Table 6. Crystal Data and Measurement Details for 3·2CH3OH, 4·0.5Et2O·solv, 5·CH2Cl2·2H2O, 6·solv, 7·CH3COCH3·H2O, and 8·2H2O.
| 3·2CH3OH | 4·0.5Et2O·solv | 5·CH2Cl2·2H2O | 6·solv | 7·CH3COCH3·H2O | 8·2H2O | |
|---|---|---|---|---|---|---|
| formula | C34H39Cl2N8O2PRu | C37H36Cl2N8O0.5PRu | C32H35Cl4N8O2PRu | C33H30Cl2N7OPRu | C34H42Cl2N6O5P2Ru | C35H40Cl2N7O2PRu |
| FW | 794.67 | 803.68 | 837.52 | 743.58 | 848.64 | 793.68 |
| T, K | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) |
| λ, Å | 0.71073 | 0.71073 | 0.71073 | 0.71073 | 0.71073 | 0.71073 |
| crystal system | triclinic | monoclinic | triclinic | triclinic | monoclinic | monoclinic |
| space group | P1̅ | P21/c | P1̅ | P1̅1̅ | C2/c | P21/c |
| a, Å | 10.1428(8) | 20.5145(12) | 9.7016(8) | 11.1525(4) | 41.370(8) | 17.110(2) |
| b, Å | 13.2743(11) | 20.6593(12) | 10.0588(8) | 12.4862(5) | 9.756(2) | 10.1025(13) |
| c, Å | 13.9235(11) | 19.0486(11) | 19.2103(16) | 14.7685(6) | 19.152(4) | 21.524(3) |
| α, deg | 72.776(2) | 90 | 97.728(2) | 87.2220(10) | 90 | 90 |
| β, deg | 77.299(2) | 100.126(2) | 103.181(3) | 73.5550(10) | 91.34(3) | 106.679(8) |
| γ, deg | 85.255(3) | 90 | 97.790(2) | 89.3910(10) | 90 | 90 |
| cell volume, Å3 | 1746.4(2) | 7947.3(8) | 1781.7(3) | 1970.09(13) | 7728(3) | 3564.1(8) |
| Z | 2 | 8 | 2 | 2 | 8 | 4 |
| Dc, g·cm–3 | 1.511 | 1.343 | 1.561 | 1.253 | 1.459 | 1.479 |
| μ, mm–1 | 0.692 | 0.607 | 0.828 | 0.606 | 0.674 | 0.677 |
| F(000) | 816 | 3288 | 852 | 756 | 2488 | 1632 |
| crystal size, mm | 0.16 × 0.13 × 0.10 | 0.22 × 0.16 × 0.14 | 0.22 × 0.18 × 0.15 | 0.18 × 0.15 × 0.12 | 0.24 × 0.21 × 0.18 | 0.18 × 0.13 × 0.10 |
| θ limits, deg | 1.5649–26.998 | 1.467–25.998 | 2.074–25.997 | 1.633–27.227 | 1.970–26.000 | 1.9759–26.998 |
| reflections collected | 32 233 | 142 792 | 29 925 | 27 297 | 54 659 | 72 769 |
| independent reflections | 75 857 [Rint = 0.0850] | 15 547 [Rint = 0.1422] | 6987 [Rint = 0.0724] | 8722 [Rint = 0.0465] | 7594 [Rint = 0.0553] | 7780 [Rint = 0.0673] |
| data/restraints/parameters | 7585/17/428 | 15 547/8/871 | 6987/39/445 | 8722/0/407 | 7594/130/473 | 7780/6/445 |
| goodness on fit on F2 a | 1.193 | 1.075 | 1.036 | 1.097 | 1.038 | 1.064 |
| R1 (I > 2σ(I))b | 0.0628 | 0.0799 | 0.0610 | 0.0486 | 0.0336 | 0.0308 |
| wR2 (all data)c | 0.1366 | 0.1881 | 0.1604 | 0.1053 | 0.0772 | 0.0767 |
| largest diff. peak and hole, e Å–3 | 1.972/–1.232 | 3.653/–1.407 | 3.443/–2.006 | 1.132/–0.668 | 1.028/–0.793 | 0.651/–0.568 |
a
Goodness on fit on F2 = [Σw(FO2 – FC2)2/(Nref – Nparam)]1/2, where w = 1/[σ2(FO2) + (aP)2 + bP], where P = (FO2 + 2FC2)/3; Nref = number of reflections used in the refinement; Nparam = number of refined parameters.
b
R1 = Σ||FO| – |FC||/Σ|FO|.
c
wR2 = [Σw(FO2 – FC2)2/Σw(FO2)2]1/2, where w = 1/[σ2(FO2) + (aP)2 + bP], where P = (FO2 + 2FC2)/3.