48 | 1.39 | 1.36 | 1.85 |
| Δρmin [e/Å3] | −0.14 | −0.64 | −0.86 | −0.87 | −0.75 | −0.73 |
[a]
R factor definition: R = Σ (‖F0| – |Fc‖) / Σ |F0|.
[b]
SHELX-97 wR factor definition: wR = [Σ w(F02 – Fc2)2 / Σ w(F02)]1/2. Weighting scheme: w = 1 / [σ2(F0)2 + (np)2], p = [F02 + 2 Fc2] / 3.