Table 2.
Crystallographic data for complexes 1, 5, 7, 9 and 10.
| 1 | 5 | 7 | 9 | 10 | |
|---|---|---|---|---|---|
| formula | C38H55Cl2N4Nb | C41H58Cl2N3Nb | C40H57ClN3Nb | C42H64N5Nb | C44H69N6Nb |
| fw | 731.67 | 756.71 | 708.25 | 731.89 | 774.96 |
| space group | P21/c | Pbca | P212121 | Pbca | P21/n |
| a (Å) | 8.865(1) | 17.840(5) | 13.757(2) | 19.649(1) | 15.530(3) |
| b (Å) | 17.986(2) | 21.065(6) | 16.524(3) | 18.887(1) | 12.284(2) |
| c (Å) | 24.392(2) | 21.778(6) | 17.039(3) | 22.364(1) | 23.724(4) |
| α (°) | 90 | 90 | 90 | 90 | 90 |
| β (°) | 99.792(1) | 90 | 90 | 90 | 107.887(3) |
| γ (°) | 90 | 90 | 90 | 90 | 90 |
| V (Å3) | 3832.8(6) | 8184(4) | 3873.3(11) | 8299.5(9) | 4307.3(14) |
| Z | 4 | 8 | 4 | 8 | 4 |
| ρcalcd (g/cm3) | 1.268 | 1.228 | 1.215 | 1.171 | 1.195 |
| F000 | 1544 | 3200 | 1504 | 3136 | 1664 |
| μ (cm−1) | 0.48 | 0.46 | 0.41 | 0.32 | 0.31 |
| Tmin/Tmax | 0.917772 | 0.90033 | 0.870265 | 0.887106 | 0.921823 |
| no. rflns measured | 16890 | 37957 | 17262 | 33520 | 17130 |
| no. indep. rflns | 6495 | 8076 | 6488 | 5593 | 6328 |
| Rint | 0.0291 | 0.0398 | 0.0626 | 0.0517 | 0.0457 |
| no. obs. (I > 2.00σ(I)) | 5096 | 6046 | 5497 | 4337 | 4105 |
| no. variables | 406 | 426 | 407 | 433 | 460 |
| R1a, wR2b | 0.0367, 0.0872 | 0.0356, 0.0860 | 0.0473, 0.1137 | 0.0349, 0.0862 | 0.0406, 0.0910 |
| R1 (all data) | 0.0531 | 0.0560 | 0.0617 | 0.0521 | 0.0792 |
| goodness-of-fit on F2 | 1.206 | 1.117 | 0.969 | 1.382 | 1.071 |
| res. peak, hole (e−/Å3) | 1.014, −0.399 | 0.882, −0.287 | 1.261, −0.298 | 0.417, −0.308 | 0.717, −0.393 |
| CCDC ref. # | 675084 | 758024 | 758023 | 675086 | 758025 |
a
R1 = Σ(|Fo| − |Fc|)/Σ(|Fo|);
b
wR2 = [Σ{w(Fo2 − Fc2)2}/Σ{w(Fo2)2}]1/2