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Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807045321/er2041sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536807045321/er2041Isup2.hkl |
CCDC reference: 648019
All synthetic procedures were carried out in the inert atmosphere of a glove box. The starting material - Cp*Ru(NO)OTf2 (OTf = OSO2CF3) – was prepared according to synthetic methods reported by Burns & Hubbard (1994). 2-Propanol (10 ml) was added with a syringe to Cp*Ru(NO)OTf2 (125 mg, 0.22 mmol) with a syringe. A color change from green to red/brown was observed immediately upon addition of 2-propanol to Cp*Ru(NO)OTf2. This color persisted throughout the reaction. The solution was stirred for ~2 h after which the deep red microcrystalline powder was collected by filtration. The product was washed with diethyl ether and dried, yielding 37 mg (.068 mmol, 62% yield). The structure was confirmed by 1H NMR and 13C NMR spectroscopy. Alternate routes entailing reductive elimination of Cp*Ru(NO)Cl2 or Cp*Ru(NO)Ph2 have been reported by Bergman & Chang (1987) and Hayton et al. (2002) Recrystallization was attempted in several solvents. The highest quality crystals (and ultimately, the crystal used for x-ray analysis) were obtained from CH2Cl2 solutions.
Support of the REU program CHE-0453206 by the national Science Foundation is gratefully acknowledged.
X-ray diffraction data on title compound were collected at 90 (1) K using a Bruker SMART APEX2 CCD diffractometer installed at a rotating anode source (Mo Kα radiation, λ =0.71073 Å), and equipped with an Oxford Cryosystems nitrogen gas-flow apparatus. The data were collected by the oscillation method with 0.5°frame-width (ω-scan) and a 15 sec exposure per frame. Four sets of data (360 frames in each set) were collected, nominally covering complete reciprocal space. The data were integrated, scaled, sorted and averaged using the APEX2 software package.
All crystals examined were twinned. The metric symmetry of the unit cell suggested a monoclinic C-centred cell. However the structure could be solved, with some difficulties, in the triclinic space group P 1 only (Direct Methods, SHELXTL Version 6.14). The twin law (0 - 1 0, -1 0 0, 0 0 - 1) was used during refinement. The volume ratios of the twins refined to 0.298 (1): 0.702 (1).
All non-hydrogen atoms were refined anisotropically. Positions of hydrogen atoms were calculated from the geometry of surrounding carbon atoms. The CH3 H atoms were treated as part of idealized CH3 groups with Uiso=1.5Ueq. For the carbon atoms C22, C31 and C35 isotropic restraints have been imposed to avoid non positive definite ADPs.
For related literature, see: Bergman & Chang (1987); Bernal et al. (1977); Bottomley (1983); Burns & Hubbard (1994); Hayton et al. (2002); Kubat-Martin et al. (1987).
Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL (Sheldrick, 2000).
![]() | Fig. 1. Molecular structure of title compound, hydrogen atoms are omitted for clarity. Displacement ellipsoids are drawn at the 50% probability level. |
[Ru2(C10H15)2(NO)2] | Z = 4 |
Mr = 532.60 | F(000) = 1072 |
Triclinic, P1 | Dx = 1.721 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.7181 (3) Å | Cell parameters from 7139 reflections |
b = 10.7364 (3) Å | θ = 3–28° |
c = 17.9238 (5) Å | µ = 1.49 mm−1 |
α = 89.209 (1)° | T = 90 K |
β = 89.220 (1)° | Parallelepiped, red |
γ = 85.373 (1)° | 0.3 × 0.2 × 0.13 mm |
V = 2055.48 (10) Å3 |
Bruker SMART APEXII diffractometer | 10102 independent reflections |
Radiation source: rotating anode | 9591 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 1.9° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Bruker 2004) | k = −14→14 |
Tmin = 0.705, Tmax = 0.824 | l = −23→23 |
29941 measured reflections |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.139 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (0.0465P)2 + 11.2766P] where P = (Fo2 + 2Fc2)/3 |
10102 reflections | (Δ/σ)max = 0.001 |
490 parameters | Δρmax = 2.12 e Å−3 |
18 restraints | Δρmin = −2.33 e Å−3 |
[Ru2(C10H15)2(NO)2] | γ = 85.373 (1)° |
Mr = 532.60 | V = 2055.48 (10) Å3 |
Triclinic, P1 | Z = 4 |
a = 10.7181 (3) Å | Mo Kα radiation |
b = 10.7364 (3) Å | µ = 1.49 mm−1 |
c = 17.9238 (5) Å | T = 90 K |
α = 89.209 (1)° | 0.3 × 0.2 × 0.13 mm |
β = 89.220 (1)° |
Bruker SMART APEXII diffractometer | 10102 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker 2004) | 9591 reflections with I > 2σ(I) |
Tmin = 0.705, Tmax = 0.824 | Rint = 0.040 |
29941 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 18 restraints |
wR(F2) = 0.139 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (0.0465P)2 + 11.2766P] where P = (Fo2 + 2Fc2)/3 |
10102 reflections | Δρmax = 2.12 e Å−3 |
490 parameters | Δρmin = −2.33 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 | ||
Ru1 | 0.83429 (5) | 0.25167 (5) | 0.55223 (3) | 0.01071 (12) | |
Ru2 | 0.69033 (5) | 0.26716 (5) | 0.44039 (3) | 0.01077 (12) | |
Ru3 | 0.74543 (5) | 0.83347 (5) | 1.05050 (3) | 0.01092 (12) | |
Ru4 | 0.75823 (6) | 0.69028 (6) | 0.93893 (3) | 0.01274 (13) | |
N1 | 0.8686 (5) | 0.2772 (5) | 0.4483 (3) | 0.0138 (10) | |
N2 | 0.6564 (5) | 0.2350 (5) | 0.5441 (3) | 0.0120 (10) | |
N3 | 0.7691 (5) | 0.8663 (5) | 0.9461 (3) | 0.0137 (10) | |
N4 | 0.7283 (6) | 0.6576 (6) | 1.0431 (3) | 0.0165 (11) | |
O1 | 0.9603 (5) | 0.2868 (5) | 0.4067 (3) | 0.0186 (10) | |
O2 | 0.5687 (5) | 0.2106 (5) | 0.5845 (3) | 0.0178 (10) | |
O3 | 0.7819 (5) | 0.9550 (5) | 0.9043 (3) | 0.0188 (10) | |
O4 | 0.7083 (6) | 0.5701 (5) | 1.0848 (3) | 0.0248 (11) | |
C1 | 1.0123 (6) | 0.3019 (6) | 0.6016 (3) | 0.0153 (12) | |
C2 | 0.9088 (6) | 0.3454 (6) | 0.6490 (3) | 0.0133 (12) | |
C3 | 0.8506 (6) | 0.2399 (7) | 0.6759 (3) | 0.0157 (13) | |
C4 | 0.9122 (7) | 0.1307 (6) | 0.6430 (3) | 0.0157 (13) | |
C5 | 1.0147 (6) | 0.1707 (7) | 0.5976 (3) | 0.0196 (14) | |
C6 | 1.1027 (7) | 0.3803 (7) | 0.5625 (4) | 0.0229 (14) | |
H6A | 1.1861 | 0.3628 | 0.5839 | 0.034* | |
H6B | 1.0753 | 0.4689 | 0.5688 | 0.034* | |
H6C | 1.1060 | 0.3606 | 0.5093 | 0.034* | |
C7 | 0.8771 (8) | 0.4764 (7) | 0.6728 (4) | 0.0242 (15) | |
H7A | 0.7871 | 0.4891 | 0.6836 | 0.036* | |
H7B | 0.8994 | 0.5339 | 0.6327 | 0.036* | |
H7C | 0.9240 | 0.4926 | 0.7177 | 0.036* | |
C8 | 0.7401 (7) | 0.2394 (7) | 0.7287 (4) | 0.0229 (14) | |
H8A | 0.7593 | 0.1790 | 0.7692 | 0.034* | |
H8B | 0.6669 | 0.2159 | 0.7017 | 0.034* | |
H8C | 0.7223 | 0.3229 | 0.7495 | 0.034* | |
C9 | 0.8799 (8) | −0.0006 (7) | 0.6564 (4) | 0.0271 (16) | |
H9A | 0.7887 | −0.0033 | 0.6564 | 0.041* | |
H9B | 0.9125 | −0.0305 | 0.7048 | 0.041* | |
H9C | 0.9172 | −0.0542 | 0.6169 | 0.041* | |
C10 | 1.1114 (7) | 0.0898 (7) | 0.5546 (4) | 0.0245 (15) | |
H10A | 1.1234 | 0.1266 | 0.5050 | 0.037* | |
H10B | 1.0828 | 0.0059 | 0.5496 | 0.037* | |
H10C | 1.1908 | 0.0843 | 0.5814 | 0.037* | |
C11 | 0.6615 (6) | 0.3406 (6) | 0.3248 (3) | 0.0133 (12) | |
C12 | 0.5575 (6) | 0.3859 (7) | 0.3712 (3) | 0.0165 (13) | |
C13 | 0.4952 (6) | 0.2823 (7) | 0.3977 (3) | 0.0193 (14) | |
C14 | 0.5631 (6) | 0.1703 (7) | 0.3703 (4) | 0.0177 (13) | |
C15 | 0.6642 (7) | 0.2080 (6) | 0.3252 (3) | 0.0176 (13) | |
C16 | 0.7511 (7) | 0.4163 (7) | 0.2847 (4) | 0.0208 (13) | |
H16A | 0.8368 | 0.3839 | 0.2962 | 0.031* | |
H16B | 0.7379 | 0.5035 | 0.3004 | 0.031* | |
H16C | 0.7379 | 0.4118 | 0.2308 | 0.031* | |
C17 | 0.5142 (7) | 0.5198 (7) | 0.3828 (4) | 0.0240 (15) | |
H17A | 0.4592 | 0.5493 | 0.3419 | 0.036* | |
H17B | 0.5867 | 0.5697 | 0.3837 | 0.036* | |
H17C | 0.4681 | 0.5283 | 0.4303 | 0.036* | |
C18 | 0.3795 (7) | 0.2856 (8) | 0.4461 (4) | 0.0272 (16) | |
H18A | 0.3560 | 0.3717 | 0.4612 | 0.041* | |
H18B | 0.3960 | 0.2330 | 0.4905 | 0.041* | |
H18C | 0.3110 | 0.2541 | 0.4180 | 0.041* | |
C19 | 0.5247 (7) | 0.0418 (7) | 0.3822 (4) | 0.0238 (14) | |
H19A | 0.4850 | 0.0355 | 0.4315 | 0.036* | |
H19B | 0.5986 | −0.0180 | 0.3793 | 0.036* | |
H19C | 0.4652 | 0.0231 | 0.3437 | 0.036* | |
C20 | 0.7578 (7) | 0.1247 (7) | 0.2829 (4) | 0.0227 (14) | |
H20A | 0.7445 | 0.1370 | 0.2292 | 0.034* | |
H20B | 0.7477 | 0.0374 | 0.2965 | 0.034* | |
H20C | 0.8425 | 0.1452 | 0.2951 | 0.034* | |
C21 | 0.6700 (6) | 1.0141 (6) | 1.0968 (3) | 0.0140 (12) | |
C22 | 0.6316 (6) | 0.9149 (7) | 1.1443 (3) | 0.0164 (13) | |
C23 | 0.7421 (7) | 0.8505 (7) | 1.1744 (3) | 0.0167 (13) | |
C24 | 0.8494 (7) | 0.9067 (7) | 1.1437 (3) | 0.0179 (13) | |
C25 | 0.8036 (6) | 1.0098 (6) | 1.0966 (3) | 0.0134 (12) | |
C26 | 0.5862 (7) | 1.1095 (7) | 1.0562 (4) | 0.0230 (15) | |
H26A | 0.5833 | 1.1891 | 1.0826 | 0.035* | |
H26B | 0.5017 | 1.0812 | 1.0541 | 0.035* | |
H26C | 0.6187 | 1.1209 | 1.0054 | 0.035* | |
C27 | 0.5004 (7) | 0.8876 (7) | 1.1648 (4) | 0.0250 (15) | |
H27A | 0.4784 | 0.9221 | 1.2140 | 0.038* | |
H27B | 0.4944 | 0.7970 | 1.1661 | 0.038* | |
H27C | 0.4425 | 0.9260 | 1.1276 | 0.038* | |
C28 | 0.7445 (8) | 0.7443 (7) | 1.2286 (4) | 0.0246 (15) | |
H28A | 0.8299 | 0.7261 | 1.2470 | 0.037* | |
H28B | 0.7173 | 0.6703 | 1.2040 | 0.037* | |
H28C | 0.6880 | 0.7664 | 1.2707 | 0.037* | |
C29 | 0.9852 (7) | 0.8728 (7) | 1.1631 (4) | 0.0227 (14) | |
H29A | 1.0022 | 0.9058 | 1.2123 | 0.034* | |
H29B | 1.0395 | 0.9089 | 1.1256 | 0.034* | |
H29C | 1.0017 | 0.7816 | 1.1639 | 0.034* | |
C30 | 0.8801 (6) | 1.0991 (7) | 1.0552 (4) | 0.0196 (13) | |
H30A | 0.9692 | 1.0736 | 1.0616 | 0.029* | |
H30B | 0.8614 | 1.1833 | 1.0749 | 0.029* | |
H30C | 0.8598 | 1.0989 | 1.0021 | 0.029* | |
C31 | 0.7173 (7) | 0.6749 (7) | 0.8191 (4) | 0.0205 (15) | |
C32 | 0.6613 (8) | 0.5753 (9) | 0.8593 (5) | 0.033 (2) | |
C33 | 0.7600 (9) | 0.4985 (8) | 0.8929 (4) | 0.0311 (19) | |
C34 | 0.8759 (7) | 0.5494 (7) | 0.8756 (4) | 0.0207 (14) | |
C35 | 0.8486 (6) | 0.6582 (6) | 0.8296 (3) | 0.0141 (12) | |
C36 | 0.6512 (9) | 0.7775 (10) | 0.7736 (4) | 0.042 (3) | |
H36A | 0.6766 | 0.8584 | 0.7898 | 0.064* | |
H36B | 0.5606 | 0.7753 | 0.7804 | 0.064* | |
H36C | 0.6733 | 0.7659 | 0.7207 | 0.064* | |
C37 | 0.5250 (11) | 0.5529 (14) | 0.8582 (7) | 0.073 (5) | |
H37A | 0.5099 | 0.4958 | 0.8177 | 0.110* | |
H37B | 0.4751 | 0.6324 | 0.8502 | 0.110* | |
H37C | 0.5008 | 0.5157 | 0.9060 | 0.110* | |
C38 | 0.7469 (14) | 0.3831 (9) | 0.9393 (5) | 0.066 (4) | |
H38A | 0.8107 | 0.3771 | 0.9782 | 0.100* | |
H38B | 0.7580 | 0.3094 | 0.9075 | 0.100* | |
H38C | 0.6635 | 0.3873 | 0.9626 | 0.100* | |
C39 | 1.0063 (9) | 0.4968 (9) | 0.8946 (4) | 0.040 (2) | |
H39A | 1.0023 | 0.4367 | 0.9361 | 0.060* | |
H39B | 1.0563 | 0.5648 | 0.9091 | 0.060* | |
H39C | 1.0451 | 0.4545 | 0.8510 | 0.060* | |
C40 | 0.9426 (7) | 0.7408 (7) | 0.7966 (4) | 0.0248 (15) | |
H40A | 0.9467 | 0.7307 | 0.7423 | 0.037* | |
H40B | 1.0251 | 0.7174 | 0.8178 | 0.037* | |
H40C | 0.9172 | 0.8282 | 0.8082 | 0.037* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0143 (3) | 0.0127 (2) | 0.0044 (2) | 0.00371 (17) | −0.00232 (18) | −0.00081 (18) |
Ru2 | 0.0137 (2) | 0.0132 (2) | 0.0047 (2) | 0.00386 (17) | −0.00250 (18) | −0.00123 (18) |
Ru3 | 0.0137 (2) | 0.0128 (3) | 0.0058 (2) | 0.00216 (17) | −0.00055 (18) | −0.00242 (19) |
Ru4 | 0.0167 (3) | 0.0142 (3) | 0.0073 (2) | −0.00047 (19) | 0.00158 (19) | −0.0039 (2) |
N1 | 0.017 (3) | 0.016 (3) | 0.008 (2) | 0.0050 (19) | −0.002 (2) | 0.000 (2) |
N2 | 0.013 (3) | 0.012 (3) | 0.011 (2) | 0.0018 (18) | −0.0028 (19) | −0.0030 (19) |
N3 | 0.015 (3) | 0.014 (3) | 0.011 (2) | 0.002 (2) | −0.002 (2) | −0.004 (2) |
N4 | 0.018 (3) | 0.018 (3) | 0.014 (3) | −0.004 (2) | 0.002 (2) | −0.003 (2) |
O1 | 0.021 (2) | 0.024 (3) | 0.011 (2) | −0.0013 (19) | 0.0020 (18) | −0.0005 (19) |
O2 | 0.017 (2) | 0.024 (3) | 0.011 (2) | 0.0000 (18) | 0.0014 (18) | 0.0019 (19) |
O3 | 0.034 (3) | 0.013 (2) | 0.009 (2) | 0.0006 (19) | −0.0011 (19) | 0.0024 (17) |
O4 | 0.041 (3) | 0.019 (3) | 0.016 (2) | −0.008 (2) | 0.008 (2) | 0.001 (2) |
C1 | 0.017 (3) | 0.021 (3) | 0.008 (3) | 0.000 (2) | −0.005 (2) | −0.005 (2) |
C2 | 0.017 (3) | 0.015 (3) | 0.007 (3) | 0.002 (2) | −0.001 (2) | −0.003 (2) |
C3 | 0.016 (3) | 0.027 (4) | 0.004 (3) | 0.000 (3) | 0.000 (2) | 0.002 (2) |
C4 | 0.024 (3) | 0.014 (3) | 0.010 (3) | −0.002 (2) | −0.010 (2) | 0.002 (2) |
C5 | 0.019 (3) | 0.029 (4) | 0.009 (3) | 0.012 (3) | −0.005 (2) | −0.002 (3) |
C6 | 0.023 (3) | 0.033 (4) | 0.012 (3) | 0.001 (3) | 0.001 (2) | −0.006 (3) |
C7 | 0.037 (4) | 0.023 (3) | 0.012 (3) | 0.005 (3) | 0.001 (3) | −0.010 (3) |
C8 | 0.025 (4) | 0.034 (4) | 0.009 (3) | −0.002 (3) | 0.002 (3) | 0.003 (3) |
C9 | 0.045 (5) | 0.020 (3) | 0.016 (3) | −0.004 (3) | −0.008 (3) | 0.005 (3) |
C10 | 0.027 (4) | 0.027 (4) | 0.018 (3) | 0.013 (3) | −0.004 (3) | −0.007 (3) |
C11 | 0.017 (3) | 0.017 (3) | 0.005 (2) | 0.003 (2) | −0.001 (2) | 0.000 (2) |
C12 | 0.017 (3) | 0.023 (3) | 0.008 (3) | 0.009 (2) | −0.004 (2) | −0.001 (2) |
C13 | 0.016 (3) | 0.034 (4) | 0.008 (3) | 0.004 (3) | −0.004 (2) | 0.001 (3) |
C14 | 0.019 (3) | 0.025 (3) | 0.009 (3) | −0.001 (2) | −0.007 (2) | 0.001 (2) |
C15 | 0.026 (3) | 0.019 (3) | 0.007 (3) | 0.007 (3) | −0.007 (2) | −0.007 (2) |
C16 | 0.027 (3) | 0.024 (3) | 0.011 (3) | 0.000 (3) | −0.001 (2) | 0.004 (3) |
C17 | 0.027 (4) | 0.023 (3) | 0.020 (3) | 0.011 (3) | −0.006 (3) | −0.004 (3) |
C18 | 0.022 (4) | 0.044 (5) | 0.015 (3) | 0.000 (3) | −0.002 (3) | 0.001 (3) |
C19 | 0.031 (4) | 0.022 (3) | 0.020 (3) | −0.009 (3) | −0.004 (3) | 0.004 (3) |
C20 | 0.030 (4) | 0.026 (3) | 0.010 (3) | 0.008 (3) | −0.001 (3) | −0.006 (3) |
C21 | 0.016 (3) | 0.016 (3) | 0.010 (3) | 0.003 (2) | −0.001 (2) | −0.006 (2) |
C22 | 0.019 (3) | 0.024 (3) | 0.006 (3) | 0.003 (2) | 0.004 (2) | −0.008 (2) |
C23 | 0.025 (3) | 0.018 (3) | 0.007 (3) | 0.000 (3) | 0.000 (2) | −0.007 (2) |
C24 | 0.028 (4) | 0.018 (3) | 0.008 (3) | 0.003 (3) | −0.005 (2) | −0.003 (2) |
C25 | 0.019 (3) | 0.015 (3) | 0.006 (2) | 0.001 (2) | 0.000 (2) | −0.002 (2) |
C26 | 0.020 (3) | 0.024 (4) | 0.023 (3) | 0.010 (3) | −0.005 (3) | −0.003 (3) |
C27 | 0.023 (3) | 0.034 (4) | 0.018 (3) | −0.003 (3) | 0.009 (3) | −0.006 (3) |
C28 | 0.041 (4) | 0.021 (4) | 0.012 (3) | −0.002 (3) | −0.002 (3) | −0.002 (3) |
C29 | 0.022 (3) | 0.026 (4) | 0.019 (3) | 0.006 (3) | −0.006 (3) | −0.001 (3) |
C30 | 0.025 (3) | 0.018 (3) | 0.016 (3) | −0.003 (2) | 0.000 (2) | −0.001 (2) |
C31 | 0.025 (3) | 0.026 (4) | 0.010 (3) | 0.004 (3) | −0.004 (2) | −0.013 (3) |
C32 | 0.027 (4) | 0.047 (5) | 0.026 (4) | −0.019 (4) | 0.012 (3) | −0.026 (4) |
C33 | 0.057 (6) | 0.021 (4) | 0.016 (3) | −0.011 (3) | 0.016 (3) | −0.010 (3) |
C34 | 0.034 (4) | 0.020 (3) | 0.006 (3) | 0.011 (3) | −0.003 (2) | −0.007 (2) |
C35 | 0.020 (3) | 0.017 (3) | 0.005 (2) | 0.002 (2) | 0.004 (2) | −0.006 (2) |
C36 | 0.045 (5) | 0.058 (6) | 0.019 (4) | 0.028 (4) | −0.021 (3) | −0.019 (4) |
C37 | 0.053 (7) | 0.105 (11) | 0.069 (8) | −0.040 (7) | 0.026 (6) | −0.070 (8) |
C38 | 0.153 (13) | 0.023 (5) | 0.026 (4) | −0.028 (6) | 0.039 (6) | −0.009 (4) |
C39 | 0.057 (6) | 0.040 (5) | 0.018 (3) | 0.033 (4) | −0.011 (3) | −0.010 (3) |
C40 | 0.035 (4) | 0.029 (4) | 0.011 (3) | −0.008 (3) | 0.011 (3) | −0.005 (3) |
Ru1—N1 | 1.915 (5) | C14—C19 | 1.483 (10) |
Ru1—N2 | 1.937 (5) | C15—C20 | 1.495 (9) |
Ru1—C4 | 2.199 (6) | C16—H16A | 0.9800 |
Ru1—C2 | 2.208 (6) | C16—H16B | 0.9800 |
Ru1—C5 | 2.215 (6) | C16—H16C | 0.9800 |
Ru1—C1 | 2.223 (6) | C17—H17A | 0.9800 |
Ru1—C3 | 2.227 (6) | C17—H17B | 0.9800 |
Ru1—Ru2 | 2.5418 (7) | C17—H17C | 0.9800 |
Ru2—N2 | 1.921 (5) | C18—H18A | 0.9800 |
Ru2—N1 | 1.929 (6) | C18—H18B | 0.9800 |
Ru2—C15 | 2.197 (6) | C18—H18C | 0.9800 |
Ru2—C14 | 2.199 (6) | C19—H19A | 0.9800 |
Ru2—C12 | 2.214 (6) | C19—H19B | 0.9800 |
Ru2—C11 | 2.224 (6) | C19—H19C | 0.9800 |
Ru2—C13 | 2.229 (7) | C20—H20A | 0.9800 |
Ru3—N3 | 1.917 (5) | C20—H20B | 0.9800 |
Ru3—N4 | 1.918 (6) | C20—H20C | 0.9800 |
Ru3—C21 | 2.208 (6) | C21—C25 | 1.429 (9) |
Ru3—C24 | 2.208 (6) | C21—C22 | 1.437 (10) |
Ru3—C22 | 2.212 (6) | C21—C26 | 1.494 (9) |
Ru3—C25 | 2.214 (6) | C22—C23 | 1.430 (10) |
Ru3—C23 | 2.230 (6) | C22—C27 | 1.500 (9) |
Ru3—Ru4 | 2.5347 (7) | C23—C24 | 1.441 (10) |
Ru4—N3 | 1.908 (6) | C23—C28 | 1.488 (10) |
Ru4—N4 | 1.923 (6) | C24—C25 | 1.442 (9) |
Ru4—C35 | 2.194 (6) | C24—C29 | 1.515 (9) |
Ru4—C34 | 2.206 (7) | C25—C30 | 1.493 (9) |
Ru4—C31 | 2.210 (6) | C26—H26A | 0.9800 |
Ru4—C32 | 2.222 (7) | C26—H26B | 0.9800 |
Ru4—C33 | 2.227 (8) | C26—H26C | 0.9800 |
N1—O1 | 1.235 (7) | C27—H27A | 0.9800 |
N2—O2 | 1.222 (7) | C27—H27B | 0.9800 |
N3—O3 | 1.219 (7) | C27—H27C | 0.9800 |
N4—O4 | 1.224 (8) | C28—H28A | 0.9800 |
C1—C5 | 1.409 (10) | C28—H28B | 0.9800 |
C1—C2 | 1.440 (9) | C28—H28C | 0.9800 |
C1—C6 | 1.495 (10) | C29—H29A | 0.9800 |
C2—C3 | 1.412 (9) | C29—H29B | 0.9800 |
C2—C7 | 1.486 (9) | C29—H29C | 0.9800 |
C3—C4 | 1.428 (10) | C30—H30A | 0.9800 |
C3—C8 | 1.506 (9) | C30—H30B | 0.9800 |
C4—C5 | 1.447 (10) | C30—H30C | 0.9800 |
C4—C9 | 1.495 (9) | C31—C35 | 1.419 (9) |
C5—C10 | 1.508 (9) | C31—C32 | 1.447 (12) |
C6—H6A | 0.9800 | C31—C36 | 1.498 (11) |
C6—H6B | 0.9800 | C32—C33 | 1.423 (14) |
C6—H6C | 0.9800 | C32—C37 | 1.500 (13) |
C7—H7A | 0.9800 | C33—C34 | 1.425 (12) |
C7—H7B | 0.9800 | C33—C38 | 1.498 (12) |
C7—H7C | 0.9800 | C34—C35 | 1.435 (9) |
C8—H8A | 0.9800 | C34—C39 | 1.506 (11) |
C8—H8B | 0.9800 | C35—C40 | 1.505 (9) |
C8—H8C | 0.9800 | C36—H36A | 0.9800 |
C9—H9A | 0.9800 | C36—H36B | 0.9800 |
C9—H9B | 0.9800 | C36—H36C | 0.9800 |
C9—H9C | 0.9800 | C37—H37A | 0.9800 |
C10—H10A | 0.9800 | C37—H37B | 0.9800 |
C10—H10B | 0.9800 | C37—H37C | 0.9800 |
C10—H10C | 0.9800 | C38—H38A | 0.9800 |
C11—C15 | 1.422 (9) | C38—H38B | 0.9800 |
C11—C12 | 1.439 (9) | C38—H38C | 0.9800 |
C11—C16 | 1.480 (9) | C39—H39A | 0.9800 |
C12—C13 | 1.416 (10) | C39—H39B | 0.9800 |
C12—C17 | 1.490 (9) | C39—H39C | 0.9800 |
C13—C14 | 1.443 (10) | C40—H40A | 0.9800 |
C13—C18 | 1.502 (10) | C40—H40B | 0.9800 |
C14—C15 | 1.425 (10) | C40—H40C | 0.9800 |
N1—Ru1—N2 | 97.3 (2) | H10A—C10—H10C | 109.5 |
N1—Ru1—C4 | 136.9 (3) | H10B—C10—H10C | 109.5 |
N2—Ru1—C4 | 110.0 (2) | C15—C11—C12 | 107.2 (6) |
N1—Ru1—C2 | 128.8 (2) | C15—C11—C16 | 125.7 (6) |
N2—Ru1—C2 | 120.6 (2) | C12—C11—C16 | 127.0 (6) |
C4—Ru1—C2 | 63.1 (2) | C15—C11—Ru2 | 70.2 (3) |
N1—Ru1—C5 | 104.3 (2) | C12—C11—Ru2 | 70.7 (3) |
N2—Ru1—C5 | 146.3 (3) | C16—C11—Ru2 | 123.6 (4) |
C4—Ru1—C5 | 38.3 (3) | C13—C12—C11 | 108.5 (6) |
C2—Ru1—C5 | 62.9 (2) | C13—C12—C17 | 125.5 (6) |
N1—Ru1—C1 | 100.8 (2) | C11—C12—C17 | 125.7 (7) |
N2—Ru1—C1 | 158.4 (2) | C13—C12—Ru2 | 72.0 (4) |
C4—Ru1—C1 | 63.0 (2) | C11—C12—Ru2 | 71.4 (3) |
C2—Ru1—C1 | 37.9 (2) | C17—C12—Ru2 | 127.5 (5) |
C5—Ru1—C1 | 37.0 (3) | C12—C13—C14 | 107.9 (6) |
N1—Ru1—C3 | 163.2 (2) | C12—C13—C18 | 127.0 (7) |
N2—Ru1—C3 | 99.1 (2) | C14—C13—C18 | 125.1 (7) |
C4—Ru1—C3 | 37.7 (2) | C12—C13—Ru2 | 70.8 (4) |
C2—Ru1—C3 | 37.1 (2) | C14—C13—Ru2 | 69.8 (4) |
C5—Ru1—C3 | 62.8 (2) | C18—C13—Ru2 | 124.6 (4) |
C1—Ru1—C3 | 62.4 (2) | C15—C14—C13 | 107.3 (6) |
N1—Ru1—Ru2 | 48.86 (17) | C15—C14—C19 | 127.6 (7) |
N2—Ru1—Ru2 | 48.52 (16) | C13—C14—C19 | 124.9 (7) |
C4—Ru1—Ru2 | 145.59 (17) | C15—C14—Ru2 | 71.0 (4) |
C2—Ru1—Ru2 | 147.60 (18) | C13—C14—Ru2 | 72.1 (4) |
C5—Ru1—Ru2 | 146.00 (17) | C19—C14—Ru2 | 126.5 (5) |
C1—Ru1—Ru2 | 147.30 (17) | C11—C15—C14 | 109.0 (6) |
C3—Ru1—Ru2 | 147.23 (17) | C11—C15—C20 | 124.2 (7) |
N2—Ru2—N1 | 97.4 (2) | C14—C15—C20 | 126.8 (7) |
N2—Ru2—C15 | 145.9 (3) | C11—C15—Ru2 | 72.3 (3) |
N1—Ru2—C15 | 104.4 (2) | C14—C15—Ru2 | 71.1 (4) |
N2—Ru2—C14 | 110.2 (2) | C20—C15—Ru2 | 123.8 (4) |
N1—Ru2—C14 | 137.1 (3) | C11—C16—H16A | 109.5 |
C15—Ru2—C14 | 37.8 (3) | C11—C16—H16B | 109.5 |
N2—Ru2—C12 | 121.4 (2) | H16A—C16—H16B | 109.5 |
N1—Ru2—C12 | 127.6 (3) | C11—C16—H16C | 109.5 |
C15—Ru2—C12 | 62.9 (2) | H16A—C16—H16C | 109.5 |
C14—Ru2—C12 | 63.2 (3) | H16B—C16—H16C | 109.5 |
N2—Ru2—C11 | 159.2 (2) | C12—C17—H17A | 109.5 |
N1—Ru2—C11 | 99.9 (2) | C12—C17—H17B | 109.5 |
C15—Ru2—C11 | 37.5 (2) | H17A—C17—H17B | 109.5 |
C14—Ru2—C11 | 63.2 (2) | C12—C17—H17C | 109.5 |
C12—Ru2—C11 | 37.8 (2) | H17A—C17—H17C | 109.5 |
N2—Ru2—C13 | 99.5 (2) | H17B—C17—H17C | 109.5 |
N1—Ru2—C13 | 162.6 (2) | C13—C18—H18A | 109.5 |
C15—Ru2—C13 | 62.9 (3) | C13—C18—H18B | 109.5 |
C14—Ru2—C13 | 38.0 (3) | H18A—C18—H18B | 109.5 |
C12—Ru2—C13 | 37.2 (3) | C13—C18—H18C | 109.5 |
C11—Ru2—C13 | 62.7 (2) | H18A—C18—H18C | 109.5 |
N2—Ru2—Ru1 | 49.06 (16) | H18B—C18—H18C | 109.5 |
N1—Ru2—Ru1 | 48.36 (15) | C14—C19—H19A | 109.5 |
C15—Ru2—Ru1 | 145.55 (17) | C14—C19—H19B | 109.5 |
C14—Ru2—Ru1 | 146.36 (18) | H19A—C19—H19B | 109.5 |
C12—Ru2—Ru1 | 147.44 (18) | C14—C19—H19C | 109.5 |
C11—Ru2—Ru1 | 145.97 (17) | H19A—C19—H19C | 109.5 |
C13—Ru2—Ru1 | 148.02 (17) | H19B—C19—H19C | 109.5 |
N3—Ru3—N4 | 97.1 (2) | C15—C20—H20A | 109.5 |
N3—Ru3—C21 | 104.8 (2) | C15—C20—H20B | 109.5 |
N4—Ru3—C21 | 147.1 (2) | H20A—C20—H20B | 109.5 |
N3—Ru3—C24 | 127.1 (3) | C15—C20—H20C | 109.5 |
N4—Ru3—C24 | 120.4 (3) | H20A—C20—H20C | 109.5 |
C21—Ru3—C24 | 63.5 (2) | H20B—C20—H20C | 109.5 |
N3—Ru3—C22 | 137.8 (3) | C25—C21—C22 | 108.4 (6) |
N4—Ru3—C22 | 111.1 (3) | C25—C21—C26 | 124.9 (6) |
C21—Ru3—C22 | 37.9 (2) | C22—C21—C26 | 126.6 (6) |
C24—Ru3—C22 | 63.6 (3) | C25—C21—Ru3 | 71.4 (4) |
N3—Ru3—C25 | 99.8 (2) | C22—C21—Ru3 | 71.2 (4) |
N4—Ru3—C25 | 158.4 (2) | C26—C21—Ru3 | 125.0 (4) |
C21—Ru3—C25 | 37.7 (2) | C23—C22—C21 | 107.7 (6) |
C24—Ru3—C25 | 38.1 (2) | C23—C22—C27 | 124.8 (7) |
C22—Ru3—C25 | 63.4 (2) | C21—C22—C27 | 127.3 (6) |
N3—Ru3—C23 | 162.8 (3) | C23—C22—Ru3 | 71.9 (4) |
N4—Ru3—C23 | 99.3 (3) | C21—C22—Ru3 | 70.9 (3) |
C21—Ru3—C23 | 62.9 (2) | C27—C22—Ru3 | 126.3 (5) |
C24—Ru3—C23 | 37.9 (3) | C22—C23—C24 | 108.4 (6) |
C22—Ru3—C23 | 37.6 (2) | C22—C23—C28 | 125.4 (7) |
C25—Ru3—C23 | 63.0 (2) | C24—C23—C28 | 126.2 (6) |
N3—Ru3—Ru4 | 48.36 (17) | C22—C23—Ru3 | 70.6 (3) |
N4—Ru3—Ru4 | 48.78 (17) | C24—C23—Ru3 | 70.3 (4) |
C21—Ru3—Ru4 | 146.67 (16) | C28—C23—Ru3 | 125.4 (5) |
C24—Ru3—Ru4 | 145.42 (19) | C23—C24—C25 | 107.4 (6) |
C22—Ru3—Ru4 | 147.66 (18) | C23—C24—C29 | 126.6 (6) |
C25—Ru3—Ru4 | 145.37 (16) | C25—C24—C29 | 125.8 (7) |
C23—Ru3—Ru4 | 147.50 (18) | C23—C24—Ru3 | 71.9 (4) |
N3—Ru4—N4 | 97.2 (2) | C25—C24—Ru3 | 71.2 (4) |
N3—Ru4—C35 | 99.6 (2) | C29—C24—Ru3 | 126.9 (5) |
N4—Ru4—C35 | 155.4 (3) | C21—C25—C24 | 108.0 (6) |
N3—Ru4—C34 | 130.1 (3) | C21—C25—C30 | 125.1 (6) |
N4—Ru4—C34 | 117.9 (3) | C24—C25—C30 | 126.9 (6) |
C35—Ru4—C34 | 38.1 (2) | C21—C25—Ru3 | 70.9 (4) |
N3—Ru4—C31 | 100.5 (3) | C24—C25—Ru3 | 70.8 (4) |
N4—Ru4—C31 | 153.2 (3) | C30—C25—Ru3 | 124.7 (4) |
C35—Ru4—C31 | 37.6 (2) | C21—C26—H26A | 109.5 |
C34—Ru4—C31 | 63.3 (2) | C21—C26—H26B | 109.5 |
N3—Ru4—C32 | 132.2 (3) | H26A—C26—H26B | 109.5 |
N4—Ru4—C32 | 116.2 (3) | C21—C26—H26C | 109.5 |
C35—Ru4—C32 | 63.2 (3) | H26A—C26—H26C | 109.5 |
C34—Ru4—C32 | 63.1 (3) | H26B—C26—H26C | 109.5 |
C31—Ru4—C32 | 38.1 (3) | C22—C27—H27A | 109.5 |
N3—Ru4—C33 | 161.7 (3) | C22—C27—H27B | 109.5 |
N4—Ru4—C33 | 101.0 (3) | H27A—C27—H27B | 109.5 |
C35—Ru4—C33 | 62.8 (3) | C22—C27—H27C | 109.5 |
C34—Ru4—C33 | 37.5 (3) | H27A—C27—H27C | 109.5 |
C31—Ru4—C33 | 62.9 (3) | H27B—C27—H27C | 109.5 |
C32—Ru4—C33 | 37.3 (4) | C23—C28—H28A | 109.5 |
N3—Ru4—Ru3 | 48.64 (16) | C23—C28—H28B | 109.5 |
N4—Ru4—Ru3 | 48.63 (18) | H28A—C28—H28B | 109.5 |
C35—Ru4—Ru3 | 143.66 (18) | C23—C28—H28C | 109.5 |
C34—Ru4—Ru3 | 145.77 (19) | H28A—C28—H28C | 109.5 |
C31—Ru4—Ru3 | 145.23 (19) | H28B—C28—H28C | 109.5 |
C32—Ru4—Ru3 | 148.8 (2) | C24—C29—H29A | 109.5 |
C33—Ru4—Ru3 | 149.5 (2) | C24—C29—H29B | 109.5 |
O1—N1—Ru1 | 138.4 (5) | H29A—C29—H29B | 109.5 |
O1—N1—Ru2 | 138.7 (4) | C24—C29—H29C | 109.5 |
Ru1—N1—Ru2 | 82.8 (2) | H29A—C29—H29C | 109.5 |
O2—N2—Ru2 | 139.1 (4) | H29B—C29—H29C | 109.5 |
O2—N2—Ru1 | 138.4 (4) | C25—C30—H30A | 109.5 |
Ru2—N2—Ru1 | 82.4 (2) | C25—C30—H30B | 109.5 |
O3—N3—Ru4 | 138.1 (4) | H30A—C30—H30B | 109.5 |
O3—N3—Ru3 | 138.9 (5) | C25—C30—H30C | 109.5 |
Ru4—N3—Ru3 | 83.0 (2) | H30A—C30—H30C | 109.5 |
O4—N4—Ru3 | 137.9 (5) | H30B—C30—H30C | 109.5 |
O4—N4—Ru4 | 139.5 (5) | C35—C31—C32 | 107.7 (7) |
Ru3—N4—Ru4 | 82.6 (2) | C35—C31—C36 | 125.2 (8) |
C5—C1—C2 | 108.3 (6) | C32—C31—C36 | 127.1 (8) |
C5—C1—C6 | 125.0 (6) | C35—C31—Ru4 | 70.6 (3) |
C2—C1—C6 | 126.8 (6) | C32—C31—Ru4 | 71.4 (4) |
C5—C1—Ru1 | 71.2 (4) | C36—C31—Ru4 | 123.9 (5) |
C2—C1—Ru1 | 70.5 (4) | C33—C32—C31 | 107.5 (7) |
C6—C1—Ru1 | 123.9 (4) | C33—C32—C37 | 127.4 (10) |
C3—C2—C1 | 107.9 (6) | C31—C32—C37 | 124.9 (10) |
C3—C2—C7 | 125.5 (6) | C33—C32—Ru4 | 71.6 (4) |
C1—C2—C7 | 126.2 (6) | C31—C32—Ru4 | 70.5 (4) |
C3—C2—Ru1 | 72.2 (4) | C37—C32—Ru4 | 127.8 (6) |
C1—C2—Ru1 | 71.6 (3) | C32—C33—C34 | 108.8 (7) |
C7—C2—Ru1 | 127.2 (5) | C32—C33—C38 | 126.6 (10) |
C2—C3—C4 | 108.5 (6) | C34—C33—C38 | 124.6 (10) |
C2—C3—C8 | 126.9 (6) | C32—C33—Ru4 | 71.1 (4) |
C4—C3—C8 | 124.5 (6) | C34—C33—Ru4 | 70.4 (4) |
C2—C3—Ru1 | 70.7 (3) | C38—C33—Ru4 | 124.2 (5) |
C4—C3—Ru1 | 70.1 (3) | C33—C34—C35 | 107.4 (7) |
C8—C3—Ru1 | 123.8 (4) | C33—C34—C39 | 128.4 (8) |
C3—C4—C5 | 107.3 (6) | C35—C34—C39 | 124.1 (8) |
C3—C4—C9 | 125.9 (7) | C33—C34—Ru4 | 72.1 (4) |
C5—C4—C9 | 126.8 (7) | C35—C34—Ru4 | 70.5 (4) |
C3—C4—Ru1 | 72.2 (3) | C39—C34—Ru4 | 126.8 (5) |
C5—C4—Ru1 | 71.5 (3) | C31—C35—C34 | 108.7 (6) |
C9—C4—Ru1 | 123.9 (4) | C31—C35—C40 | 125.2 (6) |
C1—C5—C4 | 107.9 (6) | C34—C35—C40 | 126.2 (7) |
C1—C5—C10 | 124.4 (7) | C31—C35—Ru4 | 71.8 (4) |
C4—C5—C10 | 127.7 (7) | C34—C35—Ru4 | 71.4 (4) |
C1—C5—Ru1 | 71.8 (4) | C40—C35—Ru4 | 123.4 (4) |
C4—C5—Ru1 | 70.2 (4) | C31—C36—H36A | 109.5 |
C10—C5—Ru1 | 125.0 (4) | C31—C36—H36B | 109.5 |
C1—C6—H6A | 109.5 | H36A—C36—H36B | 109.5 |
C1—C6—H6B | 109.5 | C31—C36—H36C | 109.5 |
H6A—C6—H6B | 109.5 | H36A—C36—H36C | 109.5 |
C1—C6—H6C | 109.5 | H36B—C36—H36C | 109.5 |
H6A—C6—H6C | 109.5 | C32—C37—H37A | 109.5 |
H6B—C6—H6C | 109.5 | C32—C37—H37B | 109.5 |
C2—C7—H7A | 109.5 | H37A—C37—H37B | 109.5 |
C2—C7—H7B | 109.5 | C32—C37—H37C | 109.5 |
H7A—C7—H7B | 109.5 | H37A—C37—H37C | 109.5 |
C2—C7—H7C | 109.5 | H37B—C37—H37C | 109.5 |
H7A—C7—H7C | 109.5 | C33—C38—H38A | 109.5 |
H7B—C7—H7C | 109.5 | C33—C38—H38B | 109.5 |
C3—C8—H8A | 109.5 | H38A—C38—H38B | 109.5 |
C3—C8—H8B | 109.5 | C33—C38—H38C | 109.5 |
H8A—C8—H8B | 109.5 | H38A—C38—H38C | 109.5 |
C3—C8—H8C | 109.5 | H38B—C38—H38C | 109.5 |
H8A—C8—H8C | 109.5 | C34—C39—H39A | 109.5 |
H8B—C8—H8C | 109.5 | C34—C39—H39B | 109.5 |
C4—C9—H9A | 109.5 | H39A—C39—H39B | 109.5 |
C4—C9—H9B | 109.5 | C34—C39—H39C | 109.5 |
H9A—C9—H9B | 109.5 | H39A—C39—H39C | 109.5 |
C4—C9—H9C | 109.5 | H39B—C39—H39C | 109.5 |
H9A—C9—H9C | 109.5 | C35—C40—H40A | 109.5 |
H9B—C9—H9C | 109.5 | C35—C40—H40B | 109.5 |
C5—C10—H10A | 109.5 | H40A—C40—H40B | 109.5 |
C5—C10—H10B | 109.5 | C35—C40—H40C | 109.5 |
H10A—C10—H10B | 109.5 | H40A—C40—H40C | 109.5 |
C5—C10—H10C | 109.5 | H40B—C40—H40C | 109.5 |
N1—Ru1—Ru2—N2 | 177.2 (3) | C14—Ru2—C12—C11 | −80.1 (4) |
C4—Ru1—Ru2—N2 | 61.1 (4) | C13—Ru2—C12—C11 | −117.5 (6) |
C2—Ru1—Ru2—N2 | −82.7 (4) | Ru1—Ru2—C12—C11 | 119.6 (4) |
C5—Ru1—Ru2—N2 | 132.4 (4) | N2—Ru2—C12—C17 | 60.4 (7) |
C1—Ru1—Ru2—N2 | −157.1 (4) | N1—Ru2—C12—C17 | −71.0 (7) |
C3—Ru1—Ru2—N2 | −10.2 (4) | C15—Ru2—C12—C17 | −158.6 (7) |
N2—Ru1—Ru2—N1 | −177.2 (3) | C14—Ru2—C12—C17 | 158.8 (7) |
C4—Ru1—Ru2—N1 | −116.1 (4) | C11—Ru2—C12—C17 | −121.2 (8) |
C2—Ru1—Ru2—N1 | 100.1 (4) | C13—Ru2—C12—C17 | 121.4 (8) |
C5—Ru1—Ru2—N1 | −44.8 (4) | Ru1—Ru2—C12—C17 | −1.6 (9) |
C1—Ru1—Ru2—N1 | 25.8 (4) | C11—C12—C13—C14 | 2.2 (7) |
C3—Ru1—Ru2—N1 | 172.6 (4) | C17—C12—C13—C14 | 176.1 (6) |
N1—Ru1—Ru2—C15 | 44.9 (4) | Ru2—C12—C13—C14 | −60.3 (4) |
N2—Ru1—Ru2—C15 | −132.3 (4) | C11—C12—C13—C18 | −178.1 (6) |
C4—Ru1—Ru2—C15 | −71.2 (5) | C17—C12—C13—C18 | −4.2 (11) |
C2—Ru1—Ru2—C15 | 145.0 (5) | Ru2—C12—C13—C18 | 119.4 (7) |
C5—Ru1—Ru2—C15 | 0.1 (5) | C11—C12—C13—Ru2 | 62.5 (4) |
C1—Ru1—Ru2—C15 | 70.6 (5) | C17—C12—C13—Ru2 | −123.6 (6) |
C3—Ru1—Ru2—C15 | −142.5 (5) | N2—Ru2—C13—C12 | 130.8 (4) |
N1—Ru1—Ru2—C14 | 115.7 (4) | N1—Ru2—C13—C12 | −34.3 (10) |
N2—Ru1—Ru2—C14 | −61.5 (4) | C15—Ru2—C13—C12 | −80.1 (4) |
C4—Ru1—Ru2—C14 | −0.5 (5) | C14—Ru2—C13—C12 | −118.3 (5) |
C2—Ru1—Ru2—C14 | −144.3 (5) | C11—Ru2—C13—C12 | −37.8 (4) |
C5—Ru1—Ru2—C14 | 70.9 (5) | Ru1—Ru2—C13—C12 | 121.4 (4) |
C1—Ru1—Ru2—C14 | 141.4 (5) | N2—Ru2—C13—C14 | −110.8 (4) |
C3—Ru1—Ru2—C14 | −71.8 (5) | N1—Ru2—C13—C14 | 84.0 (10) |
N1—Ru1—Ru2—C12 | −97.2 (4) | C15—Ru2—C13—C14 | 38.2 (4) |
N2—Ru1—Ru2—C12 | 85.6 (4) | C12—Ru2—C13—C14 | 118.3 (5) |
C4—Ru1—Ru2—C12 | 146.7 (5) | C11—Ru2—C13—C14 | 80.6 (4) |
C2—Ru1—Ru2—C12 | 2.9 (5) | Ru1—Ru2—C13—C14 | −120.2 (4) |
C5—Ru1—Ru2—C12 | −142.0 (5) | N2—Ru2—C13—C18 | 8.5 (7) |
C1—Ru1—Ru2—C12 | −71.5 (5) | N1—Ru2—C13—C18 | −156.6 (7) |
C3—Ru1—Ru2—C12 | 75.4 (5) | C15—Ru2—C13—C18 | 157.6 (8) |
N1—Ru1—Ru2—C11 | −24.8 (4) | C14—Ru2—C13—C18 | 119.4 (8) |
N2—Ru1—Ru2—C11 | 158.0 (4) | C12—Ru2—C13—C18 | −122.3 (8) |
C4—Ru1—Ru2—C11 | −140.9 (5) | C11—Ru2—C13—C18 | −160.1 (8) |
C2—Ru1—Ru2—C11 | 75.3 (4) | Ru1—Ru2—C13—C18 | −0.8 (9) |
C5—Ru1—Ru2—C11 | −69.6 (5) | C12—C13—C14—C15 | −1.8 (7) |
C1—Ru1—Ru2—C11 | 0.9 (4) | C18—C13—C14—C15 | 178.5 (6) |
C3—Ru1—Ru2—C11 | 147.8 (5) | Ru2—C13—C14—C15 | −62.7 (4) |
N1—Ru1—Ru2—C13 | −170.5 (4) | C12—C13—C14—C19 | −176.7 (6) |
N2—Ru1—Ru2—C13 | 12.3 (4) | C18—C13—C14—C19 | 3.6 (10) |
C4—Ru1—Ru2—C13 | 73.4 (5) | Ru2—C13—C14—C19 | 122.4 (6) |
C2—Ru1—Ru2—C13 | −70.4 (5) | C12—C13—C14—Ru2 | 60.9 (4) |
C5—Ru1—Ru2—C13 | 144.7 (5) | C18—C13—C14—Ru2 | −118.8 (6) |
C1—Ru1—Ru2—C13 | −144.8 (5) | N2—Ru2—C14—C15 | −164.5 (4) |
C3—Ru1—Ru2—C13 | 2.1 (5) | N1—Ru2—C14—C15 | −37.8 (5) |
N4—Ru3—Ru4—N3 | 177.4 (3) | C12—Ru2—C14—C15 | 79.6 (4) |
C21—Ru3—Ru4—N3 | 43.1 (4) | C11—Ru2—C14—C15 | 37.0 (4) |
C24—Ru3—Ru4—N3 | −97.6 (4) | C13—Ru2—C14—C15 | 116.2 (6) |
C22—Ru3—Ru4—N3 | 116.7 (4) | Ru1—Ru2—C14—C15 | −119.5 (4) |
C25—Ru3—Ru4—N3 | −27.6 (4) | N2—Ru2—C14—C13 | 79.3 (4) |
C23—Ru3—Ru4—N3 | −169.5 (4) | N1—Ru2—C14—C13 | −154.0 (4) |
N3—Ru3—Ru4—N4 | −177.4 (3) | C15—Ru2—C14—C13 | −116.2 (6) |
C21—Ru3—Ru4—N4 | −134.3 (4) | C12—Ru2—C14—C13 | −36.6 (4) |
C24—Ru3—Ru4—N4 | 85.0 (4) | C11—Ru2—C14—C13 | −79.2 (4) |
C22—Ru3—Ru4—N4 | −60.6 (4) | Ru1—Ru2—C14—C13 | 124.3 (4) |
C25—Ru3—Ru4—N4 | 155.1 (4) | N2—Ru2—C14—C19 | −41.4 (7) |
C23—Ru3—Ru4—N4 | 13.2 (4) | N1—Ru2—C14—C19 | 85.4 (7) |
N3—Ru3—Ru4—C35 | 34.7 (4) | C15—Ru2—C14—C19 | 123.2 (8) |
N4—Ru3—Ru4—C35 | −147.9 (4) | C12—Ru2—C14—C19 | −157.2 (7) |
C21—Ru3—Ru4—C35 | 77.8 (4) | C11—Ru2—C14—C19 | 160.2 (7) |
C24—Ru3—Ru4—C35 | −62.9 (4) | C13—Ru2—C14—C19 | −120.6 (8) |
C22—Ru3—Ru4—C35 | 151.4 (5) | Ru1—Ru2—C14—C19 | 3.7 (9) |
C25—Ru3—Ru4—C35 | 7.1 (4) | C12—C11—C15—C14 | 0.7 (7) |
C23—Ru3—Ru4—C35 | −134.8 (5) | C16—C11—C15—C14 | 179.8 (6) |
N3—Ru3—Ru4—C34 | 103.4 (4) | Ru2—C11—C15—C14 | 62.0 (4) |
N4—Ru3—Ru4—C34 | −79.3 (4) | C12—C11—C15—C20 | 179.3 (6) |
C21—Ru3—Ru4—C34 | 146.4 (5) | C16—C11—C15—C20 | −1.6 (10) |
C24—Ru3—Ru4—C34 | 5.8 (5) | Ru2—C11—C15—C20 | −119.3 (6) |
C22—Ru3—Ru4—C34 | −139.9 (5) | C12—C11—C15—Ru2 | −61.4 (4) |
C25—Ru3—Ru4—C34 | 75.8 (5) | C16—C11—C15—Ru2 | 117.7 (6) |
C23—Ru3—Ru4—C34 | −66.1 (5) | C13—C14—C15—C11 | 0.7 (7) |
N3—Ru3—Ru4—C31 | −32.5 (4) | C19—C14—C15—C11 | 175.4 (6) |
N4—Ru3—Ru4—C31 | 144.8 (4) | Ru2—C14—C15—C11 | −62.8 (4) |
C21—Ru3—Ru4—C31 | 10.5 (5) | C13—C14—C15—C20 | −177.9 (6) |
C24—Ru3—Ru4—C31 | −130.1 (5) | C19—C14—C15—C20 | −3.2 (11) |
C22—Ru3—Ru4—C31 | 84.2 (5) | Ru2—C14—C15—C20 | 118.7 (6) |
C25—Ru3—Ru4—C31 | −60.1 (5) | C13—C14—C15—Ru2 | 63.5 (4) |
C23—Ru3—Ru4—C31 | 158.0 (5) | C19—C14—C15—Ru2 | −121.9 (7) |
N3—Ru3—Ru4—C32 | −105.9 (6) | N2—Ru2—C15—C11 | 144.6 (4) |
N4—Ru3—Ru4—C32 | 71.4 (6) | N1—Ru2—C15—C11 | −87.5 (4) |
C21—Ru3—Ru4—C32 | −62.9 (6) | C14—Ru2—C15—C11 | 118.0 (6) |
C24—Ru3—Ru4—C32 | 156.5 (6) | C12—Ru2—C15—C11 | 37.7 (4) |
C22—Ru3—Ru4—C32 | 10.8 (6) | C13—Ru2—C15—C11 | 79.7 (4) |
C25—Ru3—Ru4—C32 | −133.5 (6) | Ru1—Ru2—C15—C11 | −120.5 (4) |
C23—Ru3—Ru4—C32 | 84.6 (6) | N2—Ru2—C15—C14 | 26.5 (6) |
N3—Ru3—Ru4—C33 | 176.9 (6) | N1—Ru2—C15—C14 | 154.5 (4) |
N4—Ru3—Ru4—C33 | −5.7 (6) | C12—Ru2—C15—C14 | −80.3 (4) |
C21—Ru3—Ru4—C33 | −140.0 (6) | C11—Ru2—C15—C14 | −118.0 (6) |
C24—Ru3—Ru4—C33 | 79.3 (6) | C13—Ru2—C15—C14 | −38.4 (4) |
C22—Ru3—Ru4—C33 | −66.4 (6) | Ru1—Ru2—C15—C14 | 121.5 (4) |
C25—Ru3—Ru4—C33 | 149.4 (6) | N2—Ru2—C15—C20 | −95.7 (7) |
C23—Ru3—Ru4—C33 | 7.4 (6) | N1—Ru2—C15—C20 | 32.3 (7) |
N2—Ru1—N1—O1 | −173.6 (7) | C14—Ru2—C15—C20 | −122.2 (8) |
C4—Ru1—N1—O1 | −43.7 (9) | C12—Ru2—C15—C20 | 157.5 (7) |
C2—Ru1—N1—O1 | 46.8 (8) | C11—Ru2—C15—C20 | 119.8 (8) |
C5—Ru1—N1—O1 | −19.8 (8) | C13—Ru2—C15—C20 | −160.6 (7) |
C1—Ru1—N1—O1 | 18.1 (8) | Ru1—Ru2—C15—C20 | −0.7 (9) |
C3—Ru1—N1—O1 | 18.3 (14) | N3—Ru3—C21—C25 | −86.9 (4) |
Ru2—Ru1—N1—O1 | −175.8 (9) | N4—Ru3—C21—C25 | 143.1 (4) |
N2—Ru1—N1—Ru2 | 2.1 (2) | C24—Ru3—C21—C25 | 37.5 (4) |
C4—Ru1—N1—Ru2 | 132.1 (3) | C22—Ru3—C21—C25 | 117.8 (5) |
C2—Ru1—N1—Ru2 | −137.4 (3) | C23—Ru3—C21—C25 | 80.2 (4) |
C5—Ru1—N1—Ru2 | 156.0 (2) | Ru4—Ru3—C21—C25 | −118.8 (3) |
C1—Ru1—N1—Ru2 | −166.2 (2) | N3—Ru3—C21—C22 | 155.2 (4) |
C3—Ru1—N1—Ru2 | −166.0 (8) | N4—Ru3—C21—C22 | 25.3 (6) |
N2—Ru2—N1—O1 | 173.6 (8) | C24—Ru3—C21—C22 | −80.3 (4) |
C15—Ru2—N1—O1 | 20.1 (8) | C25—Ru3—C21—C22 | −117.8 (5) |
C14—Ru2—N1—O1 | 42.9 (9) | C23—Ru3—C21—C22 | −37.7 (4) |
C12—Ru2—N1—O1 | −46.6 (8) | Ru4—Ru3—C21—C22 | 123.4 (4) |
C11—Ru2—N1—O1 | −18.1 (8) | N3—Ru3—C21—C26 | 33.2 (6) |
C13—Ru2—N1—O1 | −21.2 (14) | N4—Ru3—C21—C26 | −96.8 (7) |
Ru1—Ru2—N1—O1 | 175.7 (9) | C24—Ru3—C21—C26 | 157.6 (7) |
N2—Ru2—N1—Ru1 | −2.1 (2) | C22—Ru3—C21—C26 | −122.1 (7) |
C15—Ru2—N1—Ru1 | −155.7 (2) | C25—Ru3—C21—C26 | 120.1 (7) |
C14—Ru2—N1—Ru1 | −132.8 (3) | C23—Ru3—C21—C26 | −159.7 (7) |
C12—Ru2—N1—Ru1 | 137.6 (2) | Ru4—Ru3—C21—C26 | 1.3 (8) |
C11—Ru2—N1—Ru1 | 166.2 (2) | C25—C21—C22—C23 | 0.9 (7) |
C13—Ru2—N1—Ru1 | 163.1 (8) | C26—C21—C22—C23 | −177.0 (6) |
N1—Ru2—N2—O2 | −175.0 (7) | Ru3—C21—C22—C23 | 62.9 (4) |
C15—Ru2—N2—O2 | −45.3 (10) | C25—C21—C22—C27 | 176.4 (6) |
C14—Ru2—N2—O2 | −28.4 (8) | C26—C21—C22—C27 | −1.5 (10) |
C12—Ru2—N2—O2 | 41.9 (8) | Ru3—C21—C22—C27 | −121.6 (7) |
C11—Ru2—N2—O2 | 39.1 (11) | C25—C21—C22—Ru3 | −62.0 (4) |
C13—Ru2—N2—O2 | 9.5 (8) | C26—C21—C22—Ru3 | 120.1 (6) |
Ru1—Ru2—N2—O2 | −177.1 (8) | N3—Ru3—C22—C23 | −154.0 (4) |
N1—Ru2—N2—Ru1 | 2.1 (2) | N4—Ru3—C22—C23 | 77.5 (4) |
C15—Ru2—N2—Ru1 | 131.8 (4) | C21—Ru3—C22—C23 | −116.9 (6) |
C14—Ru2—N2—Ru1 | 148.7 (2) | C24—Ru3—C22—C23 | −36.9 (4) |
C12—Ru2—N2—Ru1 | −141.0 (2) | C25—Ru3—C22—C23 | −79.6 (4) |
C11—Ru2—N2—Ru1 | −143.8 (6) | Ru4—Ru3—C22—C23 | 122.2 (4) |
C13—Ru2—N2—Ru1 | −173.4 (2) | N3—Ru3—C22—C21 | −37.1 (5) |
N1—Ru1—N2—O2 | 175.0 (7) | N4—Ru3—C22—C21 | −165.6 (4) |
C4—Ru1—N2—O2 | 28.9 (8) | C24—Ru3—C22—C21 | 80.0 (4) |
C2—Ru1—N2—O2 | −41.0 (8) | C25—Ru3—C22—C21 | 37.2 (4) |
C5—Ru1—N2—O2 | 45.2 (9) | C23—Ru3—C22—C21 | 116.9 (6) |
C1—Ru1—N2—O2 | −37.8 (11) | Ru4—Ru3—C22—C21 | −121.0 (4) |
C3—Ru1—N2—O2 | −8.5 (7) | N3—Ru3—C22—C27 | 85.7 (7) |
Ru2—Ru1—N2—O2 | 177.1 (8) | N4—Ru3—C22—C27 | −42.8 (7) |
N1—Ru1—N2—Ru2 | −2.1 (2) | C21—Ru3—C22—C27 | 122.8 (8) |
C4—Ru1—N2—Ru2 | −148.2 (2) | C24—Ru3—C22—C27 | −157.3 (7) |
C2—Ru1—N2—Ru2 | 141.9 (2) | C25—Ru3—C22—C27 | 160.0 (7) |
C5—Ru1—N2—Ru2 | −132.0 (4) | C23—Ru3—C22—C27 | −120.4 (8) |
C1—Ru1—N2—Ru2 | 145.0 (6) | Ru4—Ru3—C22—C27 | 1.8 (9) |
C3—Ru1—N2—Ru2 | 174.4 (2) | C21—C22—C23—C24 | −1.9 (7) |
N4—Ru4—N3—O3 | −176.6 (7) | C27—C22—C23—C24 | −177.6 (6) |
C35—Ru4—N3—O3 | 21.4 (8) | Ru3—C22—C23—C24 | 60.3 (4) |
C34—Ru4—N3—O3 | 47.1 (8) | C21—C22—C23—C28 | 177.6 (6) |
C31—Ru4—N3—O3 | −16.8 (8) | C27—C22—C23—C28 | 1.9 (10) |
C32—Ru4—N3—O3 | −40.9 (9) | Ru3—C22—C23—C28 | −120.2 (6) |
C33—Ru4—N3—O3 | 6.4 (14) | C21—C22—C23—Ru3 | −62.2 (4) |
Ru3—Ru4—N3—O3 | −178.6 (8) | C27—C22—C23—Ru3 | 122.1 (6) |
N4—Ru4—N3—Ru3 | 2.0 (2) | N3—Ru3—C23—C22 | 84.9 (9) |
C35—Ru4—N3—Ru3 | −160.0 (2) | N4—Ru3—C23—C22 | −112.6 (4) |
C34—Ru4—N3—Ru3 | −134.3 (3) | C21—Ru3—C23—C22 | 38.1 (4) |
C31—Ru4—N3—Ru3 | 161.8 (2) | C24—Ru3—C23—C22 | 118.9 (6) |
C32—Ru4—N3—Ru3 | 137.7 (3) | C25—Ru3—C23—C22 | 80.6 (4) |
C33—Ru4—N3—Ru3 | −175.0 (9) | Ru4—Ru3—C23—C22 | −122.6 (4) |
N4—Ru3—N3—O3 | 176.6 (8) | N3—Ru3—C23—C24 | −34.0 (10) |
C21—Ru3—N3—O3 | 21.4 (8) | N4—Ru3—C23—C24 | 128.5 (4) |
C24—Ru3—N3—O3 | −46.3 (8) | C21—Ru3—C23—C24 | −80.8 (4) |
C22—Ru3—N3—O3 | 43.9 (9) | C22—Ru3—C23—C24 | −118.9 (6) |
C25—Ru3—N3—O3 | −16.9 (8) | C25—Ru3—C23—C24 | −38.3 (4) |
C23—Ru3—N3—O3 | −20.8 (14) | Ru4—Ru3—C23—C24 | 118.6 (4) |
Ru4—Ru3—N3—O3 | 178.6 (9) | N3—Ru3—C23—C28 | −155.0 (8) |
N4—Ru3—N3—Ru4 | −2.0 (2) | N4—Ru3—C23—C28 | 7.6 (7) |
C21—Ru3—N3—Ru4 | −157.2 (2) | C21—Ru3—C23—C28 | 158.2 (7) |
C24—Ru3—N3—Ru4 | 135.1 (3) | C24—Ru3—C23—C28 | −121.0 (8) |
C22—Ru3—N3—Ru4 | −134.6 (3) | C22—Ru3—C23—C28 | 120.1 (8) |
C25—Ru3—N3—Ru4 | 164.5 (2) | C25—Ru3—C23—C28 | −159.3 (7) |
C23—Ru3—N3—Ru4 | 160.6 (7) | Ru4—Ru3—C23—C28 | −2.4 (9) |
N3—Ru3—N4—O4 | −177.9 (8) | C22—C23—C24—C25 | 2.2 (7) |
C21—Ru3—N4—O4 | −46.2 (10) | C28—C23—C24—C25 | −177.3 (6) |
C24—Ru3—N4—O4 | 41.0 (9) | Ru3—C23—C24—C25 | 62.7 (4) |
C22—Ru3—N4—O4 | −29.9 (8) | C22—C23—C24—C29 | 176.5 (6) |
C25—Ru3—N4—O4 | 40.7 (12) | C28—C23—C24—C29 | −3.0 (11) |
C23—Ru3—N4—O4 | 7.2 (8) | Ru3—C23—C24—C29 | −123.0 (7) |
Ru4—Ru3—N4—O4 | −179.9 (9) | C22—C23—C24—Ru3 | −60.5 (4) |
N3—Ru3—N4—Ru4 | 2.0 (2) | C28—C23—C24—Ru3 | 120.0 (6) |
C21—Ru3—N4—Ru4 | 133.7 (4) | N3—Ru3—C24—C23 | 168.0 (4) |
C24—Ru3—N4—Ru4 | −139.1 (2) | N4—Ru3—C24—C23 | −63.4 (5) |
C22—Ru3—N4—Ru4 | 150.0 (2) | C21—Ru3—C24—C23 | 79.2 (4) |
C25—Ru3—N4—Ru4 | −139.4 (5) | C22—Ru3—C24—C23 | 36.6 (4) |
C23—Ru3—N4—Ru4 | −172.9 (2) | C25—Ru3—C24—C23 | 116.4 (6) |
N3—Ru4—N4—O4 | 177.9 (8) | Ru4—Ru3—C24—C23 | −123.7 (4) |
C35—Ru4—N4—O4 | −49.2 (11) | N3—Ru3—C24—C25 | 51.7 (5) |
C34—Ru4—N4—O4 | −38.8 (9) | N4—Ru3—C24—C25 | −179.8 (4) |
C31—Ru4—N4—O4 | 46.7 (11) | C21—Ru3—C24—C25 | −37.2 (4) |
C32—Ru4—N4—O4 | 33.1 (9) | C22—Ru3—C24—C25 | −79.8 (4) |
C33—Ru4—N4—O4 | −3.0 (9) | C23—Ru3—C24—C25 | −116.4 (6) |
Ru3—Ru4—N4—O4 | 179.9 (9) | Ru4—Ru3—C24—C25 | 119.9 (4) |
N3—Ru4—N4—Ru3 | −2.0 (2) | N3—Ru3—C24—C29 | −69.4 (7) |
C35—Ru4—N4—Ru3 | 130.9 (5) | N4—Ru3—C24—C29 | 59.1 (7) |
C34—Ru4—N4—Ru3 | 141.3 (3) | C21—Ru3—C24—C29 | −158.3 (7) |
C31—Ru4—N4—Ru3 | −133.2 (5) | C22—Ru3—C24—C29 | 159.1 (7) |
C32—Ru4—N4—Ru3 | −146.8 (3) | C25—Ru3—C24—C29 | −121.1 (8) |
C33—Ru4—N4—Ru3 | 177.0 (3) | C23—Ru3—C24—C29 | 122.6 (8) |
N1—Ru1—C1—C5 | −99.4 (4) | Ru4—Ru3—C24—C29 | −1.2 (8) |
N2—Ru1—C1—C5 | 113.8 (7) | C22—C21—C25—C24 | 0.5 (7) |
C4—Ru1—C1—C5 | 38.0 (4) | C26—C21—C25—C24 | 178.4 (6) |
C2—Ru1—C1—C5 | 118.2 (6) | Ru3—C21—C25—C24 | −61.4 (4) |
C3—Ru1—C1—C5 | 80.6 (4) | C22—C21—C25—C30 | −178.6 (6) |
Ru2—Ru1—C1—C5 | −118.9 (4) | C26—C21—C25—C30 | −0.7 (10) |
N1—Ru1—C1—C2 | 142.4 (4) | Ru3—C21—C25—C30 | 119.5 (6) |
N2—Ru1—C1—C2 | −4.4 (8) | C22—C21—C25—Ru3 | 61.9 (4) |
C4—Ru1—C1—C2 | −80.1 (4) | C26—C21—C25—Ru3 | −120.2 (6) |
C5—Ru1—C1—C2 | −118.2 (6) | C23—C24—C25—C21 | −1.7 (7) |
C3—Ru1—C1—C2 | −37.5 (4) | C29—C24—C25—C21 | −176.1 (6) |
Ru2—Ru1—C1—C2 | 122.9 (4) | Ru3—C24—C25—C21 | 61.5 (4) |
N1—Ru1—C1—C6 | 20.6 (6) | C23—C24—C25—C30 | 177.4 (6) |
N2—Ru1—C1—C6 | −126.2 (7) | C29—C24—C25—C30 | 3.0 (10) |
C4—Ru1—C1—C6 | 158.1 (6) | Ru3—C24—C25—C30 | −119.5 (6) |
C2—Ru1—C1—C6 | −121.8 (7) | C23—C24—C25—Ru3 | −63.2 (4) |
C5—Ru1—C1—C6 | 120.0 (7) | C29—C24—C25—Ru3 | 122.5 (7) |
C3—Ru1—C1—C6 | −159.3 (6) | N3—Ru3—C25—C21 | 101.5 (4) |
Ru2—Ru1—C1—C6 | 1.1 (8) | N4—Ru3—C25—C21 | −117.4 (7) |
C5—C1—C2—C3 | 1.9 (7) | C24—Ru3—C25—C21 | −117.9 (5) |
C6—C1—C2—C3 | −178.3 (6) | C22—Ru3—C25—C21 | −37.5 (4) |
Ru1—C1—C2—C3 | 63.5 (4) | C23—Ru3—C25—C21 | −79.8 (4) |
C5—C1—C2—C7 | 175.4 (6) | Ru4—Ru3—C25—C21 | 122.1 (3) |
C6—C1—C2—C7 | −4.8 (10) | N3—Ru3—C25—C24 | −140.6 (4) |
Ru1—C1—C2—C7 | −123.0 (6) | N4—Ru3—C25—C24 | 0.5 (8) |
C5—C1—C2—Ru1 | −61.5 (4) | C21—Ru3—C25—C24 | 117.9 (5) |
C6—C1—C2—Ru1 | 118.3 (6) | C22—Ru3—C25—C24 | 80.4 (4) |
N1—Ru1—C2—C3 | −166.8 (4) | C23—Ru3—C25—C24 | 38.1 (4) |
N2—Ru1—C2—C3 | 61.6 (5) | Ru4—Ru3—C25—C24 | −120.1 (4) |
C4—Ru1—C2—C3 | −36.8 (4) | N3—Ru3—C25—C30 | −18.5 (6) |
C5—Ru1—C2—C3 | −80.0 (4) | N4—Ru3—C25—C30 | 122.6 (7) |
C1—Ru1—C2—C3 | −116.6 (6) | C21—Ru3—C25—C30 | −120.0 (7) |
Ru2—Ru1—C2—C3 | 121.2 (4) | C24—Ru3—C25—C30 | 122.1 (7) |
N1—Ru1—C2—C1 | −50.2 (5) | C22—Ru3—C25—C30 | −157.5 (6) |
N2—Ru1—C2—C1 | 178.1 (4) | C23—Ru3—C25—C30 | 160.2 (6) |
C4—Ru1—C2—C1 | 79.8 (4) | Ru4—Ru3—C25—C30 | 2.1 (7) |
C5—Ru1—C2—C1 | 36.6 (4) | N3—Ru4—C31—C35 | 92.1 (4) |
C3—Ru1—C2—C1 | 116.6 (6) | N4—Ru4—C31—C35 | −137.3 (6) |
Ru2—Ru1—C2—C1 | −122.2 (4) | C34—Ru4—C31—C35 | −37.6 (4) |
N1—Ru1—C2—C7 | 71.8 (7) | C32—Ru4—C31—C35 | −117.3 (6) |
N2—Ru1—C2—C7 | −59.9 (7) | C33—Ru4—C31—C35 | −79.9 (5) |
C4—Ru1—C2—C7 | −158.3 (7) | Ru3—Ru4—C31—C35 | 116.4 (4) |
C5—Ru1—C2—C7 | 158.6 (7) | N3—Ru4—C31—C32 | −150.6 (5) |
C1—Ru1—C2—C7 | 122.0 (8) | N4—Ru4—C31—C32 | −20.0 (8) |
C3—Ru1—C2—C7 | −121.5 (8) | C35—Ru4—C31—C32 | 117.3 (6) |
Ru2—Ru1—C2—C7 | −0.2 (8) | C34—Ru4—C31—C32 | 79.6 (5) |
C1—C2—C3—C4 | −2.9 (7) | C33—Ru4—C31—C32 | 37.4 (5) |
C7—C2—C3—C4 | −176.5 (6) | Ru3—Ru4—C31—C32 | −126.4 (5) |
Ru1—C2—C3—C4 | 60.2 (4) | N3—Ru4—C31—C36 | −27.8 (8) |
C1—C2—C3—C8 | 178.6 (6) | N4—Ru4—C31—C36 | 102.8 (9) |
C7—C2—C3—C8 | 5.0 (10) | C35—Ru4—C31—C36 | −119.9 (9) |
Ru1—C2—C3—C8 | −118.3 (6) | C34—Ru4—C31—C36 | −157.6 (8) |
C1—C2—C3—Ru1 | −63.1 (4) | C32—Ru4—C31—C36 | 122.8 (9) |
C7—C2—C3—Ru1 | 123.3 (7) | C33—Ru4—C31—C36 | 160.2 (8) |
N1—Ru1—C3—C2 | 38.1 (10) | Ru3—Ru4—C31—C36 | −3.6 (10) |
N2—Ru1—C3—C2 | −129.9 (4) | C35—C31—C32—C33 | −0.8 (7) |
C4—Ru1—C3—C2 | 119.0 (6) | C36—C31—C32—C33 | 178.7 (7) |
C5—Ru1—C3—C2 | 80.2 (4) | Ru4—C31—C32—C33 | −62.4 (5) |
C1—Ru1—C3—C2 | 38.3 (4) | C35—C31—C32—C37 | −175.3 (7) |
Ru2—Ru1—C3—C2 | −122.2 (4) | C36—C31—C32—C37 | 4.2 (12) |
N1—Ru1—C3—C4 | −80.9 (10) | Ru4—C31—C32—C37 | 123.1 (8) |
N2—Ru1—C3—C4 | 111.1 (4) | C35—C31—C32—Ru4 | 61.6 (4) |
C2—Ru1—C3—C4 | −119.0 (6) | C36—C31—C32—Ru4 | −118.9 (7) |
C5—Ru1—C3—C4 | −38.8 (4) | N3—Ru4—C32—C33 | 157.7 (4) |
C1—Ru1—C3—C4 | −80.7 (4) | N4—Ru4—C32—C33 | −72.9 (5) |
Ru2—Ru1—C3—C4 | 118.8 (4) | C35—Ru4—C32—C33 | 79.6 (5) |
N1—Ru1—C3—C8 | 160.2 (8) | C34—Ru4—C32—C33 | 36.7 (4) |
N2—Ru1—C3—C8 | −7.8 (6) | C31—Ru4—C32—C33 | 117.0 (6) |
C4—Ru1—C3—C8 | −118.9 (8) | Ru3—Ru4—C32—C33 | −125.3 (5) |
C2—Ru1—C3—C8 | 122.1 (8) | N3—Ru4—C32—C31 | 40.7 (6) |
C5—Ru1—C3—C8 | −157.7 (7) | N4—Ru4—C32—C31 | 170.1 (4) |
C1—Ru1—C3—C8 | 160.4 (7) | C35—Ru4—C32—C31 | −37.4 (4) |
Ru2—Ru1—C3—C8 | −0.1 (8) | C34—Ru4—C32—C31 | −80.3 (5) |
C2—C3—C4—C5 | 2.8 (7) | C33—Ru4—C32—C31 | −117.0 (6) |
C8—C3—C4—C5 | −178.7 (6) | Ru3—Ru4—C32—C31 | 117.7 (4) |
Ru1—C3—C4—C5 | 63.3 (4) | N3—Ru4—C32—C37 | −78.9 (12) |
C2—C3—C4—C9 | −180.0 (6) | N4—Ru4—C32—C37 | 50.5 (12) |
C8—C3—C4—C9 | −1.4 (10) | C35—Ru4—C32—C37 | −157.0 (12) |
Ru1—C3—C4—C9 | −119.4 (6) | C34—Ru4—C32—C37 | 160.1 (12) |
C2—C3—C4—Ru1 | −60.5 (4) | C31—Ru4—C32—C37 | −119.6 (13) |
C8—C3—C4—Ru1 | 118.0 (6) | C33—Ru4—C32—C37 | 123.4 (13) |
N1—Ru1—C4—C3 | 155.3 (4) | Ru3—Ru4—C32—C37 | −1.9 (15) |
N2—Ru1—C4—C3 | −78.7 (4) | C31—C32—C33—C34 | 1.1 (8) |
C2—Ru1—C4—C3 | 36.3 (4) | C37—C32—C33—C34 | 175.4 (8) |
C5—Ru1—C4—C3 | 115.9 (5) | Ru4—C32—C33—C34 | −60.6 (5) |
C1—Ru1—C4—C3 | 79.1 (4) | C31—C32—C33—C38 | −179.2 (7) |
Ru2—Ru1—C4—C3 | −122.9 (4) | C37—C32—C33—C38 | −4.9 (12) |
N1—Ru1—C4—C5 | 39.5 (5) | Ru4—C32—C33—C38 | 119.1 (8) |
N2—Ru1—C4—C5 | 165.4 (4) | C31—C32—C33—Ru4 | 61.7 (5) |
C2—Ru1—C4—C5 | −79.6 (4) | C37—C32—C33—Ru4 | −123.9 (8) |
C1—Ru1—C4—C5 | −36.8 (4) | N3—Ru4—C33—C32 | −63.9 (11) |
C3—Ru1—C4—C5 | −115.9 (5) | N4—Ru4—C33—C32 | 119.1 (5) |
Ru2—Ru1—C4—C5 | 121.2 (4) | C35—Ru4—C33—C32 | −80.6 (5) |
N1—Ru1—C4—C9 | −82.9 (7) | C34—Ru4—C33—C32 | −118.9 (6) |
N2—Ru1—C4—C9 | 43.1 (7) | C31—Ru4—C33—C32 | −38.2 (4) |
C2—Ru1—C4—C9 | 158.1 (7) | Ru3—Ru4—C33—C32 | 123.5 (5) |
C5—Ru1—C4—C9 | −122.4 (8) | N3—Ru4—C33—C34 | 55.0 (12) |
C1—Ru1—C4—C9 | −159.2 (7) | N4—Ru4—C33—C34 | −122.0 (4) |
C3—Ru1—C4—C9 | 121.8 (8) | C35—Ru4—C33—C34 | 38.3 (4) |
Ru2—Ru1—C4—C9 | −1.2 (9) | C31—Ru4—C33—C34 | 80.8 (4) |
C2—C1—C5—C4 | −0.2 (7) | C32—Ru4—C33—C34 | 118.9 (6) |
C6—C1—C5—C4 | 180.0 (6) | Ru3—Ru4—C33—C34 | −117.6 (4) |
Ru1—C1—C5—C4 | −61.3 (4) | N3—Ru4—C33—C38 | 174.2 (9) |
C2—C1—C5—C10 | −178.6 (6) | N4—Ru4—C33—C38 | −2.8 (10) |
C6—C1—C5—C10 | 1.6 (10) | C35—Ru4—C33—C38 | 157.5 (11) |
Ru1—C1—C5—C10 | 120.4 (6) | C34—Ru4—C33—C38 | 119.2 (12) |
C2—C1—C5—Ru1 | 61.1 (4) | C31—Ru4—C33—C38 | −160.1 (11) |
C6—C1—C5—Ru1 | −118.7 (6) | C32—Ru4—C33—C38 | −121.9 (12) |
C3—C4—C5—C1 | −1.6 (7) | Ru3—Ru4—C33—C38 | 1.5 (13) |
C9—C4—C5—C1 | −178.8 (6) | C32—C33—C34—C35 | −1.0 (7) |
Ru1—C4—C5—C1 | 62.2 (4) | C38—C33—C34—C35 | 179.3 (7) |
C3—C4—C5—C10 | 176.7 (6) | Ru4—C33—C34—C35 | −62.0 (4) |
C9—C4—C5—C10 | −0.5 (10) | C32—C33—C34—C39 | −175.8 (7) |
Ru1—C4—C5—C10 | −119.5 (7) | C38—C33—C34—C39 | 4.5 (11) |
C3—C4—C5—Ru1 | −63.8 (4) | Ru4—C33—C34—C39 | 123.1 (7) |
C9—C4—C5—Ru1 | 119.0 (6) | C32—C33—C34—Ru4 | 61.1 (5) |
N1—Ru1—C5—C1 | 89.1 (4) | C38—C33—C34—Ru4 | −118.6 (7) |
N2—Ru1—C5—C1 | −142.7 (4) | N3—Ru4—C34—C33 | −160.4 (4) |
C4—Ru1—C5—C1 | −117.6 (5) | N4—Ru4—C34—C33 | 70.4 (5) |
C2—Ru1—C5—C1 | −37.5 (4) | C35—Ru4—C34—C33 | −116.6 (6) |
C3—Ru1—C5—C1 | −79.4 (4) | C31—Ru4—C34—C33 | −79.4 (5) |
Ru2—Ru1—C5—C1 | 122.2 (4) | C32—Ru4—C34—C33 | −36.5 (5) |
N1—Ru1—C5—C4 | −153.4 (4) | Ru3—Ru4—C34—C33 | 127.0 (5) |
N2—Ru1—C5—C4 | −25.2 (6) | N3—Ru4—C34—C35 | −43.8 (5) |
C2—Ru1—C5—C4 | 80.1 (4) | N4—Ru4—C34—C35 | −173.0 (4) |
C1—Ru1—C5—C4 | 117.6 (5) | C31—Ru4—C34—C35 | 37.2 (4) |
C3—Ru1—C5—C4 | 38.2 (4) | C32—Ru4—C34—C35 | 80.1 (5) |
Ru2—Ru1—C5—C4 | −120.2 (4) | C33—Ru4—C34—C35 | 116.6 (6) |
N1—Ru1—C5—C10 | −30.6 (7) | Ru3—Ru4—C34—C35 | −116.5 (4) |
N2—Ru1—C5—C10 | 97.6 (7) | N3—Ru4—C34—C39 | 74.7 (8) |
C4—Ru1—C5—C10 | 122.8 (8) | N4—Ru4—C34—C39 | −54.5 (8) |
C2—Ru1—C5—C10 | −157.2 (7) | C35—Ru4—C34—C39 | 118.5 (9) |
C1—Ru1—C5—C10 | −119.7 (8) | C31—Ru4—C34—C39 | 155.7 (9) |
C3—Ru1—C5—C10 | 160.9 (8) | C32—Ru4—C34—C39 | −161.4 (9) |
Ru2—Ru1—C5—C10 | 2.6 (9) | C33—Ru4—C34—C39 | −124.9 (9) |
N2—Ru2—C11—C15 | −113.6 (7) | Ru3—Ru4—C34—C39 | 2.1 (10) |
N1—Ru2—C11—C15 | 100.8 (4) | C32—C31—C35—C34 | 0.2 (7) |
C14—Ru2—C11—C15 | −37.3 (4) | C36—C31—C35—C34 | −179.3 (6) |
C12—Ru2—C11—C15 | −117.3 (6) | Ru4—C31—C35—C34 | 62.3 (4) |
C13—Ru2—C11—C15 | −80.2 (4) | C32—C31—C35—C40 | 179.4 (6) |
Ru1—Ru2—C11—C15 | 119.4 (4) | C36—C31—C35—C40 | −0.1 (10) |
N2—Ru2—C11—C12 | 3.8 (8) | Ru4—C31—C35—C40 | −118.5 (6) |
N1—Ru2—C11—C12 | −141.8 (4) | C32—C31—C35—Ru4 | −62.1 (5) |
C15—Ru2—C11—C12 | 117.3 (6) | C36—C31—C35—Ru4 | 118.3 (7) |
C14—Ru2—C11—C12 | 80.0 (4) | C33—C34—C35—C31 | 0.5 (7) |
C13—Ru2—C11—C12 | 37.1 (4) | C39—C34—C35—C31 | 175.6 (6) |
Ru1—Ru2—C11—C12 | −123.3 (4) | Ru4—C34—C35—C31 | −62.6 (4) |
N2—Ru2—C11—C16 | 126.0 (7) | C33—C34—C35—C40 | −178.7 (6) |
N1—Ru2—C11—C16 | −19.6 (6) | C39—C34—C35—C40 | −3.6 (10) |
C15—Ru2—C11—C16 | −120.4 (7) | Ru4—C34—C35—C40 | 118.2 (6) |
C14—Ru2—C11—C16 | −157.8 (6) | C33—C34—C35—Ru4 | 63.1 (5) |
C12—Ru2—C11—C16 | 122.2 (7) | C39—C34—C35—Ru4 | −121.8 (6) |
C13—Ru2—C11—C16 | 159.3 (6) | N3—Ru4—C35—C31 | −94.8 (4) |
Ru1—Ru2—C11—C16 | −1.0 (7) | N4—Ru4—C35—C31 | 132.7 (6) |
C15—C11—C12—C13 | −1.8 (7) | C34—Ru4—C35—C31 | 117.7 (6) |
C16—C11—C12—C13 | 179.1 (6) | C32—Ru4—C35—C31 | 37.9 (5) |
Ru2—C11—C12—C13 | −62.9 (4) | C33—Ru4—C35—C31 | 80.0 (5) |
C15—C11—C12—C17 | −175.7 (6) | Ru3—Ru4—C35—C31 | −120.4 (4) |
C16—C11—C12—C17 | 5.2 (10) | N3—Ru4—C35—C34 | 147.5 (4) |
Ru2—C11—C12—C17 | 123.3 (6) | N4—Ru4—C35—C34 | 15.0 (8) |
C15—C11—C12—Ru2 | 61.1 (4) | C31—Ru4—C35—C34 | −117.7 (6) |
C16—C11—C12—Ru2 | −118.0 (6) | C32—Ru4—C35—C34 | −79.8 (5) |
N2—Ru2—C12—C13 | −61.0 (4) | C33—Ru4—C35—C34 | −37.7 (5) |
N1—Ru2—C12—C13 | 167.7 (4) | Ru3—Ru4—C35—C34 | 121.8 (4) |
C15—Ru2—C12—C13 | 80.1 (4) | N3—Ru4—C35—C40 | 25.9 (6) |
C14—Ru2—C12—C13 | 37.4 (4) | N4—Ru4—C35—C40 | −106.7 (7) |
C11—Ru2—C12—C13 | 117.5 (6) | C34—Ru4—C35—C40 | −121.6 (8) |
Ru1—Ru2—C12—C13 | −122.9 (4) | C31—Ru4—C35—C40 | 120.6 (8) |
N2—Ru2—C12—C11 | −178.4 (4) | C32—Ru4—C35—C40 | 158.6 (7) |
N1—Ru2—C12—C11 | 50.2 (5) | C33—Ru4—C35—C40 | −159.4 (7) |
C15—Ru2—C12—C11 | −37.4 (4) | Ru3—Ru4—C35—C40 | 0.2 (7) |
Experimental details
Crystal data | |
Chemical formula | [Ru2(C10H15)2(NO)2] |
Mr | 532.60 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 90 |
a, b, c (Å) | 10.7181 (3), 10.7364 (3), 17.9238 (5) |
α, β, γ (°) | 89.209 (1), 89.220 (1), 85.373 (1) |
V (Å3) | 2055.48 (10) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.49 |
Crystal size (mm) | 0.3 × 0.2 × 0.13 |
Data collection | |
Diffractometer | Bruker SMART APEXII |
Absorption correction | Multi-scan (SADABS; Bruker 2004) |
Tmin, Tmax | 0.705, 0.824 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 29941, 10102, 9591 |
Rint | 0.040 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.139, 1.26 |
No. of reflections | 10102 |
No. of parameters | 490 |
No. of restraints | 18 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0465P)2 + 11.2766P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 2.12, −2.33 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 2000).
X-ray diffraction data on title compound were collected at 90 (1) K using a Bruker SMART APEX2 CCD diffractometer installed at a rotating anode source (Mo Kα radiation, λ =0.71073 Å), and equipped with an Oxford Cryosystems nitrogen gas-flow apparatus. The data were collected by the oscillation method with 0.5°frame-width (ω-scan) and a 15 sec exposure per frame. Four sets of data (360 frames in each set) were collected, nominally covering complete reciprocal space. The data were integrated, scaled, sorted and averaged using the APEX2 software package.
All crystals examined were twinned. The metric symmetry of the unit cell suggested a monoclinic C-centred cell. However the structure could be solved, with some difficulties, in the triclinic space group P 1 only (Direct Methods, SHELXTL Version 6.14). The twin law (0 - 1 0, -1 0 0, 0 0 - 1) was used during refinement. The volume ratios of the twins refined to 0.298 (1): 0.702 (1).
All non-hydrogen atoms were refined anisotropically. Positions of hydrogen atoms were calculated from the geometry of surrounding carbon atoms. The CH3 H atoms were treated as part of idealized CH3 groups with Uiso=1.5Ueq. For the carbon atoms C22, C31 and C35 isotropic restraints have been imposed to avoid non positive definite ADPs.