Table 2.
Crystal data for lanthanide complexes (Tb-Lu) with TREN-1,2-HOIQO (1).
| [Tb(1)(H2O)] • H2O | [Dy(1)(H2O)] • H2O | [Ho(1)(H2O)] • H2O | [Er(1)(H2O)] • H2O | [Tm(1)(H2O)] • H2O | [Yb(1)(H2O)] • H2O | [Lu(1)(H2O)] • H2O | |
|---|---|---|---|---|---|---|---|
| formula | C36H34N7O11Tb | C36H34DyN7O11 | C36H34HoN7O11 | C36H34ErN7O11 | C36H34N7O11Tm | C36H34N7O11Yb | C36H34LuN7O11 |
| mol. weight | 899.62 | 903.20 | 905.63 | 907.96 | 909.63 | 913.74 | 915.67 |
| crystal app. | yellow plate | colorless plate | colorless plate | colorless plate | colorless needle | red plate | colorless plate |
| crystal system | monoclinic | monoclinic | monoclinic | monoclinic | monoclinic | monoclinic | monoclinic |
| space group | P21/c | P21/c | P21/c | P21/c | P21/c | P21/c | P21/c |
| a [Å] | 12.3216(14) | 12.3472(15) | 12.345(2) | 12.3589(18) | 12.3920(13) | 12.336(5) | 12.417(2) |
| b [Å] | 26.295(3) | 26.188(3) | 26.153(4) | 26.132(4) | 26.162(3) | 26.006(10) | 26.193(4) |
| c [Å] | 10.5618(12) | 10.5624(12) | 10.5557(17) | 10.5565(15) | 10.5522(12) | 10.546(4) | 10.5619(17) |
| α [°] | 90 | 90 | 90 | 90 | 90 | 90 | 90 |
| β [°] | 96.335(2) | 96.220(2) | 96.306(3) | 96.277(2) | 96.357(3) | 96.443(5) | 96.436(4) |
| γ [°] | 90 | 90 | 90 | 90 | 90 | 90 | 90 |
| volume [Å3] | 3401.0(7) | 3395.2(7) | 3387.3(10) | 3388.9(8) | 3400.0(6) | 3362(2) | 3413.4(10) |
| Z | 4 | 4 | 4 | 4 | 4 | 4 | 4 |
| ρ [g cm−1] | 1.76 | 1.77 | 1.78 | 1.78 | 1.78 | 1.81 | 1.78 |
| μ [mm−1] | 2.16 | 2.23 | 2.41 | 2.55 | 3.21 | 2.86 | 3.56 |
| crystal size [mm3] | 0.24×0.22×0.09 | 0.18×0.16×0.06 | 0.18×0.09×0.06 | 0.22×0.08×0.06 | 0.09×0.01×0.01 | 0.15×0.07×0.04 | 0.10×0.04×0.02 |
| temperature [K] | 159(2) | 162(2) | 161(2) | 165(2) | 173(2) | 158(2) | 173(2) |
| radiation [Å] | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) | MoKα (λ=0.71073) | synchro. (λ=0.7749) | MoKα (λ=0.71073) | synchro. (λ=0.7749) |
| θ max [°] | 26.40 | 26.45 | 26.39 | 26.39 | 29.19 | 26.44 | 25.62 |
| meas. refls. | 19325 | 19202 | 19179 | 19114 | 35089 | 16284 | 20804 |
| indep. refls. | 6901 | 6888 | 6833 | 6866 | 7007 | 6475 | 4946 |
| refls. in ref. | 4833 (I ≥ 2σ(I)) | 5033 (I ≥ 2σ(I)) | 4390 (I ≥ 2σ(I)) | 4446 (I ≥ 2σ(I)) | 5731 (I ≥ 2σ(I)) | 3542 (I ≥ 2σ(I)) | 4578 (I ≥ 2σ(I)) |
| parameters | 496 | 496 | 496 | 496 | 496 | 496 | 496 |
| R[a] | 0.0517 | 0.0456 | 0.0551 | 0.0489 | 0.0474 | 0.0594 | 0.0313 |
| wR[b] | 0.1189 | 0.1027 | 0.1079 | 0.0986 | 0.1107 | 0.1059 | 0.0804 |
| R[a] (all data) | 0.0849 | 0.0725 | 0.1045 | 0.0976 | 0.0597 | 0.1432 | 0.0340 |
| wR (all data) | 0.1299 | 0.1121 | 0.1219 | 0.1118 | 0.1149 | 0.1312 | 0.0820 |
| GoF | 1.024 | 1.037 | 1.013 | 0.993 | 1.096 | 0.964 | 1.097 |
| Δρmax [e/Å3] | 2.54 | 1.35 | 1.10 | 1.15 | 1.63 | 2.61 | 1.66 |
| Δρmin [e/Å3] | −0.84 | −0.88 | −0.93 | −1.04 | −1.97 | −0.84 | −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.