Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680602900X/gk2019sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680602900X/gk2019Isup2.hkl |
CCDC reference: 621318
Data collection: COLLECT (Hooft, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL (Sheldrick, 2001) and CIFTAB (Sheldrick, 1993).
[Ru(N3)2(C25H22P2)2]·0.42CH2Cl2 | F(000) = 4060 |
Mr = 989.17 | Dx = 1.436 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 36.8818 (7) Å | Cell parameters from 8316 reflections |
b = 11.2016 (2) Å | θ = 1–25° |
c = 22.3275 (4) Å | µ = 0.57 mm−1 |
β = 97.235 (2)° | T = 173 K |
V = 9150.8 (3) Å3 | Block, yellow |
Z = 8 | 0.45 × 0.40 × 0.40 mm |
Nonius KappaCCD diffractometer | 6115 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.067 |
Graphite monochromator | θmax = 25.0°, θmin = 5.7° |
φ and ω scans | h = −34→43 |
42989 measured reflections | k = −13→13 |
7920 independent reflections | l = −26→25 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.062 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.162 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0635P)2 + 73.832P] where P = (Fo2 + 2Fc2)/3 |
7920 reflections | (Δ/σ)max = 0.001 |
566 parameters | Δρmax = 1.45 e Å−3 |
91 restraints | Δρmin = −0.91 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ru1 | 0.868972 (12) | 0.03797 (4) | 0.564765 (18) | 0.03287 (16) | |
N2 | 0.83196 (15) | −0.1139 (5) | 0.5837 (2) | 0.0444 (9) | |
N3 | 0.83097 (18) | −0.1544 (6) | 0.6155 (4) | 0.0658 (12) | |
N4 | 0.8268 (3) | −0.2228 (8) | 0.6628 (4) | 0.103 (2) | |
N5 | 0.90359 (15) | −0.0252 (5) | 0.6472 (2) | 0.0444 (9) | |
N6 | 0.90693 (18) | −0.0087 (6) | 0.6834 (4) | 0.0658 (12) | |
N7 | 0.9143 (3) | 0.0173 (10) | 0.7421 (5) | 0.131 (3) | |
P8 | 0.91616 (4) | 0.14491 (12) | 0.53215 (6) | 0.0335 (3) | |
C9 | 0.91267 (15) | 0.2889 (5) | 0.4922 (3) | 0.0369 (13) | |
C10 | 0.92532 (16) | 0.3037 (5) | 0.4367 (3) | 0.0404 (14) | |
H10 | 0.9364 | 0.2388 | 0.4184 | 0.048* | |
C11 | 0.92172 (18) | 0.4150 (6) | 0.4079 (3) | 0.0488 (16) | |
H11 | 0.9300 | 0.4249 | 0.3696 | 0.059* | |
C12 | 0.90634 (19) | 0.5093 (6) | 0.4343 (3) | 0.0534 (18) | |
H12 | 0.9045 | 0.5847 | 0.4147 | 0.064* | |
C13 | 0.89360 (18) | 0.4953 (6) | 0.4890 (3) | 0.0501 (16) | |
H13 | 0.8824 | 0.5605 | 0.5068 | 0.060* | |
C14 | 0.89707 (16) | 0.3861 (5) | 0.5181 (3) | 0.0405 (14) | |
H14 | 0.8887 | 0.3774 | 0.5564 | 0.049* | |
C15 | 0.95843 (16) | 0.1602 (5) | 0.5841 (2) | 0.0387 (13) | |
C16 | 0.97004 (17) | 0.2707 (6) | 0.6080 (3) | 0.0436 (14) | |
H16 | 0.9571 | 0.3410 | 0.5945 | 0.052* | |
C17 | 1.00055 (18) | 0.2787 (6) | 0.6515 (3) | 0.0531 (17) | |
H17 | 1.0083 | 0.3546 | 0.6670 | 0.064* | |
C18 | 1.01938 (18) | 0.1789 (7) | 0.6720 (3) | 0.0532 (17) | |
H18 | 1.0398 | 0.1851 | 0.7024 | 0.064* | |
C19 | 1.00849 (18) | 0.0678 (6) | 0.6481 (3) | 0.0514 (16) | |
H19 | 1.0218 | −0.0017 | 0.6617 | 0.062* | |
C20 | 0.97841 (17) | 0.0581 (6) | 0.6045 (3) | 0.0439 (14) | |
H20 | 0.9713 | −0.0179 | 0.5882 | 0.053* | |
C21 | 0.92712 (16) | 0.0344 (5) | 0.4761 (2) | 0.0365 (13) | |
H21A | 0.9534 | 0.0137 | 0.4805 | 0.044* | |
H21B | 0.9188 | 0.0595 | 0.4341 | 0.044* | |
P22 | 0.89870 (4) | −0.08648 (13) | 0.50193 (6) | 0.0334 (3) | |
C23 | 0.93031 (16) | −0.2035 (5) | 0.5315 (2) | 0.0375 (13) | |
C24 | 0.92452 (18) | −0.2648 (5) | 0.5836 (3) | 0.0428 (14) | |
H24 | 0.9045 | −0.2444 | 0.6046 | 0.051* | |
C25 | 0.94823 (19) | −0.3564 (6) | 0.6047 (3) | 0.0515 (17) | |
H25 | 0.9445 | −0.3974 | 0.6406 | 0.062* | |
C26 | 0.97691 (18) | −0.3885 (6) | 0.5746 (3) | 0.0493 (16) | |
H26 | 0.9929 | −0.4510 | 0.5898 | 0.059* | |
C27 | 0.98260 (17) | −0.3301 (6) | 0.5221 (3) | 0.0471 (15) | |
H27 | 1.0021 | −0.3535 | 0.5007 | 0.056* | |
C28 | 0.95960 (16) | −0.2371 (5) | 0.5008 (3) | 0.0418 (14) | |
H28 | 0.9638 | −0.1959 | 0.4651 | 0.050* | |
C29 | 0.87537 (16) | −0.1589 (5) | 0.4343 (2) | 0.0362 (13) | |
C30 | 0.89093 (18) | −0.1638 (6) | 0.3810 (3) | 0.0460 (15) | |
H30 | 0.9148 | −0.1331 | 0.3798 | 0.055* | |
C31 | 0.8718 (2) | −0.2133 (6) | 0.3292 (3) | 0.0534 (17) | |
H31 | 0.8825 | −0.2153 | 0.2926 | 0.064* | |
C32 | 0.8373 (2) | −0.2597 (6) | 0.3313 (3) | 0.0565 (18) | |
H32 | 0.8242 | −0.2937 | 0.2961 | 0.068* | |
C33 | 0.8219 (2) | −0.2568 (6) | 0.3841 (3) | 0.0543 (17) | |
H33 | 0.7982 | −0.2895 | 0.3853 | 0.065* | |
C34 | 0.84067 (18) | −0.2061 (5) | 0.4363 (3) | 0.0442 (15) | |
H34 | 0.8298 | −0.2039 | 0.4727 | 0.053* | |
P35 | 0.83974 (4) | 0.18708 (14) | 0.61468 (6) | 0.0387 (4) | |
C36 | 0.86325 (18) | 0.3138 (6) | 0.6535 (3) | 0.0456 (15) | |
C37 | 0.89788 (18) | 0.2976 (6) | 0.6848 (3) | 0.0491 (16) | |
H37 | 0.9096 | 0.2221 | 0.6848 | 0.059* | |
C38 | 0.9152 (2) | 0.3936 (8) | 0.7161 (3) | 0.064 (2) | |
H38 | 0.9388 | 0.3832 | 0.7381 | 0.076* | |
C39 | 0.8983 (3) | 0.5040 (8) | 0.7154 (4) | 0.074 (2) | |
H39 | 0.9102 | 0.5688 | 0.7372 | 0.089* | |
C40 | 0.8646 (3) | 0.5201 (8) | 0.6834 (4) | 0.078 (2) | |
H40 | 0.8533 | 0.5964 | 0.6822 | 0.093* | |
C41 | 0.8471 (2) | 0.4256 (7) | 0.6531 (3) | 0.064 (2) | |
H41 | 0.8235 | 0.4370 | 0.6315 | 0.077* | |
C42 | 0.80634 (16) | 0.1529 (6) | 0.6657 (2) | 0.0420 (14) | |
C43 | 0.81110 (18) | 0.0537 (6) | 0.7023 (3) | 0.0465 (15) | |
H43 | 0.8315 | 0.0029 | 0.7003 | 0.056* | |
C44 | 0.7861 (2) | 0.0276 (7) | 0.7422 (3) | 0.0625 (19) | |
H44 | 0.7896 | −0.0409 | 0.7673 | 0.075* | |
C45 | 0.7563 (2) | 0.1002 (9) | 0.7454 (3) | 0.070 (2) | |
H45 | 0.7389 | 0.0807 | 0.7717 | 0.084* | |
C46 | 0.75198 (19) | 0.2020 (8) | 0.7100 (3) | 0.067 (2) | |
H46 | 0.7320 | 0.2539 | 0.7132 | 0.080* | |
C47 | 0.77629 (18) | 0.2284 (7) | 0.6704 (3) | 0.0564 (18) | |
H47 | 0.7729 | 0.2979 | 0.6460 | 0.068* | |
C48 | 0.81337 (17) | 0.2476 (5) | 0.5451 (2) | 0.0405 (14) | |
H48A | 0.8231 | 0.3249 | 0.5326 | 0.049* | |
H48B | 0.7869 | 0.2546 | 0.5483 | 0.049* | |
P49 | 0.82406 (4) | 0.12182 (13) | 0.49612 (6) | 0.0343 (3) | |
C50 | 0.78078 (16) | 0.0405 (5) | 0.4795 (2) | 0.0372 (13) | |
C51 | 0.75941 (18) | 0.0201 (6) | 0.5262 (3) | 0.0462 (15) | |
H51 | 0.7665 | 0.0537 | 0.5649 | 0.055* | |
C52 | 0.72825 (19) | −0.0483 (6) | 0.5161 (3) | 0.0521 (16) | |
H52 | 0.7138 | −0.0600 | 0.5479 | 0.063* | |
C53 | 0.71782 (18) | −0.0999 (6) | 0.4610 (3) | 0.0534 (17) | |
H53 | 0.6966 | −0.1486 | 0.4547 | 0.064* | |
C54 | 0.73845 (18) | −0.0802 (6) | 0.4148 (3) | 0.0538 (17) | |
H54 | 0.7313 | −0.1157 | 0.3765 | 0.065* | |
C55 | 0.76943 (17) | −0.0096 (6) | 0.4232 (3) | 0.0448 (15) | |
H55 | 0.7830 | 0.0048 | 0.3905 | 0.054* | |
C56 | 0.83151 (15) | 0.1878 (5) | 0.4235 (2) | 0.0360 (13) | |
C57 | 0.82442 (17) | 0.3078 (5) | 0.4101 (3) | 0.0430 (14) | |
H57 | 0.8140 | 0.3568 | 0.4381 | 0.052* | |
C58 | 0.83232 (19) | 0.3554 (6) | 0.3569 (3) | 0.0544 (17) | |
H58 | 0.8277 | 0.4375 | 0.3485 | 0.065* | |
C59 | 0.84702 (19) | 0.2851 (7) | 0.3154 (3) | 0.0552 (18) | |
H59 | 0.8527 | 0.3192 | 0.2788 | 0.066* | |
C60 | 0.85357 (17) | 0.1646 (7) | 0.3269 (3) | 0.0497 (16) | |
H60 | 0.8633 | 0.1155 | 0.2980 | 0.060* | |
C61 | 0.84570 (16) | 0.1171 (6) | 0.3813 (2) | 0.0391 (13) | |
H61 | 0.8501 | 0.0348 | 0.3897 | 0.047* | |
C62 | 0.9988 (17) | 0.7316 (14) | 0.755 (4) | 0.126 (4) | 0.417 (7) |
H62A | 1.0045 | 0.7655 | 0.7960 | 0.151* | 0.417 (7) |
H62B | 0.9761 | 0.7690 | 0.7350 | 0.151* | 0.417 (7) |
Cl63 | 0.9939 (3) | 0.5799 (6) | 0.7582 (5) | 0.126 (3) | 0.417 (7) |
Cl64 | 1.03435 (16) | 0.7548 (5) | 0.7137 (2) | 0.087 (2) | 0.417 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0435 (3) | 0.0312 (3) | 0.0231 (2) | −0.0034 (2) | 0.00088 (18) | −0.00104 (18) |
N2 | 0.045 (2) | 0.052 (2) | 0.036 (2) | −0.0156 (17) | 0.0027 (17) | −0.0104 (17) |
N3 | 0.062 (2) | 0.046 (2) | 0.084 (3) | 0.0059 (19) | −0.011 (2) | −0.008 (2) |
N4 | 0.137 (6) | 0.084 (5) | 0.085 (5) | −0.011 (5) | 0.005 (4) | 0.015 (4) |
N5 | 0.045 (2) | 0.052 (2) | 0.036 (2) | −0.0156 (17) | 0.0027 (17) | −0.0104 (17) |
N6 | 0.062 (2) | 0.046 (2) | 0.084 (3) | 0.0059 (19) | −0.011 (2) | −0.008 (2) |
N7 | 0.155 (7) | 0.130 (6) | 0.101 (5) | 0.011 (6) | −0.016 (5) | −0.013 (5) |
P8 | 0.0415 (8) | 0.0264 (7) | 0.0313 (7) | −0.0016 (6) | −0.0001 (6) | −0.0002 (6) |
C9 | 0.036 (3) | 0.032 (3) | 0.040 (3) | −0.003 (2) | −0.006 (2) | 0.001 (2) |
C10 | 0.042 (3) | 0.037 (3) | 0.041 (3) | −0.005 (3) | −0.002 (3) | 0.005 (3) |
C11 | 0.057 (4) | 0.046 (4) | 0.040 (3) | −0.006 (3) | −0.004 (3) | 0.012 (3) |
C12 | 0.068 (4) | 0.035 (4) | 0.050 (4) | −0.009 (3) | −0.018 (3) | 0.012 (3) |
C13 | 0.063 (4) | 0.032 (3) | 0.049 (4) | −0.002 (3) | −0.015 (3) | −0.005 (3) |
C14 | 0.048 (3) | 0.029 (3) | 0.041 (3) | −0.002 (3) | −0.006 (3) | −0.002 (2) |
C15 | 0.046 (3) | 0.038 (3) | 0.032 (3) | −0.002 (3) | 0.002 (3) | 0.002 (2) |
C16 | 0.052 (4) | 0.038 (3) | 0.040 (3) | 0.000 (3) | 0.000 (3) | −0.001 (3) |
C17 | 0.058 (4) | 0.052 (4) | 0.045 (4) | −0.003 (3) | −0.008 (3) | −0.009 (3) |
C18 | 0.047 (4) | 0.073 (5) | 0.037 (3) | 0.002 (3) | −0.005 (3) | −0.002 (3) |
C19 | 0.049 (4) | 0.052 (4) | 0.050 (4) | 0.009 (3) | −0.004 (3) | 0.008 (3) |
C20 | 0.047 (4) | 0.040 (4) | 0.043 (3) | 0.003 (3) | −0.002 (3) | 0.000 (3) |
C21 | 0.045 (3) | 0.031 (3) | 0.033 (3) | −0.001 (3) | 0.002 (2) | 0.001 (2) |
P22 | 0.0455 (8) | 0.0270 (7) | 0.0272 (7) | −0.0011 (6) | 0.0023 (6) | 0.0000 (6) |
C23 | 0.051 (3) | 0.027 (3) | 0.033 (3) | −0.002 (3) | −0.001 (3) | −0.002 (2) |
C24 | 0.057 (4) | 0.037 (3) | 0.034 (3) | −0.004 (3) | 0.002 (3) | 0.000 (3) |
C25 | 0.065 (4) | 0.042 (4) | 0.045 (4) | −0.001 (3) | −0.004 (3) | 0.016 (3) |
C26 | 0.053 (4) | 0.037 (4) | 0.053 (4) | 0.002 (3) | −0.010 (3) | 0.011 (3) |
C27 | 0.049 (4) | 0.040 (3) | 0.051 (4) | 0.001 (3) | 0.000 (3) | −0.001 (3) |
C28 | 0.050 (4) | 0.036 (3) | 0.039 (3) | −0.001 (3) | 0.005 (3) | 0.001 (3) |
C29 | 0.053 (4) | 0.026 (3) | 0.029 (3) | 0.002 (3) | 0.003 (3) | 0.002 (2) |
C30 | 0.056 (4) | 0.043 (4) | 0.038 (3) | 0.010 (3) | 0.004 (3) | −0.001 (3) |
C31 | 0.079 (5) | 0.050 (4) | 0.031 (3) | 0.015 (4) | 0.004 (3) | −0.008 (3) |
C32 | 0.086 (5) | 0.037 (4) | 0.042 (4) | 0.004 (3) | −0.013 (4) | −0.007 (3) |
C33 | 0.066 (4) | 0.048 (4) | 0.045 (4) | −0.013 (3) | −0.009 (3) | 0.003 (3) |
C34 | 0.061 (4) | 0.037 (3) | 0.033 (3) | −0.004 (3) | −0.002 (3) | 0.006 (3) |
P35 | 0.0461 (9) | 0.0420 (9) | 0.0269 (7) | 0.0008 (7) | 0.0003 (6) | −0.0070 (6) |
C36 | 0.055 (4) | 0.050 (4) | 0.033 (3) | −0.005 (3) | 0.010 (3) | −0.012 (3) |
C37 | 0.059 (4) | 0.054 (4) | 0.034 (3) | −0.017 (3) | 0.004 (3) | 0.000 (3) |
C38 | 0.068 (5) | 0.088 (6) | 0.034 (4) | −0.028 (4) | 0.003 (3) | −0.008 (4) |
C39 | 0.095 (6) | 0.076 (6) | 0.056 (5) | −0.032 (5) | 0.027 (5) | −0.038 (4) |
C40 | 0.088 (6) | 0.069 (5) | 0.077 (6) | −0.001 (5) | 0.015 (5) | −0.042 (5) |
C41 | 0.070 (5) | 0.057 (5) | 0.065 (5) | 0.002 (4) | 0.010 (4) | −0.032 (4) |
C42 | 0.043 (3) | 0.055 (4) | 0.027 (3) | 0.000 (3) | 0.001 (2) | −0.012 (3) |
C43 | 0.050 (4) | 0.060 (4) | 0.029 (3) | 0.002 (3) | 0.004 (3) | −0.004 (3) |
C44 | 0.066 (5) | 0.076 (5) | 0.046 (4) | −0.011 (4) | 0.010 (3) | 0.005 (4) |
C45 | 0.054 (5) | 0.109 (7) | 0.051 (4) | −0.013 (5) | 0.017 (4) | −0.014 (5) |
C46 | 0.045 (4) | 0.097 (6) | 0.060 (5) | 0.006 (4) | 0.011 (4) | −0.023 (5) |
C47 | 0.051 (4) | 0.069 (5) | 0.047 (4) | 0.004 (4) | 0.001 (3) | −0.007 (3) |
C48 | 0.051 (4) | 0.042 (3) | 0.028 (3) | 0.003 (3) | 0.000 (3) | −0.008 (2) |
P49 | 0.0412 (8) | 0.0354 (8) | 0.0255 (7) | −0.0025 (6) | 0.0009 (6) | −0.0022 (6) |
C50 | 0.044 (3) | 0.039 (3) | 0.028 (3) | −0.002 (3) | 0.001 (2) | 0.002 (2) |
C51 | 0.056 (4) | 0.047 (4) | 0.036 (3) | −0.003 (3) | 0.007 (3) | −0.001 (3) |
C52 | 0.061 (4) | 0.052 (4) | 0.045 (4) | −0.011 (3) | 0.016 (3) | 0.004 (3) |
C53 | 0.052 (4) | 0.057 (4) | 0.051 (4) | −0.021 (3) | 0.005 (3) | 0.001 (3) |
C54 | 0.058 (4) | 0.062 (4) | 0.040 (3) | −0.020 (3) | 0.000 (3) | −0.013 (3) |
C55 | 0.050 (4) | 0.051 (4) | 0.033 (3) | −0.007 (3) | 0.004 (3) | −0.006 (3) |
C56 | 0.037 (3) | 0.042 (3) | 0.027 (3) | −0.007 (3) | −0.005 (2) | 0.001 (2) |
C57 | 0.051 (4) | 0.040 (3) | 0.034 (3) | −0.001 (3) | −0.006 (3) | 0.000 (3) |
C58 | 0.073 (5) | 0.042 (4) | 0.043 (4) | −0.012 (3) | −0.012 (3) | 0.008 (3) |
C59 | 0.063 (4) | 0.066 (5) | 0.035 (3) | −0.024 (4) | −0.003 (3) | 0.014 (3) |
C60 | 0.050 (4) | 0.067 (5) | 0.032 (3) | −0.008 (3) | 0.003 (3) | −0.004 (3) |
C61 | 0.045 (3) | 0.044 (3) | 0.028 (3) | 0.000 (3) | 0.003 (2) | 0.000 (3) |
C62 | 0.125 (5) | 0.126 (4) | 0.125 (5) | −0.002 (3) | 0.017 (3) | 0.001 (3) |
Cl63 | 0.125 (4) | 0.126 (3) | 0.123 (4) | −0.007 (3) | 0.007 (3) | 0.006 (3) |
Cl64 | 0.108 (3) | 0.071 (3) | 0.080 (3) | 0.038 (2) | 0.004 (2) | 0.006 (2) |
Ru1—N2 | 2.254 (5) | C33—H33 | 0.9500 |
Ru1—N5 | 2.220 (6) | C33—C34 | 1.398 (8) |
Ru1—P8 | 2.3050 (15) | C34—H34 | 0.9500 |
Ru1—P22 | 2.3455 (15) | P35—C36 | 1.825 (6) |
Ru1—P35 | 2.3446 (16) | P35—C42 | 1.821 (6) |
Ru1—P49 | 2.3099 (15) | P35—C48 | 1.855 (6) |
N2—N3 | 0.847 (7) | C36—C37 | 1.388 (9) |
N3—N4 | 1.330 (10) | C36—C41 | 1.386 (10) |
N5—N6 | 0.823 (7) | C37—H37 | 0.9500 |
N6—N7 | 1.336 (11) | C37—C38 | 1.394 (9) |
P8—C9 | 1.840 (6) | C38—H38 | 0.9500 |
P8—C15 | 1.830 (6) | C38—C39 | 1.384 (12) |
P8—C21 | 1.842 (6) | C39—H39 | 0.9500 |
C9—C10 | 1.387 (8) | C39—C40 | 1.366 (12) |
C9—C14 | 1.392 (8) | C40—H40 | 0.9500 |
C10—H10 | 0.9500 | C40—C41 | 1.373 (10) |
C10—C11 | 1.402 (8) | C41—H41 | 0.9500 |
C11—H11 | 0.9500 | C42—C43 | 1.377 (9) |
C11—C12 | 1.368 (10) | C42—C47 | 1.409 (9) |
C12—H12 | 0.9500 | C43—H43 | 0.9500 |
C12—C13 | 1.372 (10) | C43—C44 | 1.390 (9) |
C13—H13 | 0.9500 | C44—H44 | 0.9500 |
C13—C14 | 1.384 (8) | C44—C45 | 1.377 (11) |
C14—H14 | 0.9500 | C45—H45 | 0.9500 |
C15—C16 | 1.394 (8) | C45—C46 | 1.385 (12) |
C15—C20 | 1.404 (8) | C46—H46 | 0.9500 |
C16—H16 | 0.9500 | C46—C47 | 1.368 (10) |
C16—C17 | 1.393 (8) | C47—H47 | 0.9500 |
C17—H17 | 0.9500 | C48—H48A | 0.9900 |
C17—C18 | 1.364 (9) | C48—H48B | 0.9900 |
C18—H18 | 0.9500 | C48—P49 | 1.856 (6) |
C18—C19 | 1.394 (10) | P49—C50 | 1.835 (6) |
C19—H19 | 0.9500 | P49—C56 | 1.834 (5) |
C19—C20 | 1.385 (8) | C50—C51 | 1.402 (8) |
C20—H20 | 0.9500 | C50—C55 | 1.392 (8) |
C21—H21A | 0.9900 | C51—H51 | 0.9500 |
C21—H21B | 0.9900 | C51—C52 | 1.376 (9) |
C21—P22 | 1.848 (6) | C52—H52 | 0.9500 |
P22—C23 | 1.821 (6) | C52—C53 | 1.371 (9) |
P22—C29 | 1.831 (6) | C53—H53 | 0.9500 |
C23—C24 | 1.391 (8) | C53—C54 | 1.374 (9) |
C23—C28 | 1.401 (8) | C54—H54 | 0.9500 |
C24—H24 | 0.9500 | C54—C55 | 1.383 (9) |
C24—C25 | 1.391 (9) | C55—H55 | 0.9500 |
C25—H25 | 0.9500 | C56—C57 | 1.395 (8) |
C25—C26 | 1.371 (9) | C56—C61 | 1.383 (8) |
C26—H26 | 0.9500 | C57—H57 | 0.9500 |
C26—C27 | 1.380 (9) | C57—C58 | 1.366 (9) |
C27—H27 | 0.9500 | C58—H58 | 0.9500 |
C27—C28 | 1.390 (8) | C58—C59 | 1.378 (10) |
C28—H28 | 0.9500 | C59—H59 | 0.9500 |
C29—C30 | 1.386 (8) | C59—C60 | 1.390 (10) |
C29—C34 | 1.391 (8) | C60—H60 | 0.9500 |
C30—H30 | 0.9500 | C60—C61 | 1.391 (8) |
C30—C31 | 1.391 (9) | C61—H61 | 0.9500 |
C31—H31 | 0.9500 | C62—H62A | 0.9900 |
C31—C32 | 1.382 (10) | C62—H62B | 0.9900 |
C32—H32 | 0.9500 | C62—Cl63 | 1.711 (13) |
C32—C33 | 1.372 (10) | C62—Cl64 | 1.715 (16) |
N2—Ru1—N5 | 84.41 (19) | C32—C33—H33 | 119.6 |
N2—Ru1—P8 | 161.90 (15) | C32—C33—C34 | 120.7 (7) |
N2—Ru1—P22 | 90.18 (14) | H33—C33—C34 | 119.6 |
N2—Ru1—P35 | 97.07 (15) | C29—C34—C33 | 119.2 (6) |
N2—Ru1—P49 | 91.76 (16) | C29—C34—H34 | 120.4 |
N5—Ru1—P8 | 92.83 (14) | C33—C34—H34 | 120.4 |
N5—Ru1—P22 | 92.48 (15) | Ru1—P35—C36 | 124.1 (2) |
N5—Ru1—P35 | 94.81 (15) | Ru1—P35—C42 | 122.4 (2) |
N5—Ru1—P49 | 165.79 (15) | Ru1—P35—C48 | 94.94 (18) |
P8—Ru1—P22 | 72.03 (5) | C36—P35—C42 | 100.6 (3) |
P8—Ru1—P35 | 100.99 (6) | C36—P35—C48 | 106.4 (3) |
P8—Ru1—P49 | 94.93 (5) | C42—P35—C48 | 106.1 (3) |
P22—Ru1—P35 | 170.18 (5) | P35—C36—C37 | 119.3 (5) |
P22—Ru1—P49 | 101.24 (5) | P35—C36—C41 | 121.4 (5) |
P35—Ru1—P49 | 72.03 (5) | C37—C36—C41 | 119.3 (6) |
Ru1—N2—N3 | 130.7 (7) | C36—C37—H37 | 120.5 |
N2—N3—N4 | 174.9 (10) | C36—C37—C38 | 119.1 (7) |
Ru1—N5—N6 | 137.9 (8) | H37—C37—C38 | 120.5 |
N5—N6—N7 | 176.9 (11) | C37—C38—H38 | 119.8 |
Ru1—P8—C9 | 126.82 (19) | C37—C38—C39 | 120.4 (7) |
Ru1—P8—C15 | 117.71 (19) | H38—C38—C39 | 119.8 |
Ru1—P8—C21 | 95.99 (18) | C38—C39—H39 | 119.9 |
C9—P8—C15 | 103.1 (3) | C38—C39—C40 | 120.2 (7) |
C9—P8—C21 | 105.5 (3) | H39—C39—C40 | 119.9 |
C15—P8—C21 | 104.6 (3) | C39—C40—H40 | 120.1 |
P8—C9—C10 | 121.8 (4) | C39—C40—C41 | 119.8 (8) |
P8—C9—C14 | 119.4 (4) | H40—C40—C41 | 120.1 |
C10—C9—C14 | 118.8 (5) | C36—C41—C40 | 121.2 (8) |
C9—C10—H10 | 120.2 | C36—C41—H41 | 119.4 |
C9—C10—C11 | 119.6 (6) | C40—C41—H41 | 119.4 |
H10—C10—C11 | 120.2 | P35—C42—C43 | 119.7 (5) |
C10—C11—H11 | 119.7 | P35—C42—C47 | 121.4 (5) |
C10—C11—C12 | 120.6 (6) | C43—C42—C47 | 118.9 (6) |
H11—C11—C12 | 119.7 | C42—C43—H43 | 119.9 |
C11—C12—H12 | 119.9 | C42—C43—C44 | 120.3 (6) |
C11—C12—C13 | 120.2 (6) | H43—C43—C44 | 119.9 |
H12—C12—C13 | 119.9 | C43—C44—H44 | 119.8 |
C12—C13—H13 | 120.1 | C43—C44—C45 | 120.4 (7) |
C12—C13—C14 | 119.9 (6) | H44—C44—C45 | 119.8 |
H13—C13—C14 | 120.1 | C44—C45—H45 | 120.2 |
C9—C14—C13 | 121.0 (6) | C44—C45—C46 | 119.5 (7) |
C9—C14—H14 | 119.5 | H45—C45—C46 | 120.2 |
C13—C14—H14 | 119.5 | C45—C46—H46 | 119.7 |
P8—C15—C16 | 121.4 (4) | C45—C46—C47 | 120.6 (7) |
P8—C15—C20 | 120.0 (4) | H46—C46—C47 | 119.7 |
C16—C15—C20 | 118.4 (5) | C42—C47—C46 | 120.2 (7) |
C15—C16—H16 | 119.8 | C42—C47—H47 | 119.9 |
C15—C16—C17 | 120.4 (6) | C46—C47—H47 | 119.9 |
H16—C16—C17 | 119.8 | P35—C48—H48A | 112.7 |
C16—C17—H17 | 119.5 | P35—C48—H48B | 112.7 |
C16—C17—C18 | 120.9 (6) | P35—C48—P49 | 95.1 (3) |
H17—C17—C18 | 119.5 | H48A—C48—H48B | 110.2 |
C17—C18—H18 | 120.3 | H48A—C48—P49 | 112.7 |
C17—C18—C19 | 119.5 (6) | H48B—C48—P49 | 112.7 |
H18—C18—C19 | 120.3 | Ru1—P49—C48 | 96.06 (18) |
C18—C19—H19 | 119.8 | Ru1—P49—C50 | 117.71 (19) |
C18—C19—C20 | 120.4 (6) | Ru1—P49—C56 | 125.16 (19) |
H19—C19—C20 | 119.8 | C48—P49—C50 | 104.6 (3) |
C15—C20—C19 | 120.3 (6) | C48—P49—C56 | 106.4 (3) |
C15—C20—H20 | 119.8 | C50—P49—C56 | 104.2 (2) |
C19—C20—H20 | 119.8 | P49—C50—C51 | 119.1 (4) |
P8—C21—H21A | 112.6 | P49—C50—C55 | 122.5 (4) |
P8—C21—H21B | 112.6 | C51—C50—C55 | 118.2 (5) |
P8—C21—P22 | 95.7 (3) | C50—C51—H51 | 119.8 |
H21A—C21—H21B | 110.1 | C50—C51—C52 | 120.4 (6) |
H21A—C21—P22 | 112.6 | H51—C51—C52 | 119.8 |
H21B—C21—P22 | 112.6 | C51—C52—H52 | 119.5 |
Ru1—P22—C21 | 94.46 (18) | C51—C52—C53 | 121.0 (6) |
Ru1—P22—C23 | 122.48 (19) | H52—C52—C53 | 119.5 |
Ru1—P22—C29 | 123.4 (2) | C52—C53—H53 | 120.4 |
C21—P22—C23 | 106.1 (3) | C52—C53—C54 | 119.1 (6) |
C21—P22—C29 | 107.0 (3) | H53—C53—C54 | 120.4 |
C23—P22—C29 | 101.1 (3) | C53—C54—H54 | 119.4 |
P22—C23—C24 | 120.0 (5) | C53—C54—C55 | 121.1 (6) |
P22—C23—C28 | 120.9 (4) | H54—C54—C55 | 119.4 |
C24—C23—C28 | 119.0 (5) | C50—C55—C54 | 120.1 (6) |
C23—C24—H24 | 120.3 | C50—C55—H55 | 120.0 |
C23—C24—C25 | 119.5 (6) | C54—C55—H55 | 120.0 |
H24—C24—C25 | 120.3 | P49—C56—C57 | 122.2 (4) |
C24—C25—H25 | 119.4 | P49—C56—C61 | 118.9 (4) |
C24—C25—C26 | 121.2 (6) | C57—C56—C61 | 118.8 (5) |
H25—C25—C26 | 119.4 | C56—C57—H57 | 119.7 |
C25—C26—H26 | 120.0 | C56—C57—C58 | 120.5 (6) |
C25—C26—C27 | 120.0 (6) | H57—C57—C58 | 119.7 |
H26—C26—C27 | 120.0 | C57—C58—H58 | 119.8 |
C26—C27—H27 | 120.2 | C57—C58—C59 | 120.4 (6) |
C26—C27—C28 | 119.7 (6) | H58—C58—C59 | 119.8 |
H27—C27—C28 | 120.2 | C58—C59—H59 | 119.8 |
C23—C28—C27 | 120.6 (6) | C58—C59—C60 | 120.4 (6) |
C23—C28—H28 | 119.7 | H59—C59—C60 | 119.8 |
C27—C28—H28 | 119.7 | C59—C60—H60 | 120.6 |
P22—C29—C30 | 121.6 (5) | C59—C60—C61 | 118.8 (6) |
P22—C29—C34 | 118.7 (4) | H60—C60—C61 | 120.6 |
C30—C29—C34 | 119.7 (5) | C56—C61—C60 | 121.0 (6) |
C29—C30—H30 | 119.7 | C56—C61—H61 | 119.5 |
C29—C30—C31 | 120.5 (6) | C60—C61—H61 | 119.5 |
H30—C30—C31 | 119.7 | H62A—C62—H62B | 108.8 |
C30—C31—H31 | 120.2 | H62A—C62—Cl63 | 110.7 |
C30—C31—C32 | 119.6 (6) | H62A—C62—Cl64 | 110.7 |
H31—C31—C32 | 120.2 | H62B—C62—Cl63 | 110.7 |
C31—C32—H32 | 119.9 | H62B—C62—Cl64 | 110.7 |
C31—C32—C33 | 120.2 (6) | Cl63—C62—Cl64 | 105.3 (12) |
H32—C32—C33 | 119.9 | ||
N5—Ru1—N2—N3 | 17.1 (10) | C30—C31—C32—C33 | 0.1 (10) |
P8—Ru1—N2—N3 | 99.1 (10) | C31—C32—C33—C34 | 0.6 (10) |
P22—Ru1—N2—N3 | 109.6 (10) | P22—C29—C34—C33 | 177.1 (5) |
P35—Ru1—N2—N3 | −77.1 (10) | C30—C29—C34—C33 | −0.6 (9) |
P49—Ru1—N2—N3 | −149.2 (10) | C32—C33—C34—C29 | −0.3 (10) |
N2—Ru1—N5—N6 | −96.6 (11) | N2—Ru1—P35—C36 | 147.3 (3) |
P8—Ru1—N5—N6 | 101.3 (11) | N2—Ru1—P35—C42 | 13.5 (3) |
P22—Ru1—N5—N6 | 173.4 (11) | N2—Ru1—P35—C48 | −99.1 (3) |
P35—Ru1—N5—N6 | 0.0 (11) | N5—Ru1—P35—C36 | 62.4 (3) |
P49—Ru1—N5—N6 | −21.7 (15) | N5—Ru1—P35—C42 | −71.5 (3) |
N2—Ru1—P8—C9 | 135.0 (5) | N5—Ru1—P35—C48 | 176.0 (2) |
N2—Ru1—P8—C15 | −89.4 (5) | P8—Ru1—P35—C36 | −31.4 (3) |
N2—Ru1—P8—C21 | 20.5 (5) | P8—Ru1—P35—C42 | −165.3 (2) |
N5—Ru1—P8—C9 | −144.4 (3) | P8—Ru1—P35—C48 | 82.1 (2) |
N5—Ru1—P8—C15 | −8.8 (3) | P49—Ru1—P35—C36 | −123.1 (3) |
N5—Ru1—P8—C21 | 101.1 (2) | P49—Ru1—P35—C42 | 103.0 (2) |
P22—Ru1—P8—C9 | 123.9 (2) | P49—Ru1—P35—C48 | −9.5 (2) |
P22—Ru1—P8—C15 | −100.5 (2) | Ru1—P35—C36—C37 | −36.9 (6) |
P22—Ru1—P8—C21 | 9.44 (18) | Ru1—P35—C36—C41 | 144.0 (5) |
P35—Ru1—P8—C9 | −48.9 (2) | C42—P35—C36—C37 | 104.9 (5) |
P35—Ru1—P8—C15 | 86.7 (2) | C42—P35—C36—C41 | −74.3 (6) |
P35—Ru1—P8—C21 | −163.42 (18) | C48—P35—C36—C37 | −144.7 (5) |
P49—Ru1—P8—C9 | 23.7 (2) | C48—P35—C36—C41 | 36.1 (6) |
P49—Ru1—P8—C15 | 159.3 (2) | P35—C36—C37—C38 | −177.8 (5) |
P49—Ru1—P8—C21 | −90.79 (19) | C41—C36—C37—C38 | 1.4 (9) |
Ru1—P8—C9—C10 | −124.0 (4) | C36—C37—C38—C39 | −0.9 (10) |
Ru1—P8—C9—C14 | 56.3 (5) | C37—C38—C39—C40 | −0.6 (11) |
C15—P8—C9—C10 | 95.5 (5) | C38—C39—C40—C41 | 1.6 (13) |
C15—P8—C9—C14 | −84.2 (5) | C39—C40—C41—C36 | −1.0 (13) |
C21—P8—C9—C10 | −13.9 (5) | P35—C36—C41—C40 | 178.7 (6) |
C21—P8—C9—C14 | 166.3 (4) | C37—C36—C41—C40 | −0.5 (11) |
P8—C9—C10—C11 | 179.4 (4) | Ru1—P35—C42—C43 | 36.5 (5) |
C14—C9—C10—C11 | −0.8 (8) | Ru1—P35—C42—C47 | −145.9 (4) |
C9—C10—C11—C12 | 0.9 (9) | C36—P35—C42—C43 | −106.1 (5) |
C10—C11—C12—C13 | −1.3 (10) | C36—P35—C42—C47 | 71.4 (5) |
C11—C12—C13—C14 | 1.5 (9) | C48—P35—C42—C43 | 143.3 (5) |
C12—C13—C14—C9 | −1.4 (9) | C48—P35—C42—C47 | −39.2 (6) |
P8—C9—C14—C13 | −179.2 (4) | P35—C42—C43—C44 | 179.0 (5) |
C10—C9—C14—C13 | 1.1 (8) | C47—C42—C43—C44 | 1.4 (9) |
Ru1—P8—C15—C16 | −113.9 (5) | C42—C43—C44—C45 | 0.2 (10) |
Ru1—P8—C15—C20 | 61.1 (5) | C43—C44—C45—C46 | −2.1 (11) |
C9—P8—C15—C16 | 31.0 (6) | C44—C45—C46—C47 | 2.3 (11) |
C9—P8—C15—C20 | −154.1 (5) | C45—C46—C47—C42 | −0.8 (11) |
C21—P8—C15—C16 | 141.1 (5) | P35—C42—C47—C46 | −178.7 (5) |
C21—P8—C15—C20 | −43.9 (5) | C43—C42—C47—C46 | −1.1 (9) |
P8—C15—C16—C17 | 174.4 (5) | Ru1—P35—C48—P49 | 11.4 (2) |
C20—C15—C16—C17 | −0.7 (9) | C36—P35—C48—P49 | 139.1 (3) |
C15—C16—C17—C18 | −0.7 (10) | C42—P35—C48—P49 | −114.4 (3) |
C16—C17—C18—C19 | 1.6 (10) | P35—C48—P49—Ru1 | −11.5 (2) |
C17—C18—C19—C20 | −1.1 (10) | P35—C48—P49—C50 | 109.2 (3) |
C18—C19—C20—C15 | −0.3 (10) | P35—C48—P49—C56 | −140.9 (3) |
P8—C15—C20—C19 | −173.9 (5) | N2—Ru1—P49—C48 | 106.4 (2) |
C16—C15—C20—C19 | 1.2 (9) | N2—Ru1—P49—C50 | −3.6 (2) |
Ru1—P8—C21—P22 | −11.5 (2) | N2—Ru1—P49—C56 | −138.7 (3) |
C9—P8—C21—P22 | −142.4 (2) | N5—Ru1—P49—C48 | 32.4 (6) |
C15—P8—C21—P22 | 109.2 (3) | N5—Ru1—P49—C50 | −77.6 (6) |
P8—C21—P22—Ru1 | 11.2 (2) | N5—Ru1—P49—C56 | 147.3 (6) |
P8—C21—P22—C23 | −114.4 (3) | P8—Ru1—P49—C48 | −90.4 (2) |
P8—C21—P22—C29 | 138.2 (3) | P8—Ru1—P49—C50 | 159.6 (2) |
N2—Ru1—P22—C21 | 174.0 (2) | P8—Ru1—P49—C56 | 24.5 (2) |
N2—Ru1—P22—C23 | −73.6 (3) | P22—Ru1—P49—C48 | −163.1 (2) |
N2—Ru1—P22—C29 | 60.2 (3) | P22—Ru1—P49—C50 | 86.9 (2) |
N5—Ru1—P22—C21 | −101.6 (2) | P22—Ru1—P49—C56 | −48.1 (2) |
N5—Ru1—P22—C23 | 10.8 (3) | P35—Ru1—P49—C48 | 9.5 (2) |
N5—Ru1—P22—C29 | 144.7 (3) | P35—Ru1—P49—C50 | −100.5 (2) |
P8—Ru1—P22—C21 | −9.39 (18) | P35—Ru1—P49—C56 | 124.5 (2) |
P8—Ru1—P22—C23 | 102.9 (2) | Ru1—P49—C50—C51 | 62.1 (5) |
P8—Ru1—P22—C29 | −123.2 (2) | Ru1—P49—C50—C55 | −113.2 (5) |
P49—Ru1—P22—C21 | 82.19 (19) | C48—P49—C50—C51 | −43.0 (5) |
P49—Ru1—P22—C23 | −165.5 (2) | C48—P49—C50—C55 | 141.7 (5) |
P49—Ru1—P22—C29 | −31.6 (2) | C56—P49—C50—C51 | −154.5 (5) |
Ru1—P22—C23—C24 | 33.7 (5) | C56—P49—C50—C55 | 30.2 (6) |
Ru1—P22—C23—C28 | −149.4 (4) | P49—C50—C51—C52 | −175.1 (5) |
C21—P22—C23—C24 | 140.0 (5) | C55—C50—C51—C52 | 0.4 (9) |
C21—P22—C23—C28 | −43.2 (5) | C50—C51—C52—C53 | 1.3 (10) |
C29—P22—C23—C24 | −108.4 (5) | C51—C52—C53—C54 | −1.6 (11) |
C29—P22—C23—C28 | 68.4 (5) | C52—C53—C54—C55 | 0.0 (11) |
P22—C23—C24—C25 | 178.1 (5) | C53—C54—C55—C50 | 1.7 (11) |
C28—C23—C24—C25 | 1.2 (8) | P49—C50—C55—C54 | 173.4 (5) |
C23—C24—C25—C26 | −1.0 (9) | C51—C50—C55—C54 | −1.9 (9) |
C24—C25—C26—C27 | −0.3 (10) | Ru1—P49—C56—C57 | −118.2 (4) |
C25—C26—C27—C28 | 1.4 (10) | Ru1—P49—C56—C61 | 59.7 (5) |
C26—C27—C28—C23 | −1.2 (9) | C48—P49—C56—C57 | −8.2 (5) |
P22—C23—C28—C27 | −177.0 (5) | C48—P49—C56—C61 | 169.7 (4) |
C24—C23—C28—C27 | −0.1 (9) | C50—P49—C56—C57 | 102.0 (5) |
Ru1—P22—C29—C30 | 137.5 (4) | C50—P49—C56—C61 | −80.1 (5) |
Ru1—P22—C29—C34 | −40.2 (5) | P49—C56—C57—C58 | 176.1 (5) |
C21—P22—C29—C30 | 30.1 (5) | C61—C56—C57—C58 | −1.8 (9) |
C21—P22—C29—C34 | −147.6 (5) | C56—C57—C58—C59 | 0.8 (10) |
C23—P22—C29—C30 | −80.8 (5) | C57—C58—C59—C60 | 0.8 (10) |
C23—P22—C29—C34 | 101.5 (5) | C58—C59—C60—C61 | −1.2 (10) |
P22—C29—C30—C31 | −176.4 (5) | P49—C56—C61—C60 | −176.7 (4) |
C34—C29—C30—C31 | 1.3 (9) | C57—C56—C61—C60 | 1.3 (8) |
C29—C30—C31—C32 | −1.0 (9) | C59—C60—C61—C56 | 0.2 (9) |