Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030674/bv2024sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030674/bv2024Isup2.hkl |
CCDC reference: 620705
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å Some non-H atoms missing
- Disorder in solvent or counterion
- R factor = 0.052
- wR factor = 0.140
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level A ABSMU01_ALERT_1_A The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 0.256 Value of mu given = 0.511 CHEMW01_ALERT_1_A The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.90 <> 1.10 Calculated formula weight = 1735.6390 Formula weight given = 867.8100 CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 867.81 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 176.00 2113.94 H 1.01 134.00 135.07 N 14.01 30.00 420.21 O 16.00 16.00 255.98 Ru 101.07 4.00 404.28 Cl 35.45 4.00 141.81 Calculated formula weight 3471.29 DENSD01_ALERT_1_A The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.90 <> 1.10 Crystal density given = 1.438 Calculated crystal density = 0.360 PLAT043_ALERT_1_A Check Reported Molecular Weight ................ 867.81 PLAT046_ALERT_1_A Reported Z, MW and D(calc) are Inconsistent .... 0.36
Alert level C CHEMW01_ALERT_1_C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 12.00 Perc.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C88 H67 Cl2 N15 O8 Ru2 Atom count from _chemical_formula_moiety: 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:C88 H67 Cl2 N15 O8 Ru2 Atom count from the _atom_site data: C176 H134 Cl4 N30 O16 Ru4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C88 H67 Cl2 N15 O8 Ru2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 176.00 352.00 -176.00 H 134.00 268.00 -134.00 Cl 4.00 8.00 -4.00 N 30.00 60.00 -30.00 O 16.00 32.00 -16.00 Ru 4.00 8.00 -4.00
6 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2000); cell refinement: SAINT-Plus (Bruker, 2000); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ru(C12H8N2)2(C12H8N3)]ClO4·C7H8·0.5C2H3N | F(000) = 3544 |
Mr = 867.81 | Dx = 1.438 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1344 reflections |
a = 26.014 (11) Å | θ = 2.1–25.4° |
b = 10.050 (4) Å | µ = 0.51 mm−1 |
c = 30.708 (13) Å | T = 298 K |
β = 93.223 (7)° | Block, red |
V = 8016 (6) Å3 | 0.32 × 0.26 × 0.24 mm |
Z = 2 |
Bruker SMART APEX CCD area-detector diffractometer | 7888 independent reflections |
Radiation source: sealed tube | 6398 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 26.0°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −31→32 |
Tmin = 0.854, Tmax = 0.887 | k = −12→12 |
21776 measured reflections | l = −37→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)] = 0.052 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.140 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + (0.07P)2 + 1.99P] where P = (Fo2 + 2Fc2)/3 |
7888 reflections | (Δ/σ)max < 0.001 |
530 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.89 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) | |
C1 | 0.29755 (13) | 0.5286 (4) | 0.08398 (13) | 0.0502 (9) | |
H1 | 0.2883 | 0.5001 | 0.1113 | 0.060* | |
C2 | 0.25804 (15) | 0.5500 (4) | 0.05075 (13) | 0.0536 (9) | |
H2 | 0.2237 | 0.5325 | 0.0554 | 0.064* | |
C3 | 0.27295 (15) | 0.5976 (4) | 0.01158 (14) | 0.0581 (10) | |
H3 | 0.2480 | 0.6153 | −0.0105 | 0.070* | |
C4 | 0.32718 (15) | 0.6213 (4) | 0.00364 (12) | 0.0539 (9) | |
C5 | 0.34411 (15) | 0.6694 (4) | −0.03593 (14) | 0.0614 (11) | |
H5 | 0.3206 | 0.6855 | −0.0593 | 0.074* | |
C6 | 0.39629 (14) | 0.6929 (4) | −0.04002 (12) | 0.0534 (9) | |
H6 | 0.4076 | 0.7265 | −0.0660 | 0.064* | |
C7 | 0.43136 (14) | 0.6664 (4) | −0.00560 (12) | 0.0484 (8) | |
C8 | 0.48513 (14) | 0.6886 (4) | −0.00678 (12) | 0.0515 (9) | |
H8 | 0.4986 | 0.7188 | −0.0324 | 0.062* | |
C9 | 0.51687 (13) | 0.6668 (3) | 0.02839 (11) | 0.0417 (7) | |
H9 | 0.5517 | 0.6867 | 0.0275 | 0.050* | |
C10 | 0.49742 (13) | 0.6131 (3) | 0.06736 (11) | 0.0451 (7) | |
H10 | 0.5201 | 0.5980 | 0.0913 | 0.054* | |
C11 | 0.41458 (14) | 0.6180 (4) | 0.03377 (13) | 0.0550 (9) | |
C12 | 0.36231 (15) | 0.5959 (4) | 0.03841 (12) | 0.0555 (9) | |
C13 | 0.41668 (14) | 0.7956 (4) | 0.14924 (13) | 0.0518 (8) | |
H13 | 0.4366 | 0.8109 | 0.1255 | 0.062* | |
C14 | 0.40731 (16) | 0.9036 (4) | 0.17733 (13) | 0.0579 (9) | |
H14 | 0.4225 | 0.9861 | 0.1733 | 0.069* | |
C15 | 0.37636 (15) | 0.8838 (4) | 0.20948 (13) | 0.0561 (9) | |
H15 | 0.3672 | 0.9569 | 0.2260 | 0.067* | |
C16 | 0.35666 (13) | 0.7596 (4) | 0.22006 (12) | 0.0509 (9) | |
C17 | 0.32513 (14) | 0.7287 (4) | 0.25454 (13) | 0.0516 (9) | |
H17 | 0.3157 | 0.7979 | 0.2725 | 0.062* | |
C18 | 0.30770 (14) | 0.6060 (4) | 0.26322 (12) | 0.0525 (9) | |
H18 | 0.2880 | 0.5910 | 0.2871 | 0.063* | |
C19 | 0.32026 (14) | 0.4976 (3) | 0.23449 (12) | 0.0477 (8) | |
C20 | 0.30457 (15) | 0.3676 (4) | 0.23760 (11) | 0.0510 (9) | |
H20 | 0.2846 | 0.3418 | 0.2603 | 0.061* | |
C21 | 0.31842 (14) | 0.2744 (4) | 0.20689 (12) | 0.0510 (9) | |
H21 | 0.3064 | 0.1876 | 0.2088 | 0.061* | |
C22 | 0.34844 (14) | 0.3062 (4) | 0.17487 (12) | 0.0511 (8) | |
H22 | 0.3580 | 0.2398 | 0.1559 | 0.061* | |
C23 | 0.35078 (13) | 0.5258 (3) | 0.19887 (12) | 0.0430 (7) | |
C24 | 0.36922 (12) | 0.6552 (3) | 0.19107 (10) | 0.0402 (7) | |
C25 | 0.50251 (16) | 0.5120 (4) | 0.17800 (14) | 0.0546 (9) | |
H25 | 0.4974 | 0.6032 | 0.1750 | 0.066* | |
C26 | 0.54510 (15) | 0.4632 (4) | 0.20863 (13) | 0.0539 (9) | |
H26 | 0.5597 | 0.5156 | 0.2310 | 0.065* | |
C27 | 0.56119 (15) | 0.3338 (4) | 0.20120 (13) | 0.0578 (9) | |
H27 | 0.5902 | 0.2995 | 0.2164 | 0.069* | |
C28 | 0.53429 (14) | 0.2591 (4) | 0.17176 (12) | 0.0516 (8) | |
H28 | 0.5445 | 0.1724 | 0.1661 | 0.062* | |
C29 | 0.49143 (13) | 0.3126 (4) | 0.15005 (12) | 0.0485 (8) | |
C30 | 0.46086 (13) | 0.2452 (3) | 0.11370 (12) | 0.0469 (8) | |
C31 | 0.43149 (15) | 0.1147 (4) | 0.06469 (13) | 0.0551 (9) | |
C32 | 0.42182 (16) | 0.0113 (4) | 0.03417 (14) | 0.0540 (9) | |
H32 | 0.4404 | −0.0677 | 0.0360 | 0.065* | |
C33 | 0.38489 (15) | 0.0307 (4) | 0.00238 (13) | 0.0527 (9) | |
H33 | 0.3790 | −0.0353 | −0.0185 | 0.063* | |
C34 | 0.35503 (14) | 0.1467 (4) | −0.00037 (13) | 0.0543 (9) | |
H34 | 0.3284 | 0.1526 | −0.0218 | 0.065* | |
C35 | 0.36358 (15) | 0.2488 (4) | 0.02672 (13) | 0.0552 (9) | |
H35 | 0.3449 | 0.3275 | 0.0235 | 0.066* | |
C36 | 0.40275 (15) | 0.2327 (4) | 0.06104 (14) | 0.0560 (9) | |
C37 | 0.19044 (13) | 0.0610 (4) | 0.11880 (12) | 0.0459 (8) | |
C38 | 0.22358 (14) | 0.1444 (4) | 0.09942 (12) | 0.0506 (8) | |
H38 | 0.2123 | 0.2277 | 0.0898 | 0.061* | |
C39 | 0.27457 (13) | 0.1056 (4) | 0.09388 (11) | 0.0464 (8) | |
H39 | 0.2968 | 0.1621 | 0.0801 | 0.056* | |
C40 | 0.29179 (14) | −0.0190 (4) | 0.10927 (13) | 0.0507 (9) | |
H40 | 0.3259 | −0.0439 | 0.1065 | 0.061* | |
C41 | 0.25849 (13) | −0.1043 (4) | 0.12838 (11) | 0.0491 (8) | |
H41 | 0.2694 | −0.1885 | 0.1374 | 0.059* | |
C42 | 0.20817 (14) | −0.0634 (4) | 0.13415 (12) | 0.0503 (8) | |
H42 | 0.1860 | −0.1191 | 0.1484 | 0.060* | |
C43 | 0.13757 (14) | 0.1045 (4) | 0.12270 (14) | 0.0586 (10) | |
H43A | 0.1344 | 0.1457 | 0.1506 | 0.088* | |
H43B | 0.1150 | 0.0290 | 0.1200 | 0.088* | |
H43C | 0.1285 | 0.1673 | 0.1000 | 0.088* | |
C44 | 0.5505 (2) | 0.8855 (7) | 0.1957 (2) | 0.0422 (14) | 0.50 |
H44A | 0.5571 | 0.8333 | 0.1704 | 0.063* | 0.50 |
H44B | 0.5824 | 0.9202 | 0.2082 | 0.063* | 0.50 |
H44C | 0.5279 | 0.9578 | 0.1874 | 0.063* | 0.50 |
C45 | 0.5267 (2) | 0.8030 (8) | 0.2273 (3) | 0.0515 (17) | 0.50 |
Cl1 | 0.32889 (4) | 0.04541 (10) | 0.34075 (3) | 0.0541 (2) | |
N1 | 0.34790 (12) | 0.5478 (3) | 0.07755 (11) | 0.0547 (8) | |
N2 | 0.44774 (12) | 0.5839 (3) | 0.07032 (10) | 0.0542 (8) | |
N3 | 0.39887 (10) | 0.6758 (3) | 0.15484 (9) | 0.0425 (6) | |
N4 | 0.36533 (10) | 0.4300 (3) | 0.16891 (9) | 0.0426 (6) | |
N5 | 0.47527 (11) | 0.4397 (3) | 0.15759 (10) | 0.0483 (7) | |
N6 | 0.42144 (11) | 0.3153 (3) | 0.09387 (11) | 0.0553 (8) | |
N7 | 0.46908 (13) | 0.1248 (3) | 0.09902 (11) | 0.0569 (8) | |
N8 | 0.5000 | 0.7402 (5) | 0.2500 | 0.0535 (11) | |
O1 | 0.35012 (9) | 0.1132 (2) | 0.37188 (8) | 0.0449 (5) | |
O2 | 0.28098 (9) | 0.0751 (2) | 0.33514 (8) | 0.0479 (6) | |
O3 | 0.35120 (10) | 0.0716 (3) | 0.30610 (9) | 0.0585 (7) | |
O4 | 0.33411 (11) | −0.0814 (3) | 0.35070 (9) | 0.0605 (7) | |
Ru1 | 0.409362 (10) | 0.50139 (3) | 0.120246 (9) | 0.04328 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0348 (16) | 0.056 (2) | 0.058 (2) | 0.0025 (14) | −0.0135 (15) | 0.0126 (17) |
C2 | 0.052 (2) | 0.0509 (19) | 0.056 (2) | −0.0081 (16) | −0.0143 (17) | −0.0078 (17) |
C3 | 0.051 (2) | 0.056 (2) | 0.065 (2) | −0.0095 (17) | −0.0187 (18) | 0.0033 (18) |
C4 | 0.060 (2) | 0.050 (2) | 0.0496 (19) | −0.0179 (16) | −0.0182 (17) | 0.0077 (16) |
C5 | 0.057 (2) | 0.058 (2) | 0.068 (2) | −0.0269 (18) | −0.0135 (19) | 0.0180 (19) |
C6 | 0.056 (2) | 0.065 (2) | 0.0380 (17) | −0.0121 (17) | −0.0049 (15) | 0.0092 (16) |
C7 | 0.0539 (19) | 0.0464 (19) | 0.0466 (19) | −0.0093 (15) | 0.0169 (15) | 0.0042 (15) |
C8 | 0.0534 (19) | 0.057 (2) | 0.0469 (19) | 0.0116 (17) | 0.0250 (16) | 0.0173 (16) |
C9 | 0.0496 (17) | 0.0335 (15) | 0.0427 (17) | −0.0052 (13) | 0.0075 (14) | 0.0055 (13) |
C10 | 0.0495 (18) | 0.0370 (17) | 0.0475 (18) | 0.0037 (13) | −0.0093 (15) | 0.0053 (14) |
C11 | 0.050 (2) | 0.064 (2) | 0.052 (2) | 0.0094 (17) | 0.0112 (16) | −0.0031 (18) |
C12 | 0.067 (2) | 0.057 (2) | 0.0444 (19) | 0.0221 (18) | 0.0188 (17) | 0.0118 (17) |
C13 | 0.053 (2) | 0.050 (2) | 0.054 (2) | −0.0112 (16) | 0.0116 (16) | −0.0025 (16) |
C14 | 0.067 (2) | 0.054 (2) | 0.052 (2) | −0.0038 (18) | −0.0052 (18) | 0.0054 (17) |
C15 | 0.061 (2) | 0.052 (2) | 0.056 (2) | 0.0126 (17) | 0.0113 (18) | −0.0118 (17) |
C16 | 0.0449 (18) | 0.056 (2) | 0.052 (2) | −0.0055 (15) | 0.0088 (15) | −0.0201 (17) |
C17 | 0.0495 (19) | 0.052 (2) | 0.054 (2) | 0.0138 (16) | 0.0110 (16) | −0.0108 (17) |
C18 | 0.0502 (19) | 0.061 (2) | 0.0452 (18) | −0.0138 (17) | −0.0038 (15) | 0.0040 (16) |
C19 | 0.0453 (19) | 0.055 (2) | 0.0428 (19) | −0.0107 (14) | 0.0041 (15) | −0.0101 (15) |
C20 | 0.061 (2) | 0.057 (2) | 0.0352 (17) | −0.0129 (17) | 0.0054 (15) | 0.0134 (16) |
C21 | 0.058 (2) | 0.0449 (18) | 0.0478 (19) | −0.0159 (16) | −0.0176 (16) | 0.0130 (15) |
C22 | 0.055 (2) | 0.048 (2) | 0.052 (2) | 0.0020 (16) | 0.0180 (16) | −0.0103 (16) |
C23 | 0.0424 (17) | 0.0438 (17) | 0.0434 (18) | −0.0016 (13) | 0.0061 (14) | −0.0038 (14) |
C24 | 0.0389 (15) | 0.0477 (18) | 0.0340 (15) | −0.0088 (13) | 0.0016 (12) | 0.0046 (13) |
C25 | 0.053 (2) | 0.054 (2) | 0.058 (2) | 0.0044 (16) | 0.0168 (18) | −0.0133 (17) |
C26 | 0.052 (2) | 0.054 (2) | 0.055 (2) | −0.0117 (17) | −0.0087 (17) | −0.0020 (17) |
C27 | 0.056 (2) | 0.063 (2) | 0.053 (2) | 0.0124 (18) | −0.0027 (17) | 0.0092 (18) |
C28 | 0.0534 (19) | 0.0477 (19) | 0.055 (2) | 0.0051 (16) | 0.0154 (17) | −0.0098 (16) |
C29 | 0.0437 (17) | 0.052 (2) | 0.0504 (19) | −0.0043 (15) | 0.0087 (15) | −0.0077 (16) |
C30 | 0.0473 (18) | 0.0448 (18) | 0.0497 (19) | −0.0085 (14) | 0.0117 (15) | 0.0060 (15) |
C31 | 0.054 (2) | 0.057 (2) | 0.054 (2) | 0.0075 (17) | −0.0008 (17) | 0.0068 (17) |
C32 | 0.055 (2) | 0.051 (2) | 0.057 (2) | 0.0124 (16) | 0.0212 (18) | 0.0133 (16) |
C33 | 0.059 (2) | 0.0477 (19) | 0.053 (2) | 0.0000 (16) | 0.0186 (18) | −0.0125 (17) |
C34 | 0.052 (2) | 0.052 (2) | 0.057 (2) | 0.0086 (16) | −0.0136 (17) | 0.0109 (17) |
C35 | 0.056 (2) | 0.058 (2) | 0.050 (2) | 0.0107 (17) | −0.0085 (17) | 0.0126 (18) |
C36 | 0.053 (2) | 0.053 (2) | 0.062 (2) | 0.0130 (17) | 0.0105 (18) | 0.0098 (18) |
C37 | 0.0444 (18) | 0.0431 (18) | 0.0494 (19) | 0.0044 (14) | −0.0042 (14) | 0.0054 (15) |
C38 | 0.055 (2) | 0.052 (2) | 0.0452 (18) | 0.0019 (16) | 0.0124 (16) | 0.0097 (16) |
C39 | 0.0413 (17) | 0.058 (2) | 0.0402 (17) | −0.0016 (15) | −0.0004 (14) | −0.0024 (15) |
C40 | 0.0387 (17) | 0.061 (2) | 0.052 (2) | 0.0025 (15) | 0.0007 (15) | −0.0074 (17) |
C41 | 0.0433 (17) | 0.062 (2) | 0.0421 (18) | 0.0050 (16) | 0.0073 (14) | 0.0006 (16) |
C42 | 0.054 (2) | 0.054 (2) | 0.0434 (18) | 0.0051 (16) | 0.0085 (15) | 0.0068 (16) |
C43 | 0.056 (2) | 0.064 (2) | 0.059 (2) | −0.0050 (18) | 0.0249 (18) | −0.0043 (19) |
C44 | 0.035 (3) | 0.055 (4) | 0.036 (3) | −0.001 (3) | 0.001 (2) | 0.001 (3) |
C45 | 0.036 (3) | 0.057 (4) | 0.060 (4) | 0.005 (3) | −0.007 (3) | 0.010 (4) |
Cl1 | 0.0572 (5) | 0.0498 (5) | 0.0536 (5) | 0.0087 (4) | −0.0111 (4) | 0.0033 (4) |
N1 | 0.0521 (17) | 0.0517 (17) | 0.0584 (19) | −0.0150 (14) | −0.0141 (14) | 0.0104 (15) |
N2 | 0.0577 (17) | 0.0504 (17) | 0.0523 (17) | −0.0193 (14) | −0.0154 (14) | 0.0075 (14) |
N3 | 0.0375 (13) | 0.0504 (16) | 0.0398 (14) | −0.0118 (12) | 0.0049 (11) | −0.0102 (12) |
N4 | 0.0338 (13) | 0.0520 (17) | 0.0421 (14) | −0.0109 (11) | 0.0049 (11) | −0.0107 (13) |
N5 | 0.0488 (16) | 0.0500 (17) | 0.0477 (16) | −0.0094 (13) | 0.0162 (13) | 0.0041 (14) |
N6 | 0.0471 (16) | 0.063 (2) | 0.0566 (18) | 0.0088 (14) | 0.0115 (14) | −0.0018 (15) |
N7 | 0.0637 (19) | 0.0529 (18) | 0.0558 (18) | 0.0184 (15) | 0.0183 (15) | 0.0107 (15) |
N8 | 0.049 (2) | 0.060 (3) | 0.054 (3) | 0.000 | 0.024 (2) | 0.000 |
O1 | 0.0545 (13) | 0.0359 (12) | 0.0444 (12) | 0.0039 (10) | 0.0035 (11) | −0.0046 (10) |
O2 | 0.0507 (13) | 0.0422 (13) | 0.0496 (13) | −0.0040 (10) | −0.0072 (11) | −0.0075 (10) |
O3 | 0.0619 (16) | 0.0615 (17) | 0.0525 (15) | 0.0024 (13) | 0.0069 (12) | −0.0012 (13) |
O4 | 0.0687 (17) | 0.0607 (17) | 0.0517 (15) | 0.0021 (14) | −0.0009 (13) | 0.0004 (13) |
Ru1 | 0.03818 (17) | 0.04696 (19) | 0.04389 (18) | −0.01199 (10) | −0.00482 (12) | 0.00589 (11) |
C1—N1 | 1.349 (5) | C26—H26 | 0.9300 |
C1—C2 | 1.424 (5) | C27—C28 | 1.342 (6) |
C1—H1 | 0.9300 | C27—H27 | 0.9300 |
C2—C3 | 1.370 (6) | C28—C29 | 1.376 (5) |
C2—H2 | 0.9300 | C28—H28 | 0.9300 |
C3—C4 | 1.465 (5) | C29—N5 | 1.368 (5) |
C3—H3 | 0.9300 | C29—C30 | 1.496 (5) |
C4—C12 | 1.390 (5) | C30—N7 | 1.313 (5) |
C4—C5 | 1.401 (6) | C30—N6 | 1.359 (5) |
C5—C6 | 1.390 (5) | C31—N7 | 1.401 (5) |
C5—H5 | 0.9300 | C31—C36 | 1.403 (5) |
C6—C7 | 1.383 (5) | C31—C32 | 1.412 (6) |
C6—H6 | 0.9300 | C32—C33 | 1.345 (6) |
C7—C11 | 1.396 (5) | C32—H32 | 0.9300 |
C7—C8 | 1.419 (5) | C33—C34 | 1.401 (5) |
C8—C9 | 1.340 (5) | C33—H33 | 0.9300 |
C8—H8 | 0.9300 | C34—C35 | 1.332 (6) |
C9—C10 | 1.431 (5) | C34—H34 | 0.9300 |
C9—H9 | 0.9300 | C35—C36 | 1.433 (5) |
C10—N2 | 1.333 (5) | C35—H35 | 0.9300 |
C10—H10 | 0.9300 | C36—N6 | 1.373 (5) |
C11—C12 | 1.393 (5) | C37—C38 | 1.363 (5) |
C11—N2 | 1.418 (5) | C37—C42 | 1.404 (5) |
C12—N1 | 1.368 (5) | C37—C43 | 1.454 (5) |
C13—N3 | 1.305 (4) | C38—C39 | 1.402 (5) |
C13—C14 | 1.416 (5) | C38—H38 | 0.9300 |
C13—H13 | 0.9300 | C39—C40 | 1.403 (5) |
C14—C15 | 1.323 (6) | C39—H39 | 0.9300 |
C14—H14 | 0.9300 | C40—C41 | 1.374 (5) |
C15—C16 | 1.395 (6) | C40—H40 | 0.9300 |
C15—H15 | 0.9300 | C41—C42 | 1.393 (5) |
C16—C17 | 1.410 (5) | C41—H41 | 0.9300 |
C16—C24 | 1.426 (5) | C42—H42 | 0.9300 |
C17—C18 | 1.346 (5) | C43—H43A | 0.9600 |
C17—H17 | 0.9300 | C43—H43B | 0.9600 |
C18—C19 | 1.451 (5) | C43—H43C | 0.9600 |
C18—H18 | 0.9300 | C44—C45 | 1.443 (10) |
C19—C20 | 1.373 (5) | C44—H44A | 0.9600 |
C19—C23 | 1.416 (5) | C44—H44B | 0.9600 |
C20—C21 | 1.391 (6) | C44—H44C | 0.9600 |
C20—H20 | 0.9300 | C45—N8 | 1.193 (8) |
C21—C22 | 1.329 (5) | Cl1—O3 | 1.268 (3) |
C21—H21 | 0.9300 | Cl1—O1 | 1.274 (3) |
C22—N4 | 1.336 (5) | Cl1—O2 | 1.284 (3) |
C22—H22 | 0.9300 | Cl1—O4 | 1.316 (3) |
C23—N4 | 1.399 (4) | N1—Ru1 | 2.063 (3) |
C23—C24 | 1.411 (5) | N2—Ru1 | 2.051 (3) |
C24—N3 | 1.404 (4) | N3—Ru1 | 2.075 (3) |
C25—N5 | 1.172 (5) | N4—Ru1 | 2.062 (3) |
C25—C26 | 1.495 (6) | N5—Ru1 | 2.102 (3) |
C25—H25 | 0.9300 | N6—Ru1 | 2.069 (3) |
C26—C27 | 1.389 (6) | N8—C45i | 1.193 (8) |
N1—C1—C2 | 122.8 (4) | N7—C31—C32 | 130.1 (3) |
N1—C1—H1 | 118.6 | C36—C31—C32 | 119.7 (4) |
C2—C1—H1 | 118.6 | C33—C32—C31 | 117.9 (3) |
C3—C2—C1 | 117.0 (4) | C33—C32—H32 | 121.0 |
C3—C2—H2 | 121.5 | C31—C32—H32 | 121.0 |
C1—C2—H2 | 121.5 | C32—C33—C34 | 122.4 (4) |
C2—C3—C4 | 121.7 (3) | C32—C33—H33 | 118.8 |
C2—C3—H3 | 119.1 | C34—C33—H33 | 118.8 |
C4—C3—H3 | 119.1 | C35—C34—C33 | 122.1 (3) |
C12—C4—C5 | 120.3 (4) | C35—C34—H34 | 119.0 |
C12—C4—C3 | 116.1 (3) | C33—C34—H34 | 119.0 |
C5—C4—C3 | 123.6 (3) | C34—C35—C36 | 117.3 (3) |
C6—C5—C4 | 119.5 (4) | C34—C35—H35 | 121.3 |
C6—C5—H5 | 120.2 | C36—C35—H35 | 121.3 |
C4—C5—H5 | 120.2 | N6—C36—C31 | 106.7 (3) |
C7—C6—C5 | 120.3 (3) | N6—C36—C35 | 132.8 (4) |
C7—C6—H6 | 119.9 | C31—C36—C35 | 120.5 (4) |
C5—C6—H6 | 119.9 | C38—C37—C42 | 119.4 (3) |
C6—C7—C11 | 120.3 (3) | C38—C37—C43 | 118.4 (3) |
C6—C7—C8 | 124.0 (3) | C42—C37—C43 | 122.3 (3) |
C11—C7—C8 | 115.7 (3) | C37—C38—C39 | 120.5 (3) |
C9—C8—C7 | 121.2 (3) | C37—C38—H38 | 119.8 |
C9—C8—H8 | 119.4 | C39—C38—H38 | 119.8 |
C7—C8—H8 | 119.4 | C38—C39—C40 | 119.6 (3) |
C8—C9—C10 | 120.3 (3) | C38—C39—H39 | 120.2 |
C8—C9—H9 | 119.8 | C40—C39—H39 | 120.2 |
C10—C9—H9 | 119.8 | C41—C40—C39 | 120.3 (3) |
N2—C10—C9 | 122.0 (3) | C41—C40—H40 | 119.9 |
N2—C10—H10 | 119.0 | C39—C40—H40 | 119.9 |
C9—C10—H10 | 119.0 | C40—C41—C42 | 119.3 (4) |
C12—C11—C7 | 119.9 (4) | C40—C41—H41 | 120.3 |
C12—C11—N2 | 115.8 (3) | C42—C41—H41 | 120.3 |
C7—C11—N2 | 124.3 (3) | C41—C42—C37 | 120.9 (3) |
N1—C12—C4 | 122.7 (4) | C41—C42—H42 | 119.6 |
N1—C12—C11 | 117.6 (4) | C37—C42—H42 | 119.6 |
C4—C12—C11 | 119.7 (3) | C37—C43—H43A | 109.5 |
N3—C13—C14 | 123.5 (3) | C37—C43—H43B | 109.5 |
N3—C13—H13 | 118.2 | H43A—C43—H43B | 109.5 |
C14—C13—H13 | 118.2 | C37—C43—H43C | 109.5 |
C15—C14—C13 | 118.2 (4) | H43A—C43—H43C | 109.5 |
C15—C14—H14 | 120.9 | H43B—C43—H43C | 109.5 |
C13—C14—H14 | 120.9 | C45—C44—H44A | 109.5 |
C14—C15—C16 | 123.7 (4) | C45—C44—H44B | 109.5 |
C14—C15—H15 | 118.2 | H44A—C44—H44B | 109.5 |
C16—C15—H15 | 118.2 | C45—C44—H44C | 109.5 |
C15—C16—C17 | 127.5 (3) | H44A—C44—H44C | 109.5 |
C15—C16—C24 | 114.4 (3) | H44B—C44—H44C | 109.5 |
C17—C16—C24 | 118.1 (3) | N8—C45—C44 | 169.8 (6) |
C18—C17—C16 | 124.5 (3) | C44—C45—C45i | 143.3 (4) |
C18—C17—H17 | 117.7 | O3—Cl1—O1 | 108.60 (18) |
C16—C17—H17 | 117.7 | O3—Cl1—O2 | 109.02 (18) |
C17—C18—C19 | 118.6 (3) | O1—Cl1—O2 | 110.65 (16) |
C17—C18—H18 | 120.7 | O3—Cl1—O4 | 110.49 (19) |
C19—C18—H18 | 120.7 | O1—Cl1—O4 | 107.98 (17) |
C20—C19—C23 | 115.2 (3) | O2—Cl1—O4 | 110.08 (18) |
C20—C19—C18 | 126.5 (3) | C1—N1—C12 | 119.7 (3) |
C23—C19—C18 | 118.3 (3) | C1—N1—Ru1 | 126.8 (3) |
C19—C20—C21 | 120.3 (3) | C12—N1—Ru1 | 113.4 (3) |
C19—C20—H20 | 119.9 | C10—N2—C11 | 116.2 (3) |
C21—C20—H20 | 119.9 | C10—N2—Ru1 | 130.9 (2) |
C22—C21—C20 | 121.7 (3) | C11—N2—Ru1 | 112.9 (2) |
C22—C21—H21 | 119.2 | C13—N3—C24 | 117.1 (3) |
C20—C21—H21 | 119.2 | C13—N3—Ru1 | 130.8 (2) |
C21—C22—N4 | 122.5 (3) | C24—N3—Ru1 | 112.0 (2) |
C21—C22—H22 | 118.7 | C22—N4—C23 | 116.6 (3) |
N4—C22—H22 | 118.7 | C22—N4—Ru1 | 128.6 (2) |
N4—C23—C24 | 114.5 (3) | C23—N4—Ru1 | 114.8 (2) |
N4—C23—C19 | 123.7 (3) | C25—N5—C29 | 119.1 (4) |
C24—C23—C19 | 121.8 (3) | C25—N5—Ru1 | 124.0 (3) |
N3—C24—C23 | 118.5 (3) | C29—N5—Ru1 | 115.6 (2) |
N3—C24—C16 | 122.8 (3) | C30—N6—C36 | 104.1 (3) |
C23—C24—C16 | 118.7 (3) | C30—N6—Ru1 | 114.8 (3) |
N5—C25—C26 | 122.5 (4) | C36—N6—Ru1 | 141.1 (3) |
N5—C25—H25 | 118.7 | C30—N7—C31 | 101.9 (3) |
C26—C25—H25 | 118.7 | C45—N8—C45i | 116.1 (8) |
C27—C26—C25 | 115.0 (3) | N2—Ru1—N4 | 174.78 (12) |
C27—C26—H26 | 122.5 | N2—Ru1—N1 | 79.98 (13) |
C25—C26—H26 | 122.5 | N4—Ru1—N1 | 95.56 (12) |
C28—C27—C26 | 119.0 (4) | N2—Ru1—N6 | 88.98 (13) |
C28—C27—H27 | 120.5 | N4—Ru1—N6 | 94.13 (12) |
C26—C27—H27 | 120.5 | N1—Ru1—N6 | 94.86 (13) |
C27—C28—C29 | 119.0 (3) | N2—Ru1—N3 | 97.15 (12) |
C27—C28—H28 | 120.5 | N4—Ru1—N3 | 80.12 (11) |
C29—C28—H28 | 120.5 | N1—Ru1—N3 | 90.86 (13) |
N5—C29—C28 | 122.1 (3) | N6—Ru1—N3 | 172.27 (12) |
N5—C29—C30 | 113.2 (3) | N2—Ru1—N5 | 96.36 (12) |
C28—C29—C30 | 124.5 (3) | N4—Ru1—N5 | 88.36 (11) |
N7—C30—N6 | 117.2 (3) | N1—Ru1—N5 | 172.99 (13) |
N7—C30—C29 | 125.7 (3) | N6—Ru1—N5 | 79.02 (13) |
N6—C30—C29 | 117.1 (3) | N3—Ru1—N5 | 95.55 (12) |
N7—C31—C36 | 110.2 (4) |
Symmetry code: (i) −x+1, y, −z+1/2. |