Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806031989/ww2042sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806031989/ww2042Isup2.hkl |
CCDC reference: 621532
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- H-atom completeness 98%
- Disorder in main residue
- R factor = 0.050
- wR factor = 0.146
- Data-to-parameter ratio = 11.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.75 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.14 Ratio PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C01 PLAT301_ALERT_3_B Main Residue Disorder ......................... 31.00 Perc.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.70 mm PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for P2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C03 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 47.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 F6 P
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C48 H74 Cl2 F12 N4 P4 Ru1 Atom count from the _atom_site data: C48 H72 Cl2 F12 N4 P4 Ru1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C48 H74 Cl2 F12 N4 P4 Ru TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 192.00 192.00 0.00 H 296.00 288.00 8.00 Cl 8.00 8.00 0.00 F 48.00 48.00 0.00 N 16.00 16.00 0.00 P 16.00 16.00 0.00 Ru 4.00 4.00 0.00 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: CrystalClear (Rigaku/MSC, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1999); software used to prepare material for publication: SHELXTL.
[Ru(C2H3N)(C21H15N3)(C12H27P)2](PF6)2·CH2Cl2 | F(000) = 2544 |
Mr = 1230.96 | Dx = 1.333 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 6998 reflections |
a = 18.9433 (13) Å | θ = 3.1–27.5° |
b = 20.9992 (13) Å | µ = 0.52 mm−1 |
c = 15.4852 (10) Å | T = 293 K |
β = 95.120 (3)° | Prism, red |
V = 6135.3 (7) Å3 | 0.70 × 0.40 × 0.20 mm |
Z = 4 |
Mercury CCD diffractometer | 5404 independent reflections |
Radiation source: fine-focus sealed tube | 4961 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
φ? ω? scans | θmax = 25.0°, θmin = 3.1° |
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2000) | h = −22→22 |
Tmin = 0.714, Tmax = 0.904 | k = −24→22 |
19100 measured reflections | l = −17→18 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.146 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0866P)2 + 6.6163P] where P = (Fo2 + 2Fc2)/3 |
5404 reflections | (Δ/σ)max = 0.001 |
487 parameters | Δρmax = 0.79 e Å−3 |
467 restraints | Δρmin = −0.71 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) | |
Ru | 0.0000 | 0.159560 (15) | 0.2500 | 0.03811 (15) | |
P1 | −0.02227 (5) | 0.16437 (4) | 0.09489 (6) | 0.0489 (2) | |
F1 | −0.3174 (6) | 0.1628 (4) | −0.1631 (5) | 0.180 (3) | 0.755 (8) |
F2 | −0.2391 (4) | 0.1902 (3) | −0.2524 (7) | 0.152 (3) | 0.755 (8) |
F3 | −0.3131 (3) | 0.0624 (3) | −0.2084 (7) | 0.143 (3) | 0.755 (8) |
F4 | −0.3375 (5) | 0.1432 (6) | −0.3009 (6) | 0.156 (4) | 0.755 (8) |
F5 | −0.2347 (3) | 0.0909 (3) | −0.2971 (3) | 0.1185 (19) | 0.755 (8) |
F6 | −0.2145 (5) | 0.1103 (5) | −0.1610 (6) | 0.142 (3) | 0.755 (8) |
F1' | −0.2383 (11) | 0.1636 (12) | −0.2971 (14) | 0.143 (6) | 0.245 (8) |
F2' | −0.3487 (9) | 0.1555 (11) | −0.2710 (16) | 0.112 (7) | 0.245 (8) |
F3' | −0.2069 (9) | 0.1020 (12) | −0.1817 (16) | 0.102 (6) | 0.245 (8) |
F4' | −0.2685 (13) | 0.1883 (8) | −0.1710 (15) | 0.145 (6) | 0.245 (8) |
F5' | −0.3196 (11) | 0.0950 (14) | −0.1590 (14) | 0.165 (6) | 0.245 (8) |
F6' | −0.2872 (14) | 0.0679 (8) | −0.2846 (14) | 0.140 (6) | 0.245 (8) |
N1 | 0.10658 (13) | 0.14087 (13) | 0.23694 (17) | 0.0426 (6) | |
N2 | 0.0000 | 0.06662 (17) | 0.2500 | 0.0390 (8) | |
N3 | 0.0000 | 0.2573 (2) | 0.2500 | 0.0504 (9) | |
C1 | 0.16032 (18) | 0.18241 (18) | 0.2349 (2) | 0.0510 (8) | |
H1A | 0.1512 | 0.2256 | 0.2414 | 0.061* | |
C2 | 0.2281 (2) | 0.16333 (18) | 0.2235 (3) | 0.0610 (10) | |
H2A | 0.2642 | 0.1933 | 0.2225 | 0.073* | |
C3 | 0.24228 (19) | 0.1000 (2) | 0.2137 (3) | 0.0652 (10) | |
H3A | 0.2880 | 0.0865 | 0.2055 | 0.078* | |
C4 | 0.18791 (18) | 0.05632 (18) | 0.2161 (2) | 0.0549 (9) | |
H4A | 0.1965 | 0.0131 | 0.2094 | 0.066* | |
C5 | 0.12083 (16) | 0.07757 (15) | 0.2286 (2) | 0.0422 (7) | |
C6 | 0.06045 (15) | 0.03456 (15) | 0.23790 (19) | 0.0405 (7) | |
C7 | 0.06118 (16) | −0.03097 (15) | 0.2367 (2) | 0.0458 (7) | |
H7A | 0.1027 | −0.0524 | 0.2269 | 0.055* | |
C8 | 0.0000 | −0.0655 (2) | 0.2500 | 0.0433 (10) | |
C9 | 0.0000 | −0.1362 (2) | 0.2500 | 0.0496 (11) | |
C10 | 0.0610 (2) | −0.16972 (18) | 0.2748 (3) | 0.0645 (10) | |
H10A | 0.1026 | −0.1478 | 0.2916 | 0.077* | |
C11 | 0.0608 (3) | −0.2357 (2) | 0.2750 (3) | 0.0825 (14) | |
H11A | 0.1023 | −0.2577 | 0.2923 | 0.099* | |
C12 | 0.0000 | −0.2687 (3) | 0.2500 | 0.084 (2) | |
H12A | 0.0000 | −0.3130 | 0.2500 | 0.101* | |
C21 | 0.046 (2) | 0.2019 (18) | 0.039 (3) | 0.070 (6) | 0.20 (2) |
H21A | 0.0876 | 0.1751 | 0.0480 | 0.083* | 0.20 (2) |
H21B | 0.0304 | 0.1992 | −0.0227 | 0.083* | 0.20 (2) |
C22 | 0.071 (2) | 0.2694 (18) | 0.055 (3) | 0.079 (6) | 0.20 (2) |
H22A | 0.0873 | 0.2741 | 0.1159 | 0.095* | 0.20 (2) |
H22B | 0.0311 | 0.2983 | 0.0427 | 0.095* | 0.20 (2) |
C23 | 0.130 (2) | 0.287 (2) | −0.001 (2) | 0.093 (6) | 0.20 (2) |
H23A | 0.1741 | 0.2669 | 0.0226 | 0.112* | 0.20 (2) |
H23B | 0.1191 | 0.2708 | −0.0592 | 0.112* | 0.20 (2) |
C24 | 0.141 (3) | 0.356 (2) | −0.005 (4) | 0.129 (13) | 0.20 (2) |
H24A | 0.1726 | 0.3657 | −0.0488 | 0.194* | 0.20 (2) |
H24B | 0.1620 | 0.3712 | 0.0502 | 0.194* | 0.20 (2) |
H24C | 0.0966 | 0.3770 | −0.0189 | 0.194* | 0.20 (2) |
C21' | 0.0565 (4) | 0.1812 (5) | 0.0368 (6) | 0.0586 (18) | 0.80 (2) |
H21C | 0.0950 | 0.1542 | 0.0607 | 0.070* | 0.80 (2) |
H21D | 0.0460 | 0.1695 | −0.0235 | 0.070* | 0.80 (2) |
C22' | 0.0812 (5) | 0.2486 (5) | 0.0407 (6) | 0.076 (2) | 0.80 (2) |
H22C | 0.0848 | 0.2629 | 0.1005 | 0.091* | 0.80 (2) |
H22D | 0.0463 | 0.2751 | 0.0081 | 0.091* | 0.80 (2) |
C23' | 0.1536 (5) | 0.2574 (7) | 0.0039 (6) | 0.101 (3) | 0.80 (2) |
H23C | 0.1905 | 0.2401 | 0.0448 | 0.121* | 0.80 (2) |
H23D | 0.1539 | 0.2335 | −0.0497 | 0.121* | 0.80 (2) |
C24' | 0.1694 (9) | 0.3246 (8) | −0.0129 (9) | 0.142 (5) | 0.80 (2) |
H24D | 0.2147 | 0.3278 | −0.0359 | 0.213* | 0.80 (2) |
H24E | 0.1703 | 0.3483 | 0.0402 | 0.213* | 0.80 (2) |
H24F | 0.1334 | 0.3417 | −0.0542 | 0.213* | 0.80 (2) |
C25 | −0.092 (4) | 0.224 (3) | 0.057 (3) | 0.069 (6) | 0.354 (13) |
H25A | −0.1371 | 0.2120 | 0.0776 | 0.083* | 0.354 (13) |
H25B | −0.0793 | 0.2657 | 0.0816 | 0.083* | 0.354 (13) |
C26 | −0.102 (3) | 0.2306 (19) | −0.042 (3) | 0.086 (5) | 0.354 (13) |
H26A | −0.1358 | 0.1989 | −0.0644 | 0.104* | 0.354 (13) |
H26B | −0.0570 | 0.2215 | −0.0647 | 0.104* | 0.354 (13) |
C27 | −0.1273 (10) | 0.2963 (12) | −0.0728 (15) | 0.097 (5) | 0.354 (13) |
H27A | −0.0937 | 0.3282 | −0.0499 | 0.117* | 0.354 (13) |
H27B | −0.1291 | 0.2978 | −0.1356 | 0.117* | 0.354 (13) |
C28 | −0.1974 (9) | 0.3115 (13) | −0.0458 (13) | 0.125 (7) | 0.354 (13) |
H28A | −0.2124 | 0.3522 | −0.0690 | 0.187* | 0.354 (13) |
H28B | −0.1952 | 0.3128 | 0.0163 | 0.187* | 0.354 (13) |
H28C | −0.2306 | 0.2794 | −0.0671 | 0.187* | 0.354 (13) |
C25' | −0.0871 (18) | 0.2217 (16) | 0.0561 (16) | 0.062 (3) | 0.646 (13) |
H25C | −0.1309 | 0.2114 | 0.0810 | 0.074* | 0.646 (13) |
H25D | −0.0717 | 0.2629 | 0.0791 | 0.074* | 0.646 (13) |
C26' | −0.1043 (17) | 0.2291 (10) | −0.0419 (16) | 0.086 (3) | 0.646 (13) |
H26C | −0.0613 | 0.2403 | −0.0681 | 0.103* | 0.646 (13) |
H26D | −0.1210 | 0.1887 | −0.0661 | 0.103* | 0.646 (13) |
C27' | −0.1605 (7) | 0.2801 (6) | −0.0643 (9) | 0.115 (4) | 0.646 (13) |
H27C | −0.1796 | 0.2750 | −0.1241 | 0.138* | 0.646 (13) |
H27D | −0.1990 | 0.2750 | −0.0276 | 0.138* | 0.646 (13) |
C28' | −0.1295 (8) | 0.3450 (5) | −0.0518 (9) | 0.150 (5) | 0.646 (13) |
H28D | −0.1660 | 0.3763 | −0.0637 | 0.225* | 0.646 (13) |
H28E | −0.0933 | 0.3510 | −0.0907 | 0.225* | 0.646 (13) |
H28F | −0.1092 | 0.3496 | 0.0069 | 0.225* | 0.646 (13) |
C29 | −0.0449 (18) | 0.0946 (17) | 0.035 (3) | 0.061 (5) | 0.48 (5) |
H29A | −0.0391 | 0.1028 | −0.0255 | 0.073* | 0.48 (5) |
H29B | −0.0119 | 0.0612 | 0.0546 | 0.073* | 0.48 (5) |
C30 | −0.1194 (17) | 0.0710 (14) | 0.043 (3) | 0.067 (4) | 0.48 (5) |
H30A | −0.1529 | 0.0977 | 0.0082 | 0.080* | 0.48 (5) |
H30B | −0.1303 | 0.0733 | 0.1025 | 0.080* | 0.48 (5) |
C31 | −0.1262 (17) | 0.0026 (12) | 0.0109 (18) | 0.088 (5) | 0.48 (5) |
H31A | −0.1164 | 0.0010 | −0.0495 | 0.105* | 0.48 (5) |
H31B | −0.0911 | −0.0233 | 0.0439 | 0.105* | 0.48 (5) |
C32 | −0.196 (2) | −0.0239 (14) | 0.019 (2) | 0.120 (7) | 0.48 (5) |
H32A | −0.1981 | −0.0669 | −0.0020 | 0.180* | 0.48 (5) |
H32B | −0.2314 | 0.0012 | −0.0142 | 0.180* | 0.48 (5) |
H32C | −0.2060 | −0.0235 | 0.0790 | 0.180* | 0.48 (5) |
C29' | −0.0562 (17) | 0.0855 (16) | 0.044 (2) | 0.061 (4) | 0.52 (5) |
H29C | −0.0462 | 0.0854 | −0.0163 | 0.073* | 0.52 (5) |
H29D | −0.0292 | 0.0511 | 0.0727 | 0.073* | 0.52 (5) |
C30' | −0.1337 (16) | 0.0712 (13) | 0.048 (3) | 0.070 (4) | 0.52 (5) |
H30C | −0.1615 | 0.1019 | 0.0122 | 0.084* | 0.52 (5) |
H30D | −0.1458 | 0.0757 | 0.1068 | 0.084* | 0.52 (5) |
C31' | −0.1528 (14) | 0.0049 (11) | 0.0160 (17) | 0.084 (5) | 0.52 (5) |
H31C | −0.1363 | −0.0008 | −0.0410 | 0.101* | 0.52 (5) |
H31D | −0.1279 | −0.0256 | 0.0547 | 0.101* | 0.52 (5) |
C32' | −0.2287 (15) | −0.0092 (12) | 0.0110 (15) | 0.104 (6) | 0.52 (5) |
H32D | −0.2367 | −0.0521 | −0.0091 | 0.155* | 0.52 (5) |
H32E | −0.2537 | 0.0198 | −0.0287 | 0.155* | 0.52 (5) |
H32F | −0.2454 | −0.0046 | 0.0674 | 0.155* | 0.52 (5) |
P2 | −0.27772 (7) | 0.12683 (6) | −0.22956 (9) | 0.0781 (4) | |
C01 | 0.0000 | 0.3099 (2) | 0.2500 | 0.0693 (16) | |
C02 | 0.0000 | 0.3818 (2) | 0.2500 | 0.152 (5) | |
H02A | −0.0431 | 0.3970 | 0.2195 | 0.228* | 0.50 |
H02B | 0.0399 | 0.3970 | 0.2218 | 0.228* | 0.50 |
H02C | 0.0032 | 0.3970 | 0.3087 | 0.228* | 0.50 |
Cl2 | 0.0472 (7) | 0.4887 (7) | 0.0382 (9) | 0.380* | 0.50 |
Cl1 | −0.0276 (8) | 0.5479 (9) | 0.1678 (10) | 0.460* | 0.50 |
C03 | −0.0383 (8) | 0.5107 (13) | 0.0654 (13) | 0.243 (12)* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru | 0.0392 (2) | 0.0314 (2) | 0.0432 (2) | 0.000 | 0.00079 (14) | 0.000 |
P1 | 0.0518 (5) | 0.0499 (5) | 0.0441 (5) | −0.0033 (4) | −0.0003 (4) | 0.0017 (3) |
F1 | 0.214 (8) | 0.154 (7) | 0.188 (6) | 0.072 (6) | 0.106 (6) | −0.022 (5) |
F2 | 0.143 (4) | 0.060 (3) | 0.259 (9) | 0.023 (3) | 0.047 (5) | 0.023 (4) |
F3 | 0.117 (4) | 0.092 (4) | 0.222 (8) | −0.002 (3) | 0.028 (4) | 0.031 (4) |
F4 | 0.102 (5) | 0.213 (9) | 0.146 (6) | 0.045 (5) | −0.024 (5) | 0.032 (6) |
F5 | 0.123 (4) | 0.122 (4) | 0.113 (3) | 0.031 (3) | 0.025 (3) | −0.021 (3) |
F6 | 0.150 (6) | 0.152 (7) | 0.114 (5) | 0.030 (5) | −0.048 (5) | −0.014 (4) |
F1' | 0.133 (10) | 0.142 (13) | 0.161 (12) | −0.008 (11) | 0.049 (10) | 0.032 (10) |
F2' | 0.060 (7) | 0.095 (10) | 0.182 (18) | 0.032 (6) | 0.011 (10) | 0.015 (11) |
F3' | 0.081 (8) | 0.083 (9) | 0.143 (15) | 0.054 (7) | 0.015 (9) | 0.000 (9) |
F4' | 0.163 (13) | 0.078 (9) | 0.198 (12) | 0.031 (9) | 0.031 (11) | −0.026 (9) |
F5' | 0.179 (12) | 0.145 (13) | 0.179 (13) | 0.008 (12) | 0.056 (11) | 0.051 (11) |
F6' | 0.163 (12) | 0.095 (9) | 0.156 (11) | 0.004 (10) | −0.018 (11) | −0.043 (9) |
N1 | 0.0401 (13) | 0.0406 (14) | 0.0463 (14) | −0.0046 (11) | 0.0003 (11) | −0.0023 (11) |
N2 | 0.0374 (18) | 0.0363 (19) | 0.0431 (19) | 0.000 | 0.0019 (14) | 0.000 |
N3 | 0.048 (2) | 0.040 (2) | 0.062 (2) | 0.000 | 0.0015 (18) | 0.000 |
C1 | 0.0498 (19) | 0.0445 (19) | 0.058 (2) | −0.0110 (15) | 0.0002 (15) | −0.0022 (15) |
C2 | 0.0458 (19) | 0.062 (3) | 0.076 (3) | −0.0159 (16) | 0.0075 (18) | −0.0057 (18) |
C3 | 0.0418 (19) | 0.069 (3) | 0.086 (3) | −0.0028 (17) | 0.0134 (18) | −0.004 (2) |
C4 | 0.0459 (18) | 0.048 (2) | 0.072 (2) | 0.0033 (15) | 0.0102 (16) | −0.0039 (16) |
C5 | 0.0387 (15) | 0.0380 (17) | 0.0495 (17) | −0.0014 (12) | 0.0019 (13) | 0.0002 (13) |
C6 | 0.0398 (16) | 0.0367 (16) | 0.0449 (16) | 0.0006 (12) | 0.0027 (13) | −0.0022 (12) |
C7 | 0.0457 (17) | 0.0372 (17) | 0.0546 (19) | 0.0042 (13) | 0.0060 (14) | −0.0009 (14) |
C8 | 0.047 (2) | 0.038 (2) | 0.045 (2) | 0.000 | 0.0037 (19) | 0.000 |
C9 | 0.064 (3) | 0.034 (2) | 0.053 (3) | 0.000 | 0.015 (2) | 0.000 |
C10 | 0.071 (3) | 0.042 (2) | 0.082 (3) | 0.0054 (17) | 0.012 (2) | 0.0000 (17) |
C11 | 0.105 (4) | 0.045 (2) | 0.100 (3) | 0.022 (2) | 0.024 (3) | 0.011 (2) |
C12 | 0.118 (6) | 0.035 (3) | 0.105 (5) | 0.000 | 0.041 (4) | 0.000 |
C21 | 0.068 (11) | 0.072 (13) | 0.069 (10) | 0.003 (11) | 0.005 (9) | 0.005 (11) |
C22 | 0.074 (11) | 0.083 (13) | 0.081 (11) | −0.033 (11) | 0.015 (10) | 0.023 (11) |
C23 | 0.088 (11) | 0.105 (12) | 0.089 (10) | −0.032 (10) | 0.024 (10) | 0.020 (11) |
C24 | 0.13 (2) | 0.12 (2) | 0.14 (2) | −0.06 (2) | 0.04 (2) | 0.03 (2) |
C21' | 0.062 (4) | 0.068 (5) | 0.048 (3) | 0.004 (3) | 0.012 (2) | 0.007 (3) |
C22' | 0.077 (4) | 0.086 (6) | 0.065 (4) | −0.010 (4) | 0.012 (3) | 0.008 (4) |
C23' | 0.088 (5) | 0.125 (8) | 0.092 (5) | −0.025 (5) | 0.014 (4) | 0.024 (5) |
C24' | 0.165 (11) | 0.145 (11) | 0.123 (7) | −0.069 (9) | 0.055 (7) | 0.001 (8) |
C25 | 0.076 (10) | 0.061 (9) | 0.065 (9) | 0.010 (8) | −0.021 (9) | 0.017 (9) |
C26 | 0.098 (8) | 0.093 (8) | 0.065 (8) | 0.004 (8) | −0.015 (8) | 0.023 (8) |
C27 | 0.106 (10) | 0.107 (10) | 0.077 (8) | 0.018 (9) | −0.003 (8) | 0.027 (8) |
C28 | 0.118 (13) | 0.154 (16) | 0.102 (11) | 0.055 (12) | 0.008 (10) | 0.008 (11) |
C25' | 0.066 (7) | 0.060 (6) | 0.058 (5) | 0.001 (5) | −0.002 (5) | 0.004 (5) |
C26' | 0.102 (6) | 0.093 (6) | 0.059 (5) | −0.002 (5) | −0.022 (5) | 0.019 (5) |
C27' | 0.117 (9) | 0.131 (8) | 0.092 (6) | 0.020 (7) | −0.019 (7) | 0.041 (6) |
C28' | 0.203 (14) | 0.106 (9) | 0.139 (10) | 0.038 (9) | 0.000 (9) | 0.017 (7) |
C29 | 0.066 (8) | 0.064 (10) | 0.054 (8) | −0.008 (6) | 0.007 (6) | −0.007 (7) |
C30 | 0.073 (10) | 0.076 (6) | 0.051 (6) | −0.017 (7) | 0.006 (8) | −0.008 (5) |
C31 | 0.091 (12) | 0.091 (7) | 0.081 (7) | −0.034 (9) | 0.004 (9) | −0.016 (5) |
C32 | 0.131 (18) | 0.132 (14) | 0.099 (11) | −0.029 (14) | 0.022 (13) | −0.015 (10) |
C29' | 0.076 (10) | 0.058 (7) | 0.049 (8) | −0.012 (6) | 0.002 (7) | −0.008 (6) |
C30' | 0.075 (10) | 0.077 (6) | 0.057 (7) | −0.027 (6) | −0.002 (8) | 0.000 (5) |
C31' | 0.082 (12) | 0.082 (7) | 0.088 (7) | −0.047 (8) | 0.002 (8) | −0.014 (5) |
C32' | 0.106 (13) | 0.100 (11) | 0.100 (8) | −0.057 (10) | −0.015 (9) | 0.003 (8) |
P2 | 0.0733 (7) | 0.0605 (7) | 0.0998 (9) | 0.0244 (6) | 0.0031 (6) | 0.0009 (6) |
C01 | 0.059 (3) | 0.034 (3) | 0.115 (5) | 0.000 | 0.008 (3) | 0.000 |
C02 | 0.101 (6) | 0.037 (4) | 0.319 (16) | 0.000 | 0.028 (8) | 0.000 |
Ru—N2 | 1.952 (4) | C22'—C23' | 1.542 (8) |
Ru—N3 | 2.052 (4) | C22'—H22C | 0.9700 |
Ru—N1 | 2.084 (3) | C22'—H22D | 0.9700 |
Ru—N1i | 2.084 (3) | C23'—C24' | 1.472 (10) |
Ru—P1i | 2.4035 (9) | C23'—H23C | 0.9700 |
Ru—P1 | 2.4035 (9) | C23'—H23D | 0.9700 |
P1—C29 | 1.76 (3) | C24'—H24D | 0.9600 |
P1—C25' | 1.79 (2) | C24'—H24E | 0.9600 |
P1—C21 | 1.80 (4) | C24'—H24F | 0.9600 |
P1—C21' | 1.843 (8) | C25—C26 | 1.521 (14) |
P1—C25 | 1.89 (5) | C25—H25A | 0.9700 |
P1—C29' | 1.92 (3) | C25—H25B | 0.9700 |
F1—P2 | 1.527 (5) | C26—C27 | 1.527 (16) |
F2—P2 | 1.574 (6) | C26—H26A | 0.9700 |
F3—P2 | 1.557 (5) | C26—H26B | 0.9700 |
F4—P2 | 1.549 (6) | C27—C28 | 1.462 (15) |
F5—P2 | 1.574 (4) | C27—H27A | 0.9700 |
F6—P2 | 1.566 (6) | C27—H27B | 0.9700 |
F1'—P2 | 1.545 (12) | C28—H28A | 0.9600 |
F2'—P2 | 1.558 (12) | C28—H28B | 0.9600 |
F3'—P2 | 1.564 (11) | C28—H28C | 0.9600 |
F4'—P2 | 1.578 (11) | C25'—C26' | 1.531 (10) |
F5'—P2 | 1.558 (12) | C25'—H25C | 0.9700 |
F6'—P2 | 1.505 (14) | C25'—H25D | 0.9700 |
N1—C1 | 1.343 (4) | C26'—C27' | 1.528 (13) |
N1—C5 | 1.365 (4) | C26'—H26C | 0.9700 |
N2—C6i | 1.356 (3) | C26'—H26D | 0.9700 |
N2—C6 | 1.356 (3) | C27'—C28' | 1.489 (12) |
N3—C01 | 1.106 (6) | C27'—H27C | 0.9700 |
C1—C2 | 1.372 (5) | C27'—H27D | 0.9700 |
C1—H1A | 0.9300 | C28'—H28D | 0.9600 |
C2—C3 | 1.367 (5) | C28'—H28E | 0.9600 |
C2—H2A | 0.9300 | C28'—H28F | 0.9600 |
C3—C4 | 1.382 (5) | C29—C30 | 1.511 (12) |
C3—H3A | 0.9300 | C29—H29A | 0.9700 |
C4—C5 | 1.377 (4) | C29—H29B | 0.9700 |
C4—H4A | 0.9300 | C30—C31 | 1.518 (13) |
C5—C6 | 1.475 (4) | C30—H30A | 0.9700 |
C6—C7 | 1.376 (4) | C30—H30B | 0.9700 |
C7—C8 | 1.398 (4) | C31—C32 | 1.458 (13) |
C7—H7A | 0.9300 | C31—H31A | 0.9700 |
C8—C7i | 1.398 (4) | C31—H31B | 0.9700 |
C8—C9 | 1.484 (6) | C32—H32A | 0.9600 |
C9—C10 | 1.378 (5) | C32—H32B | 0.9600 |
C9—C10i | 1.378 (5) | C32—H32C | 0.9600 |
C10—C11 | 1.385 (6) | C29'—C30' | 1.504 (12) |
C10—H10A | 0.9300 | C29'—H29C | 0.9700 |
C11—C12 | 1.370 (6) | C29'—H29D | 0.9700 |
C11—H11A | 0.9300 | C30'—C31' | 1.508 (12) |
C12—C11i | 1.370 (6) | C30'—H30C | 0.9700 |
C12—H12A | 0.9300 | C30'—H30D | 0.9700 |
C21—C22 | 1.508 (16) | C31'—C32' | 1.463 (12) |
C21—H21A | 0.9700 | C31'—H31C | 0.9700 |
C21—H21B | 0.9700 | C31'—H31D | 0.9700 |
C22—C23 | 1.535 (16) | C32'—H32D | 0.9600 |
C22—H22A | 0.9700 | C32'—H32E | 0.9600 |
C22—H22B | 0.9700 | C32'—H32F | 0.9600 |
C23—C24 | 1.469 (16) | C01—C02 | 1.508 (5) |
C23—H23A | 0.9700 | C02—H02A | 0.9600 |
C23—H23B | 0.9700 | C02—H02B | 0.9600 |
C24—H24A | 0.9600 | C02—H02C | 0.9600 |
C24—H24B | 0.9600 | Cl2—C03ii | 1.60 (2) |
C24—H24C | 0.9600 | Cl2—C03 | 1.772 (5) |
C21'—C22' | 1.491 (8) | Cl2—Cl2ii | 2.11 (2) |
C21'—H21C | 0.9700 | Cl1—C03 | 1.764 (5) |
C21'—H21D | 0.9700 | C03—Cl2ii | 1.60 (2) |
N2—Ru—N3 | 180.0 | C27—C26—H26A | 108.9 |
N2—Ru—N1 | 79.15 (7) | C25—C26—H26B | 108.9 |
N3—Ru—N1 | 100.85 (7) | C27—C26—H26B | 108.9 |
N2—Ru—N1i | 79.15 (7) | H26A—C26—H26B | 107.7 |
N3—Ru—N1i | 100.85 (7) | C28—C27—C26 | 112 (2) |
N1—Ru—N1i | 158.29 (15) | C28—C27—H27A | 109.2 |
N2—Ru—P1i | 92.41 (2) | C26—C27—H27A | 109.2 |
N3—Ru—P1i | 87.59 (2) | C28—C27—H27B | 109.2 |
N1—Ru—P1i | 91.13 (7) | C26—C27—H27B | 109.2 |
N1i—Ru—P1i | 89.78 (7) | H27A—C27—H27B | 107.9 |
N2—Ru—P1 | 92.41 (2) | C27—C28—H28A | 109.5 |
N3—Ru—P1 | 87.59 (2) | C27—C28—H28B | 109.5 |
N1—Ru—P1 | 89.78 (7) | H28A—C28—H28B | 109.5 |
N1i—Ru—P1 | 91.13 (7) | C27—C28—H28C | 109.5 |
P1i—Ru—P1 | 175.19 (4) | H28A—C28—H28C | 109.5 |
C29—P1—C25' | 104.8 (18) | H28B—C28—H28C | 109.5 |
C29—P1—C21 | 105.1 (18) | C26'—C25'—P1 | 118.7 (18) |
C25'—P1—C21 | 92.5 (17) | C26'—C25'—H25C | 107.6 |
C29—P1—C21' | 94.2 (12) | P1—C25'—H25C | 107.6 |
C25'—P1—C21' | 105.6 (10) | C26'—C25'—H25D | 107.6 |
C29—P1—C25 | 105 (3) | P1—C25'—H25D | 107.6 |
C21—P1—C25 | 94 (2) | H25C—C25'—H25D | 107.1 |
C21'—P1—C25 | 107 (2) | C27'—C26'—C25' | 112.2 (13) |
C25'—P1—C29' | 104.4 (17) | C27'—C26'—H26C | 109.2 |
C21—P1—C29' | 114.0 (17) | C25'—C26'—H26C | 109.2 |
C21'—P1—C29' | 102.8 (11) | C27'—C26'—H26D | 109.2 |
C25—P1—C29' | 104 (3) | C25'—C26'—H26D | 109.2 |
C29—P1—Ru | 120.1 (13) | H26C—C26'—H26D | 107.9 |
C25'—P1—Ru | 114.7 (9) | C28'—C27'—C26' | 110.7 (17) |
C21—P1—Ru | 115.6 (15) | C28'—C27'—H27C | 109.5 |
C21'—P1—Ru | 114.7 (3) | C26'—C27'—H27C | 109.5 |
C25—P1—Ru | 113.4 (18) | C28'—C27'—H27D | 109.5 |
C29'—P1—Ru | 113.3 (11) | C26'—C27'—H27D | 109.5 |
C1—N1—C5 | 118.3 (3) | H27C—C27'—H27D | 108.1 |
C1—N1—Ru | 128.5 (2) | C27'—C28'—H28D | 109.5 |
C5—N1—Ru | 113.21 (19) | C27'—C28'—H28E | 109.5 |
C6i—N2—C6 | 120.5 (4) | H28D—C28'—H28E | 109.5 |
C6i—N2—Ru | 119.77 (19) | C27'—C28'—H28F | 109.5 |
C6—N2—Ru | 119.77 (19) | H28D—C28'—H28F | 109.5 |
C01—N3—Ru | 180.0 | H28E—C28'—H28F | 109.5 |
N1—C1—C2 | 122.3 (3) | C30—C29—P1 | 115 (2) |
N1—C1—H1A | 118.9 | C30—C29—H29A | 108.6 |
C2—C1—H1A | 118.9 | P1—C29—H29A | 108.6 |
C3—C2—C1 | 119.5 (3) | C30—C29—H29B | 108.6 |
C3—C2—H2A | 120.2 | P1—C29—H29B | 108.6 |
C1—C2—H2A | 120.2 | H29A—C29—H29B | 107.6 |
C2—C3—C4 | 119.3 (3) | C29—C30—C31 | 109.8 (15) |
C2—C3—H3A | 120.4 | C29—C30—H30A | 109.7 |
C4—C3—H3A | 120.4 | C31—C30—H30A | 109.7 |
C5—C4—C3 | 119.2 (3) | C29—C30—H30B | 109.7 |
C5—C4—H4A | 120.4 | C31—C30—H30B | 109.7 |
C3—C4—H4A | 120.4 | H30A—C30—H30B | 108.2 |
N1—C5—C4 | 121.5 (3) | C32—C31—C30 | 112.7 (15) |
N1—C5—C6 | 115.2 (3) | C32—C31—H31A | 109.1 |
C4—C5—C6 | 123.3 (3) | C30—C31—H31A | 109.1 |
N2—C6—C7 | 120.5 (3) | C32—C31—H31B | 109.1 |
N2—C6—C5 | 112.4 (3) | C30—C31—H31B | 109.1 |
C7—C6—C5 | 127.0 (3) | H31A—C31—H31B | 107.8 |
C6—C7—C8 | 120.5 (3) | C31—C32—H32A | 109.5 |
C6—C7—H7A | 119.8 | C31—C32—H32B | 109.5 |
C8—C7—H7A | 119.8 | H32A—C32—H32B | 109.5 |
C7i—C8—C7 | 117.5 (4) | C31—C32—H32C | 109.5 |
C7i—C8—C9 | 121.3 (2) | H32A—C32—H32C | 109.5 |
C7—C8—C9 | 121.3 (2) | H32B—C32—H32C | 109.5 |
C10—C9—C10i | 118.6 (5) | C30'—C29'—P1 | 117 (2) |
C10—C9—C8 | 120.7 (2) | C30'—C29'—H29C | 108.1 |
C10i—C9—C8 | 120.7 (2) | P1—C29'—H29C | 108.1 |
C9—C10—C11 | 120.6 (4) | C30'—C29'—H29D | 108.1 |
C9—C10—H10A | 119.7 | P1—C29'—H29D | 108.1 |
C11—C10—H10A | 119.7 | H29C—C29'—H29D | 107.3 |
C12—C11—C10 | 120.5 (5) | C29'—C30'—C31' | 112.3 (14) |
C12—C11—H11A | 119.7 | C29'—C30'—H30C | 109.1 |
C10—C11—H11A | 119.7 | C31'—C30'—H30C | 109.1 |
C11i—C12—C11 | 119.2 (6) | C29'—C30'—H30D | 109.1 |
C11i—C12—H12A | 120.4 | C31'—C30'—H30D | 109.1 |
C11—C12—H12A | 120.4 | H30C—C30'—H30D | 107.9 |
C22—C21—P1 | 124 (2) | C32'—C31'—C30' | 114.2 (14) |
C22—C21—H21A | 106.4 | C32'—C31'—H31C | 108.7 |
P1—C21—H21A | 106.4 | C30'—C31'—H31C | 108.7 |
C22—C21—H21B | 106.4 | C32'—C31'—H31D | 108.7 |
P1—C21—H21B | 106.4 | C30'—C31'—H31D | 108.7 |
H21A—C21—H21B | 106.5 | H31C—C31'—H31D | 107.6 |
C21—C22—C23 | 111 (2) | C31'—C32'—H32D | 109.5 |
C21—C22—H22A | 109.3 | C31'—C32'—H32E | 109.5 |
C23—C22—H22A | 109.3 | H32D—C32'—H32E | 109.5 |
C21—C22—H22B | 109.3 | C31'—C32'—H32F | 109.5 |
C23—C22—H22B | 109.3 | H32D—C32'—H32F | 109.5 |
H22A—C22—H22B | 108.0 | H32E—C32'—H32F | 109.5 |
C24—C23—C22 | 112 (2) | F6'—P2—F1' | 93.9 (12) |
C24—C23—H23A | 109.2 | F1—P2—F4 | 89.9 (5) |
C22—C23—H23A | 109.2 | F1—P2—F3 | 92.3 (4) |
C24—C23—H23B | 109.2 | F4—P2—F3 | 92.4 (5) |
C22—C23—H23B | 109.2 | F6'—P2—F2' | 91.6 (11) |
H23A—C23—H23B | 107.9 | F1'—P2—F2' | 88.8 (12) |
C23—C24—H24A | 109.5 | F6'—P2—F5' | 90.1 (12) |
C23—C24—H24B | 109.5 | F1'—P2—F5' | 175.4 (13) |
H24A—C24—H24B | 109.5 | F2'—P2—F5' | 88.8 (12) |
C23—C24—H24C | 109.5 | F6'—P2—F3' | 92.8 (10) |
H24A—C24—H24C | 109.5 | F1'—P2—F3' | 92.4 (13) |
H24B—C24—H24C | 109.5 | F2'—P2—F3' | 175.3 (13) |
C22'—C21'—P1 | 115.3 (5) | F5'—P2—F3' | 89.6 (12) |
C22'—C21'—H21C | 108.4 | F1—P2—F6 | 92.6 (5) |
P1—C21'—H21C | 108.4 | F4—P2—F6 | 177.1 (6) |
C22'—C21'—H21D | 108.4 | F3—P2—F6 | 89.0 (5) |
P1—C21'—H21D | 108.4 | F1—P2—F2 | 90.0 (4) |
H21C—C21'—H21D | 107.5 | F4—P2—F2 | 88.7 (5) |
C21'—C22'—C23' | 112.6 (6) | F3—P2—F2 | 177.4 (4) |
C21'—C22'—H22C | 109.1 | F6—P2—F2 | 89.9 (6) |
C23'—C22'—H22C | 109.1 | F1—P2—F5 | 178.3 (5) |
C21'—C22'—H22D | 109.1 | F4—P2—F5 | 91.2 (4) |
C23'—C22'—H22D | 109.1 | F3—P2—F5 | 88.9 (4) |
H22C—C22'—H22D | 107.8 | F6—P2—F5 | 86.3 (4) |
C24'—C23'—C22' | 112.4 (8) | F2—P2—F5 | 88.7 (4) |
C24'—C23'—H23C | 109.1 | F6'—P2—F4' | 179.2 (14) |
C22'—C23'—H23C | 109.1 | F1'—P2—F4' | 86.8 (11) |
C24'—C23'—H23D | 109.1 | F2'—P2—F4' | 88.2 (10) |
C22'—C23'—H23D | 109.1 | F5'—P2—F4' | 89.2 (12) |
H23C—C23'—H23D | 107.9 | F3'—P2—F4' | 87.4 (11) |
C23'—C24'—H24D | 109.5 | N3—C01—C02 | 180.000 (1) |
C23'—C24'—H24E | 109.5 | C01—C02—H02A | 109.5 |
H24D—C24'—H24E | 109.5 | C01—C02—H02B | 109.5 |
C23'—C24'—H24F | 109.5 | H02A—C02—H02B | 109.5 |
H24D—C24'—H24F | 109.5 | C01—C02—H02C | 109.5 |
H24E—C24'—H24F | 109.5 | H02A—C02—H02C | 109.5 |
C26—C25—P1 | 113 (4) | H02B—C02—H02C | 109.5 |
C26—C25—H25A | 109.0 | C03ii—Cl2—C03 | 102.7 (11) |
P1—C25—H25A | 109.0 | C03ii—Cl2—Cl2ii | 55.0 (7) |
C26—C25—H25B | 109.0 | C03—Cl2—Cl2ii | 47.6 (8) |
P1—C25—H25B | 109.0 | Cl2ii—C03—Cl1 | 153 (2) |
H25A—C25—H25B | 107.8 | Cl2ii—C03—Cl2 | 77.3 (11) |
C25—C26—C27 | 114 (2) | Cl1—C03—Cl2 | 107.2 (9) |
C25—C26—H26A | 108.9 |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y+1, −z. |