A cluster containing a pyrazole ligand: [Ru3(μ-H)(μ-N2C3H3)(CO)10]

Diz, E.L.; Neels, A.; Therrien, B.; Stoeckli-Evans, H.; Süss-Fink, G.

doi:10.1107/S1600536802002957

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A cluster containing a pyrazole ligand: [Ru₃(μ-H)(μ-N₂C₃H₃)(CO)₁₀]

E. L. Diz, A. Neels, B. Therrien, H. Stoeckli-Evans and G. Süss-Fink

The title cluster decacarbonyl-1κ⁴C,2κ³C,3κ³C-μ-hydrido-2:3κ²H:H-μ-pyrazolyl-2:3κ²N¹:N²-triangulo-triruthenium, (I), [Ru₃(μ-H)(μ-C₃H₃N₂)(CO)₁₀], which contains a pyrazole ligand, has been synthesized and characterized, both spectroscopically and crystalographically, as a cyclohexane solvate. The molecular structure of (I) is very similar to that of the known dimethylpyrazole derivative [Ru₃(μ-H){μ-N₂C₃H(CH₃)₂-3,5}(CO)₁₀].

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802002957/tk6053sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536802002957/tk6053Isup2.hkl Contains datablock I

CCDC reference: 182584

checkCIF report

Key indicators

Single-crystal X-ray study
T = 153 K
Mean (C-C) = 0.022 Å
R factor = 0.041
wR factor = 0.107
Data-to-parameter ratio = 8.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level A:



THETM_01  Alert A The value of sine(theta_max)/wavelength is less than 0.550
          Calculated sin(theta_max)/wavelength =    0.5348

Author response: The very long axes c forced the measurement to be done with the detector at 90mm.


 Alert Level B:



PLAT_360  Alert B Short  C(sp3)-C(sp3) Bond  C(27)  -   C(28)  =       1.29 Ang.

Author response: The half molecule of hexane is disordered, and the short distance, only reflect that.


 Alert Level C:



REFNR_01  Alert C Ratio of reflections to parameters is < 10 for a
          centrosymmetric structure
          sine(theta)/lambda                0.5348
          Proportion of unique data used    1.0000
          Ratio reflections to parameters   8.9154

PLAT_360  Alert C Short  C(sp3)-C(sp3) Bond  C(27)  -   C(29)a =       1.42 Ang.

PLAT_360  Alert C Short  C(sp3)-C(sp3) Bond  C(28)  -   C(29)  =       1.39 Ang.

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                   C4  -RU2 -RU3 -C8    153.00  3.00   1.555   1.555   1.555   1.555

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                   RU3 -RU1 -C3  -O3    121.00 19.00   1.555   1.555   1.555   1.555

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                   C6  -RU2 -C4  -O4     72.00 17.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    171
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PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    172
                   N2  -RU2 -C4  -O4   -114.00 17.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    173
                   RU3 -RU2 -C4  -O4   -157.00 15.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    174
                   RU1 -RU2 -C4  -O4   -179.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    175
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PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    177
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PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    178
                   RU3 -RU2 -C5  -O5   -161.00 19.00   1.555   1.555   1.555   1.555

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PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    181
                   C4  -RU2 -C6  -O6     40.00 18.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    182
                   N2  -RU2 -C6  -O6    -68.00 19.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    183
                   RU3 -RU2 -C6  -O6   -136.00 18.00   1.555   1.555   1.555   1.555

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                   RU1 -RU2 -C6  -O6    -78.00 18.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    185
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                   C8  -RU3 -C7  -O7     72.00  7.00   1.555   1.555   1.555   1.555

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                   C9  -RU3 -C7  -O7   -150.00  6.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    188
                   RU2 -RU3 -C7  -O7    170.00  7.00   1.555   1.555   1.555   1.555

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                   RU1 -RU3 -C7  -O7   -129.00  7.00   1.555   1.555   1.555   1.555

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                   RU1 -RU3 -C8  -O8   -141.00 36.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    195
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                   RU1 -RU3 -C10 -O10   116.00 21.00   1.555   1.555   1.555   1.555

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                   RU6 -RU4 -C11 -O11   161.00 21.00   1.555   1.555   1.555   1.555

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                   RU5 -RU4 -C11 -O11  -142.00 21.00   1.555   1.555   1.555   1.555

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                   C11 -RU4 -C12 -O12   104.00100.00   1.555   1.555   1.555   1.555

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                   C12 -RU4 -C13 -O13   -68.00 15.00   1.555   1.555   1.555   1.555

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                   N3  -RU4 -C13 -O13  -162.00 15.00   1.555   1.555   1.555   1.555

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                   RU6 -RU4 -C13 -O13   116.00 15.00   1.555   1.555   1.555   1.555

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                   RU5 -RU4 -C13 -O13   132.00 15.00   1.555   1.555   1.555   1.555

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                   C16 -RU5 -C14 -O14   -52.00 15.00   1.555   1.555   1.555   1.555

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                   C15 -RU5 -C14 -O14    39.00 15.00   1.555   1.555   1.555   1.555

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                   C14 -RU5 -C16 -O16   -10.00 14.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    235
                   N4  -RU5 -C16 -O16    82.00 15.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    236
                   RU6 -RU5 -C16 -O16   167.00 14.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    237
                   RU4 -RU5 -C16 -O16   108.00 14.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    238
                   C20 -RU6 -C17 -O17    42.00  9.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    239
                   C18 -RU6 -C17 -O17   -56.00  9.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    240
                   C19 -RU6 -C17 -O17   170.00  8.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    241
                   RU5 -RU6 -C17 -O17  -158.00  9.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    242
                   RU4 -RU6 -C17 -O17   140.00  9.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    243
                   C20 -RU6 -C18 -O18   -23.00 22.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    244
                   C19 -RU6 -C18 -O18  -116.00 22.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    245
                   C17 -RU6 -C18 -O18    70.00 22.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    246
                   RU5 -RU6 -C18 -O18   158.00 22.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    247
                   RU4 -RU6 -C18 -O18   148.00 21.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    248
                   C20 -RU6 -C19 -O19   -25.00 10.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    249
                   C18 -RU6 -C19 -O19    73.00 10.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    250
                   C17 -RU6 -C19 -O19  -154.00  9.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    251
                   RU5 -RU6 -C19 -O19   174.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    252
                   RU4 -RU6 -C19 -O19  -124.00 10.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    253
                   C18 -RU6 -C20 -O20   -12.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    254
                   C19 -RU6 -C20 -O20    81.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    255
                   C17 -RU6 -C20 -O20  -105.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    256
                   RU5 -RU6 -C20 -O20   167.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    257
                   RU4 -RU6 -C20 -O20   171.00100.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    266
                   C1  -RU1 -N1  -C21  -147.00  3.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    271
                   C1  -RU1 -N1  -N2     33.00  3.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    282
                   C6  -RU2 -N2  -N1     -6.00  4.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    287
                   C6  -RU2 -N2  -C23   165.00  3.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    294
                   C11 -RU4 -N3  -N4      1.00  4.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    299
                   C11 -RU4 -N3  -C24  -179.00 84.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    310
                   C16 -RU5 -N4  -C26  -150.00  3.00   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    316
                   C16 -RU5 -N4  -N3     26.00  4.00   1.555   1.555   1.555   1.555

PLAT_711  Alert C BOND    Unknown or Inconsistent Label ........       H1RU
                           RU1    H1RU

PLAT_711  Alert C BOND    Unknown or Inconsistent Label ........       H1RU
                           RU2    H1RU

General Notes



ABSTM_02  When printed, the submitted absorption T values will be replaced
          by the scaled T values. Since the ratio of scaled T's is
          identical to the ratio of reported T values, the scaling does
          not imply a change to the absorption corrections used in the
          study.
          Ratio of Tmax expected/reported      1.557
          Tmax scaled      0.391 Tmin scaled      0.349


 1 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 136 Alert Level C = Please check

Comment top

The parent cluster (I), as well as its derivatives [Ru₃(µ-H){µ-N₂C₃H(CH₃)₂-3,5}(CO)₁₀], (II), and [Ru₃(µ-H)(CO)₁₀{µ-N₂C₃H(CF₃)₂-3,5}], (III), were first synthesized by Bruce et al. (1986) from the reaction of Ru₃(CO)₁₂ and the corresponding pyrazole in refluxing cyclohexane. Only the di(trifluoromethyl)pyrazolyl derivative, (III), was obtained in good yield and studied by X-ray diffraction. More recently, Cabeza et al. (1995) synthesized (II) by protonation of the anionic cluster [Ru₃{µ-N₂C₃H(CH₃)₂-3,5}(µ-CO)₃(CO)₇]^-, which was synthesized by reaction between 3,5-dimethylpyrazole and the anionic cluster [Ru₃(µ-H)(µ-CO)(CO)₁₀]^- in refluxing tetrahydrofuran. Here were report a new synthetic route and the X-ray crystal structure analysis of (I), which can be obtained in good yield by reaction of potassium dihydrobis(1-pyrazolyl)borate (Trofimenko, 1970) with Ru₃(CO)₁₂ in refluxing MeOH.

The molecular structure of [Ru₃(µ-H)(µ-N₂C₃H₃)(CO)₁₀], (I), was confirmed by single-crystal X-ray analysis. The asymmetric unit comprises two independent molecules of (I) and half a molecule of cyclohexane. Fig. 1 shows only one independent molecule of (I), and significant bond lengths and angles are given in Table 1. The triruthenium core of (I) consists of an asymmetric Ru₃ triangle, the three metal–metal bonds (average of the two molecules in the asymmetric unit) [2.850 (1), 2.907 (1) and 2.843 (1) Å] are comparable to those observed in (III) [2.849 (1), 2.902 (1) and 2.846 (1) Å]. The pyrazole ligand and the hydrido bridge two Ru atoms in an axial fashion. The Ru—N bond distances [average 2.095 (9) and 2.109 (9) Å] are sligthly shorter than those in (III) [Ru—N 2.146 (3) and 2.137 (3) Å]. The angles between the planar pyrazolyl ligands and the Ru₃ planes are, respectively, 75.5° for molecule 1 and 76.8° for molecule 2.

Experimental top

A mixture of Ru₃(CO)₁₂ (200 mg, 0.31 mmol) and potassium dihydrobis(1-pyrazolyl)borate (58 mg, 0.31 mmol) was dissolved in MeOH (30 ml), under an N₂ atmosphere using standard Schlenk techniques. The solution was refluxed for 20 min, the solution became red–brown, and the characteristic Ru₃(CO)₁₂ absorption at ν_CO = 2061 cm^-1 had disappeared. The solution was cooled, concentrated to 1 ml, and chromatographed on a silica-gel (60 GF254, Merck) column, using hexane as eluent, until the first yellow fraction [a mixture of Ru₃(CO)₁₂ and Ru₄H₄(CO)₁₂ (15%)] separated. Then an orange–red fraction containing (I) was extracted using acetone as eluent. The product was isolated by evaporation of the solvent and recrystalization from cyclohexane, and dried in vacuo. Yield: 52%; ¹H NMR (200 MHz, CDCl₃): -13.42 (s, 1H), 6.23 (t, 1H), 7.24 (d, 2H); IR (KBr, cm^-1, CO): 2106 (w), 2093 (w), 2069 (s), 2060 (s), 2026 (s), 2019 (m), 2011 (m), 1991 (w). An orange crystal of compound (I) was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite-monochromated radiation (Image plate distance 90 mm, ϕ oscillation scans 0–195°, step Δϕ = 0.7°, 2θ range 2.15–22.5°, d_max-d_min = 16.00–0.93 Å).

Computing details top

Data collection: EXPOSE (Stoe & Cie, 2000); cell refinement: CELL (Stoe & Cie, 2000); data reduction: INTEGRATE (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top

Fig. 1. The molecular structure of one molecule of [Ru₃(µ-H)(µ-N₂C₃H₃)(CO)₁₀]. Displacement ellipsoids are drawn at the 50% probability level.

decacarbonyl-1κ⁴C,2 K³ C,3κ³C-µ-hydrido-2:3κ²H:H-µ-pyrazolyl- 2:3κ²N¹:N²-triangulo-triruthenium top

Crystal data top

[Ru₃H(C₃H₃N₂)(CO)₁₀]·C_1.50H₃	F(000) = 5120
M_r = 672.43	D_x = 2.290 Mg m⁻³
Monoclinic, I2/a	Mo Kα radiation, λ = 0.71073 Å
a = 14.2248 (11) Å	Cell parameters from 8000 reflections
b = 9.1670 (5) Å	θ = 2.2–22.5°
c = 59.834 (5) Å	µ = 2.35 mm⁻¹
β = 90.380 (9)°	T = 153 K
V = 7802.1 (10) Å³	Block, orange
Z = 16	0.50 × 0.45 × 0.40 mm

Data collection top

Stoe IPDS diffractometer	4743 independent reflections
Radiation source: fine-focus sealed tube	4474 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
Detector resolution: 0 pixels mm^-1	θ_max = 22.3°, θ_min = 2.0°
ϕ oscillation scans	h = −15→15
Absorption correction: multi-scan (Blessing, 1995)	k = −8→9
T_min = 0.224, T_max = 0.251	l = −60→63
18544 measured reflections

Refinement top

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.107	H atoms treated by a mixture of independent and constrained refinement
S = 1.36	w = 1/[σ²(F_o²) + 252.1712P] where P = (F_o² + 2F_c²)/3
4743 reflections	(Δ/σ)_max < 0.001
532 parameters	Δρ_max = 1.00 e Å⁻³
0 restraints	Δρ_min = −0.81 e Å⁻³

Crystal data top

[Ru₃H(C₃H₃N₂)(CO)₁₀]·C_1.50H₃	V = 7802.1 (10) Å³
M_r = 672.43	Z = 16
Monoclinic, I2/a	Mo Kα radiation
a = 14.2248 (11) Å	µ = 2.35 mm⁻¹
b = 9.1670 (5) Å	T = 153 K
c = 59.834 (5) Å	0.50 × 0.45 × 0.40 mm
β = 90.380 (9)°

Data collection top

Stoe IPDS diffractometer	4743 independent reflections
Absorption correction: multi-scan (Blessing, 1995)	4474 reflections with I > 2σ(I)
T_min = 0.224, T_max = 0.251	R_int = 0.041
18544 measured reflections	θ_max = 22.3°

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.107	H atoms treated by a mixture of independent and constrained refinement
S = 1.36	w = 1/[σ²(F_o²) + 252.1712P] where P = (F_o² + 2F_c²)/3
4743 reflections	Δρ_max = 1.00 e Å⁻³
532 parameters	Δρ_min = −0.81 e Å⁻³

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ru1	0.49279 (6)	0.94266 (9)	0.053746 (13)	0.0155 (2)
H1	0.4462	0.8556	0.0760	0.050*
Ru2	0.50356 (5)	0.69385 (9)	0.083565 (13)	0.0163 (2)
Ru3	0.54938 (6)	0.66363 (9)	0.037485 (13)	0.0181 (2)
Ru4	0.66421 (6)	1.32018 (10)	0.197832 (13)	0.0203 (2)
H2	0.7280	1.2394	0.1809	0.050*
Ru5	0.66041 (6)	1.15837 (10)	0.155947 (13)	0.0201 (2)
Ru6	0.52559 (6)	1.37891 (10)	0.164521 (14)	0.0198 (2)
C1	0.3754 (8)	0.9254 (12)	0.03840 (16)	0.020 (2)
C2	0.5550 (7)	1.0169 (12)	0.02797 (18)	0.021 (2)
C3	0.4572 (7)	1.1287 (13)	0.06658 (17)	0.022 (3)
C4	0.4754 (7)	0.7340 (12)	0.11441 (18)	0.019 (2)
C5	0.5716 (8)	0.5154 (14)	0.08797 (19)	0.028 (3)
C6	0.3902 (8)	0.5900 (13)	0.07846 (17)	0.024 (3)
C7	0.6760 (8)	0.7253 (11)	0.04577 (17)	0.021 (2)
C8	0.5872 (8)	0.4611 (15)	0.03824 (17)	0.027 (3)
C9	0.4172 (9)	0.6159 (13)	0.03119 (18)	0.030 (3)
C10	0.5720 (8)	0.7080 (12)	0.00662 (18)	0.026 (3)
C11	0.7179 (8)	1.5032 (16)	0.19033 (18)	0.033 (3)
C12	0.5831 (8)	1.4084 (14)	0.21910 (18)	0.032 (3)
C13	0.7653 (8)	1.2709 (13)	0.21846 (19)	0.027 (3)
C14	0.7531 (9)	1.0064 (15)	0.15208 (18)	0.034 (3)
C15	0.5716 (8)	1.0957 (13)	0.13378 (19)	0.030 (3)
C16	0.7224 (7)	1.2771 (13)	0.13502 (18)	0.026 (3)
C17	0.4534 (8)	1.2308 (13)	0.18054 (18)	0.026 (3)
C18	0.4464 (8)	1.3675 (12)	0.1384 (2)	0.027 (3)
C19	0.6121 (8)	1.5101 (14)	0.15011 (18)	0.028 (3)
C20	0.4618 (8)	1.5336 (15)	0.17916 (19)	0.033 (3)
C21	0.6877 (7)	1.0353 (12)	0.07774 (17)	0.021 (2)
H21A	0.6995	1.1257	0.0705	0.025*
C22	0.7444 (7)	0.9723 (12)	0.09416 (16)	0.022 (2)
H22A	0.8008	1.0107	0.1004	0.026*
C23	0.7016 (7)	0.8439 (13)	0.09942 (16)	0.023 (3)
H23A	0.7238	0.7757	0.1102	0.028*
C24	0.5712 (8)	1.0272 (13)	0.21818 (18)	0.028 (3)
H24A	0.5663	1.0524	0.2335	0.034*
C25	0.5437 (9)	0.8955 (14)	0.20850 (19)	0.037 (3)
H25A	0.5166	0.8142	0.2159	0.045*
C26	0.5635 (9)	0.9066 (13)	0.1861 (2)	0.035 (3)
H26A	0.5524	0.8337	0.1751	0.042*
C27	0.2375 (14)	1.095 (3)	0.2549 (3)	0.094 (7)
H27A	0.2803	1.0695	0.2674	0.112*
H27B	0.1990	1.0089	0.2509	0.112*
C28	0.2835 (17)	1.143 (3)	0.2379 (4)	0.114 (9)
H28A	0.2415	1.1392	0.2247	0.137*
H28B	0.3363	1.0749	0.2351	0.137*
C29	0.3199 (13)	1.283 (2)	0.2397 (3)	0.071 (5)
H29A	0.3498	1.3060	0.2252	0.085*
H29B	0.3709	1.2797	0.2510	0.085*
N1	0.6142 (5)	0.9482 (9)	0.07381 (12)	0.0159 (19)
N2	0.6224 (5)	0.8288 (9)	0.08690 (13)	0.0169 (19)
N3	0.6061 (6)	1.1120 (10)	0.20190 (14)	0.026 (2)
N4	0.6011 (6)	1.0382 (10)	0.18253 (13)	0.023 (2)
O1	0.3039 (6)	0.9206 (9)	0.03019 (12)	0.033 (2)
O2	0.5914 (5)	1.0604 (9)	0.01271 (12)	0.0288 (18)
O3	0.4389 (5)	1.2394 (9)	0.07338 (13)	0.0325 (19)
O4	0.4596 (5)	0.7516 (9)	0.13268 (12)	0.0314 (19)
O5	0.6096 (6)	0.4095 (9)	0.09149 (13)	0.034 (2)
O6	0.3197 (5)	0.5326 (9)	0.07603 (13)	0.035 (2)
O7	0.7524 (5)	0.7570 (9)	0.04826 (12)	0.0302 (18)
O8	0.6109 (6)	0.3441 (10)	0.03819 (14)	0.041 (2)
O9	0.3432 (6)	0.5910 (10)	0.02628 (15)	0.043 (2)
O10	0.5891 (6)	0.7327 (10)	−0.01142 (13)	0.040 (2)
O11	0.7521 (6)	1.6126 (10)	0.18675 (15)	0.042 (2)
O12	0.5340 (6)	1.4612 (11)	0.23173 (16)	0.055 (3)
O13	0.8245 (6)	1.2498 (10)	0.23048 (14)	0.043 (2)
O14	0.8065 (7)	0.9177 (12)	0.14830 (15)	0.059 (3)
O15	0.5196 (6)	1.0610 (9)	0.12020 (13)	0.035 (2)
O16	0.7650 (6)	1.3439 (10)	0.12222 (14)	0.042 (2)
O17	0.4052 (5)	1.1532 (9)	0.18943 (12)	0.0290 (18)
O18	0.3959 (6)	1.3631 (10)	0.12307 (13)	0.037 (2)
O19	0.6581 (6)	1.5964 (10)	0.14171 (14)	0.040 (2)
O20	0.4223 (6)	1.6284 (10)	0.18783 (17)	0.050 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ru1	0.0197 (5)	0.0140 (5)	0.0130 (4)	0.0018 (3)	−0.0001 (3)	0.0002 (3)
Ru2	0.0180 (4)	0.0158 (5)	0.0151 (4)	−0.0007 (3)	0.0004 (3)	0.0008 (3)
Ru3	0.0219 (5)	0.0163 (5)	0.0161 (4)	0.0008 (4)	0.0006 (3)	−0.0038 (3)
Ru4	0.0202 (5)	0.0240 (6)	0.0167 (4)	−0.0033 (4)	0.0022 (3)	−0.0021 (4)
Ru5	0.0230 (5)	0.0227 (6)	0.0147 (4)	0.0039 (4)	0.0016 (3)	0.0000 (4)
Ru6	0.0196 (5)	0.0190 (5)	0.0209 (5)	−0.0006 (4)	0.0019 (4)	−0.0002 (4)
C1	0.024 (6)	0.026 (7)	0.010 (5)	0.003 (5)	0.006 (5)	−0.002 (4)
C2	0.025 (6)	0.019 (7)	0.018 (6)	−0.002 (5)	−0.004 (5)	−0.003 (5)
C3	0.019 (6)	0.026 (8)	0.020 (6)	−0.001 (5)	0.001 (4)	0.006 (5)
C4	0.017 (5)	0.021 (7)	0.020 (6)	−0.004 (4)	0.001 (4)	0.002 (5)
C5	0.020 (6)	0.030 (9)	0.035 (7)	−0.008 (6)	−0.005 (5)	−0.009 (6)
C6	0.030 (7)	0.022 (7)	0.021 (6)	0.006 (5)	−0.002 (5)	0.000 (5)
C7	0.029 (7)	0.012 (6)	0.022 (6)	0.010 (5)	−0.001 (5)	−0.001 (4)
C8	0.033 (7)	0.026 (9)	0.020 (6)	−0.006 (6)	0.002 (5)	−0.006 (5)
C9	0.035 (8)	0.033 (8)	0.021 (6)	0.005 (6)	0.000 (5)	−0.015 (5)
C10	0.042 (7)	0.018 (7)	0.018 (7)	0.001 (5)	0.001 (5)	−0.002 (5)
C11	0.025 (7)	0.050 (10)	0.024 (6)	0.005 (6)	−0.005 (5)	−0.002 (6)
C12	0.031 (7)	0.043 (8)	0.021 (6)	−0.013 (6)	0.007 (5)	−0.009 (6)
C13	0.029 (7)	0.027 (7)	0.025 (6)	−0.005 (5)	0.007 (6)	0.003 (5)
C14	0.039 (7)	0.044 (9)	0.017 (6)	0.009 (7)	−0.005 (5)	0.003 (5)
C15	0.033 (7)	0.028 (8)	0.027 (7)	0.004 (5)	0.013 (6)	0.000 (5)
C16	0.024 (6)	0.032 (8)	0.020 (6)	0.009 (5)	0.000 (5)	0.003 (5)
C17	0.025 (6)	0.025 (7)	0.027 (6)	0.008 (5)	−0.002 (5)	0.000 (5)
C18	0.033 (7)	0.013 (7)	0.036 (7)	0.003 (5)	0.011 (6)	0.008 (5)
C19	0.027 (6)	0.029 (8)	0.027 (6)	0.001 (6)	−0.001 (5)	−0.004 (5)
C20	0.028 (7)	0.038 (9)	0.034 (7)	−0.012 (6)	−0.001 (5)	0.007 (6)
C21	0.024 (6)	0.015 (7)	0.024 (6)	−0.006 (5)	0.002 (5)	−0.004 (5)
C22	0.019 (6)	0.024 (7)	0.022 (6)	−0.007 (5)	−0.003 (4)	−0.001 (5)
C23	0.024 (6)	0.033 (8)	0.012 (5)	0.007 (5)	−0.003 (4)	−0.001 (5)
C24	0.031 (6)	0.038 (8)	0.017 (6)	−0.013 (5)	0.001 (5)	0.006 (5)
C25	0.042 (8)	0.038 (9)	0.031 (7)	−0.009 (6)	0.002 (6)	0.014 (6)
C26	0.049 (8)	0.023 (8)	0.033 (7)	−0.008 (6)	0.002 (6)	0.002 (5)
C27	0.085 (14)	0.13 (2)	0.066 (13)	0.005 (14)	−0.002 (11)	0.033 (13)
C28	0.14 (2)	0.11 (2)	0.089 (16)	−0.070 (16)	−0.049 (15)	0.041 (13)
C29	0.086 (13)	0.078 (14)	0.050 (10)	0.005 (11)	0.000 (9)	−0.007 (9)
N1	0.021 (5)	0.015 (5)	0.012 (4)	0.004 (4)	0.004 (3)	−0.001 (4)
N2	0.017 (5)	0.019 (5)	0.014 (4)	0.005 (4)	−0.001 (3)	0.004 (4)
N3	0.024 (5)	0.028 (6)	0.025 (5)	−0.008 (4)	0.001 (4)	0.004 (4)
N4	0.032 (5)	0.022 (6)	0.014 (5)	−0.002 (4)	−0.006 (4)	−0.003 (4)
O1	0.026 (5)	0.048 (6)	0.024 (4)	0.003 (4)	−0.001 (4)	−0.003 (4)
O2	0.039 (5)	0.027 (5)	0.021 (4)	−0.003 (4)	−0.002 (4)	0.003 (4)
O3	0.034 (5)	0.020 (5)	0.043 (5)	0.006 (4)	−0.001 (4)	−0.014 (4)
O4	0.038 (5)	0.038 (5)	0.018 (5)	−0.002 (4)	0.003 (3)	0.000 (4)
O5	0.036 (5)	0.021 (5)	0.044 (5)	0.013 (4)	−0.008 (4)	0.000 (4)
O6	0.024 (5)	0.039 (6)	0.041 (5)	−0.007 (4)	0.001 (4)	−0.010 (4)
O7	0.025 (5)	0.034 (5)	0.032 (4)	0.000 (4)	0.005 (4)	−0.004 (4)
O8	0.054 (6)	0.017 (6)	0.052 (6)	0.007 (4)	0.002 (4)	−0.002 (4)
O9	0.028 (5)	0.046 (6)	0.054 (6)	−0.004 (4)	−0.006 (4)	−0.017 (4)
O10	0.054 (6)	0.043 (6)	0.022 (5)	0.007 (4)	0.004 (4)	−0.001 (4)
O11	0.038 (5)	0.032 (6)	0.055 (6)	−0.013 (4)	−0.001 (4)	0.010 (4)
O12	0.043 (5)	0.067 (8)	0.057 (6)	−0.003 (5)	0.015 (5)	−0.034 (5)
O13	0.035 (5)	0.063 (7)	0.031 (5)	0.005 (4)	−0.005 (4)	0.001 (4)
O14	0.062 (6)	0.069 (8)	0.045 (6)	0.049 (6)	−0.014 (5)	−0.010 (5)
O15	0.039 (5)	0.039 (6)	0.028 (4)	0.001 (4)	−0.006 (4)	−0.010 (4)
O16	0.030 (5)	0.060 (7)	0.037 (5)	0.001 (4)	0.009 (4)	0.018 (5)
O17	0.028 (4)	0.031 (5)	0.029 (4)	−0.003 (4)	0.003 (3)	0.010 (4)
O18	0.040 (5)	0.047 (6)	0.026 (4)	−0.001 (4)	−0.017 (4)	0.002 (4)
O19	0.038 (5)	0.038 (6)	0.044 (5)	−0.009 (4)	0.002 (4)	0.017 (4)
O20	0.038 (5)	0.029 (6)	0.084 (7)	−0.001 (4)	0.020 (5)	−0.024 (5)

Geometric parameters (Å, º) top

Ru1—C1	1.907 (11)	C1—O1	1.127 (12)
Ru1—C2	1.909 (11)	C2—O2	1.126 (12)
Ru1—C3	1.939 (13)	C3—O3	1.125 (13)
Ru1—N1	2.097 (8)	C4—O4	1.129 (12)
Ru1—Ru3	2.8544 (12)	C5—O5	1.130 (14)
Ru1—Ru2	2.8992 (11)	C6—O6	1.142 (13)
Ru1—H1	1.69	C7—O7	1.134 (12)
Ru2—C6	1.895 (12)	C8—O8	1.125 (14)
Ru2—C5	1.918 (13)	C9—O9	1.115 (13)
Ru2—C4	1.927 (11)	C10—O10	1.131 (12)
Ru2—N2	2.103 (8)	C11—O11	1.136 (15)
Ru2—Ru3	2.8509 (11)	C12—O12	1.140 (14)
Ru2—H1	1.75	C13—O13	1.121 (13)
Ru3—C10	1.920 (11)	C14—O14	1.136 (14)
Ru3—C8	1.933 (14)	C15—O15	1.141 (14)
Ru3—C7	1.949 (12)	C16—O16	1.156 (13)
Ru3—C9	1.964 (13)	C17—O17	1.125 (13)
Ru4—C11	1.898 (15)	C18—O18	1.160 (14)
Ru4—C12	1.904 (12)	C19—O19	1.145 (14)
Ru4—C13	1.942 (12)	C20—O20	1.159 (15)
Ru4—N3	2.094 (9)	C21—N1	1.336 (13)
Ru4—Ru6	2.8457 (12)	C21—C22	1.391 (15)
Ru4—Ru5	2.9124 (12)	C22—C23	1.363 (15)
Ru4—H2	1.55	C23—N2	1.356 (13)
Ru5—C16	1.883 (12)	C24—N3	1.344 (14)
Ru5—C15	1.914 (13)	C24—C25	1.394 (17)
Ru5—H2	1.92	C25—C26	1.374 (16)
Ru5—C14	1.933 (13)	C26—N4	1.338 (15)
Ru5—N4	2.115 (9)	C27—C28	1.29 (2)
Ru5—Ru6	2.8357 (12)	C27—C29ⁱ	1.42 (3)
Ru5—H2	1.92	C28—C29	1.39 (2)
Ru6—C20	1.901 (14)	C29—C27ⁱ	1.42 (3)
Ru6—C18	1.925 (13)	N1—N2	1.351 (11)
Ru6—C19	1.928 (13)	N3—N4	1.344 (12)
Ru6—C17	1.957 (13)

C1—Ru1—C2	92.8 (4)	C16—Ru5—C14	90.8 (5)
C1—Ru1—C3	91.9 (4)	C15—Ru5—C14	98.5 (5)
C2—Ru1—C3	97.5 (4)	H2—Ru5—C14	91.9
C1—Ru1—N1	173.1 (4)	C16—Ru5—N4	172.8 (4)
C2—Ru1—N1	94.0 (4)	C15—Ru5—N4	95.7 (4)
C3—Ru1—N1	88.2 (4)	H2—Ru5—N4	79.5
C1—Ru1—Ru3	90.6 (3)	C14—Ru5—N4	89.5 (4)
C2—Ru1—Ru3	84.9 (3)	C16—Ru5—Ru6	91.6 (3)
C3—Ru1—Ru3	176.5 (3)	C15—Ru5—Ru6	84.0 (3)
N1—Ru1—Ru3	89.1 (2)	H2—Ru5—Ru6	85.4
C1—Ru1—Ru2	105.9 (3)	C14—Ru5—Ru6	176.4 (3)
C2—Ru1—Ru2	139.0 (3)	N4—Ru5—Ru6	87.8 (2)
C3—Ru1—Ru2	117.5 (3)	C16—Ru5—Ru4	105.8 (3)
N1—Ru1—Ru2	68.1 (2)	C15—Ru5—Ru4	139.3 (3)
Ru3—Ru1—Ru2	59.40 (3)	H2—Ru5—Ru4	29.2
C1—Ru1—H1	89.6	C14—Ru5—Ru4	117.5 (3)
C2—Ru1—H1	172.1	N4—Ru5—Ru4	67.9 (2)
C3—Ru1—H1	89.9	Ru6—Ru5—Ru4	59.33 (3)
N1—Ru1—H1	83.5	C16—Ru5—H2	93.4
Ru3—Ru1—H1	87.6	C15—Ru5—H2	168.5
Ru2—Ru1—H1	33.3	C14—Ru5—H2	91.9
C6—Ru2—C5	91.2 (5)	N4—Ru5—H2	79.5
C6—Ru2—C4	93.9 (4)	Ru6—Ru5—H2	85.4
C5—Ru2—C4	98.0 (5)	Ru4—Ru5—H2	29.2
C6—Ru2—N2	173.2 (4)	C20—Ru6—C18	97.9 (5)
C5—Ru2—N2	94.8 (4)	C20—Ru6—C19	92.8 (5)
C4—Ru2—N2	88.2 (4)	C18—Ru6—C19	92.4 (4)
C6—Ru2—Ru3	89.7 (3)	C20—Ru6—C17	92.2 (5)
C5—Ru2—Ru3	86.1 (3)	C18—Ru6—C17	93.1 (4)
C4—Ru2—Ru3	174.5 (3)	C19—Ru6—C17	172.0 (5)
N2—Ru2—Ru3	87.7 (2)	C20—Ru6—Ru5	160.2 (3)
C6—Ru2—Ru1	104.8 (3)	C18—Ru6—Ru5	101.9 (3)
C5—Ru2—Ru1	141.3 (3)	C19—Ru6—Ru5	86.0 (3)
C4—Ru2—Ru1	115.4 (3)	C17—Ru6—Ru5	87.2 (3)
N2—Ru2—Ru1	68.6 (2)	C20—Ru6—Ru4	98.6 (3)
Ru3—Ru2—Ru1	59.52 (3)	C18—Ru6—Ru4	163.4 (3)
C6—Ru2—H1	89.4	C19—Ru6—Ru4	89.4 (3)
C5—Ru2—H1	172.8	C17—Ru6—Ru4	83.6 (3)
C4—Ru2—H1	89.2	Ru5—Ru6—Ru4	61.68 (3)
N2—Ru2—H1	84.2	O1—C1—Ru1	176.1 (9)
Ru3—Ru2—H1	86.7	O2—C2—Ru1	179.7 (10)
Ru1—Ru2—H1	32.0	O3—C3—Ru1	177.1 (10)
C10—Ru3—C8	100.2 (5)	O4—C4—Ru2	177.1 (10)
C10—Ru3—C7	91.3 (4)	O5—C5—Ru2	176.8 (10)
C8—Ru3—C7	90.9 (4)	O6—C6—Ru2	176.5 (10)
C10—Ru3—C9	91.7 (5)	O7—C7—Ru3	172.4 (9)
C8—Ru3—C9	93.2 (5)	O8—C8—Ru3	178.0 (11)
C7—Ru3—C9	174.4 (4)	O9—C9—Ru3	175.7 (10)
C10—Ru3—Ru2	161.9 (3)	O10—C10—Ru3	177.2 (10)
C8—Ru3—Ru2	97.8 (3)	O11—C11—Ru4	176.9 (10)
C7—Ru3—Ru2	86.7 (3)	O12—C12—Ru4	179.5 (11)
C9—Ru3—Ru2	89.0 (3)	O13—C13—Ru4	176.5 (11)
C10—Ru3—Ru1	100.8 (3)	O14—C14—Ru5	175.4 (10)
C8—Ru3—Ru1	158.7 (3)	O15—C15—Ru5	178.2 (10)
C7—Ru3—Ru1	85.1 (3)	O16—C16—Ru5	175.7 (10)
C9—Ru3—Ru1	89.6 (3)	O17—C17—Ru6	173.9 (10)
Ru2—Ru3—Ru1	61.08 (3)	O18—C18—Ru6	177.4 (10)
C11—Ru4—C12	91.7 (5)	O19—C19—Ru6	174.6 (10)
C11—Ru4—C13	93.4 (5)	O20—C20—Ru6	179.1 (11)
C12—Ru4—C13	97.1 (5)	N1—C21—C22	109.0 (10)
C11—Ru4—N3	172.9 (4)	C23—C22—C21	105.3 (9)
C12—Ru4—N3	93.9 (4)	N2—C23—C22	109.3 (9)
C13—Ru4—N3	90.3 (4)	N3—C24—C25	107.7 (10)
C11—Ru4—Ru6	86.8 (3)	C26—C25—C24	106.4 (10)
C12—Ru4—Ru6	88.1 (4)	N4—C26—C25	108.0 (11)
C13—Ru4—Ru6	174.8 (3)	C28—C27—C29ⁱ	102 (2)
N3—Ru4—Ru6	89.0 (2)	C27—C28—C29	116 (2)
C11—Ru4—Ru5	104.6 (3)	C28—C29—C27ⁱ	122 (2)
C12—Ru4—Ru5	141.6 (3)	C21—N1—N2	108.5 (8)
C13—Ru4—Ru5	116.0 (3)	C21—N1—Ru1	139.1 (7)
N3—Ru4—Ru5	68.3 (2)	N2—N1—Ru1	112.3 (6)
Ru6—Ru4—Ru5	58.99 (3)	N1—N2—C23	107.8 (8)
C11—Ru4—H2	91.7	N1—N2—Ru2	110.8 (6)
C12—Ru4—H2	176.6	C23—N2—Ru2	141.0 (7)
C13—Ru4—H2	82.6	N4—N3—C24	108.4 (9)
N3—Ru4—H2	82.8	N4—N3—Ru4	112.2 (6)
Ru6—Ru4—H2	92.2	C24—N3—Ru4	139.4 (8)
Ru5—Ru4—H2	37.2	C26—N4—N3	109.6 (9)
C16—Ru5—C15	91.3 (5)	C26—N4—Ru5	138.8 (7)
C16—Ru5—H2	93.4	N3—N4—Ru5	111.5 (7)
C15—Ru5—H2	168.5

C1—Ru1—Ru2—C6	0.3 (4)	N1—Ru1—C2—O2	153 (100)
C2—Ru1—Ru2—C6	−113.7 (6)	Ru3—Ru1—C2—O2	65 (100)
C3—Ru1—Ru2—C6	101.0 (5)	Ru2—Ru1—C2—O2	93 (100)
N1—Ru1—Ru2—C6	176.7 (4)	C1—Ru1—C3—O3	−104 (21)
Ru3—Ru1—Ru2—C6	−80.7 (3)	C2—Ru1—C3—O3	−11 (21)
C1—Ru1—Ru2—C5	111.6 (6)	N1—Ru1—C3—O3	83 (21)
C2—Ru1—Ru2—C5	−2.4 (7)	Ru3—Ru1—C3—O3	121 (19)
C3—Ru1—Ru2—C5	−147.7 (6)	Ru2—Ru1—C3—O3	147 (20)
N1—Ru1—Ru2—C5	−72.0 (5)	C6—Ru2—C4—O4	72 (17)
Ru3—Ru1—Ru2—C5	30.6 (5)	C5—Ru2—C4—O4	−19 (18)
C1—Ru1—Ru2—C4	−101.5 (4)	N2—Ru2—C4—O4	−114 (17)
C2—Ru1—Ru2—C4	144.6 (6)	Ru3—Ru2—C4—O4	−157 (15)
C3—Ru1—Ru2—C4	−0.7 (5)	Ru1—Ru2—C4—O4	−179 (100)
N1—Ru1—Ru2—C4	75.0 (4)	C6—Ru2—C5—O5	−72 (19)
Ru3—Ru1—Ru2—C4	177.5 (3)	C4—Ru2—C5—O5	22 (19)
C1—Ru1—Ru2—N2	−178.6 (4)	N2—Ru2—C5—O5	111 (19)
C2—Ru1—Ru2—N2	67.5 (5)	Ru3—Ru2—C5—O5	−161 (19)
C3—Ru1—Ru2—N2	−77.8 (4)	Ru1—Ru2—C5—O5	173 (100)
N1—Ru1—Ru2—N2	−2.1 (3)	C5—Ru2—C6—O6	138 (18)
Ru3—Ru1—Ru2—N2	100.4 (2)	C4—Ru2—C6—O6	40 (18)
C1—Ru1—Ru2—Ru3	81.0 (3)	N2—Ru2—C6—O6	−68 (19)
C2—Ru1—Ru2—Ru3	−33.0 (5)	Ru3—Ru2—C6—O6	−136 (18)
C3—Ru1—Ru2—Ru3	−178.2 (3)	Ru1—Ru2—C6—O6	−78 (18)
N1—Ru1—Ru2—Ru3	−102.6 (2)	C10—Ru3—C7—O7	−28 (7)
C6—Ru2—Ru3—C10	109.5 (11)	C8—Ru3—C7—O7	72 (7)
C5—Ru2—Ru3—C10	−159.2 (11)	C9—Ru3—C7—O7	−150 (6)
C4—Ru2—Ru3—C10	−21 (3)	Ru2—Ru3—C7—O7	170 (7)
N2—Ru2—Ru3—C10	−64.2 (11)	Ru1—Ru3—C7—O7	−129 (7)
Ru1—Ru2—Ru3—C10	2.2 (11)	C10—Ru3—C8—O8	29 (36)
C6—Ru2—Ru3—C8	−75.9 (5)	C7—Ru3—C8—O8	−62 (36)
C5—Ru2—Ru3—C8	15.4 (5)	C9—Ru3—C8—O8	121 (36)
C4—Ru2—Ru3—C8	153 (3)	Ru2—Ru3—C8—O8	−149 (36)
N2—Ru2—Ru3—C8	110.4 (4)	Ru1—Ru3—C8—O8	−141 (36)
Ru1—Ru2—Ru3—C8	176.8 (3)	C10—Ru3—C9—O9	−2 (14)
C6—Ru2—Ru3—C7	−166.4 (4)	C8—Ru3—C9—O9	−102 (14)
C5—Ru2—Ru3—C7	−75.1 (4)	C7—Ru3—C9—O9	120 (13)
C4—Ru2—Ru3—C7	63 (3)	Ru2—Ru3—C9—O9	160 (14)
N2—Ru2—Ru3—C7	19.9 (4)	Ru1—Ru3—C9—O9	99 (14)
Ru1—Ru2—Ru3—C7	86.3 (3)	C8—Ru3—C10—O10	−60 (21)
C6—Ru2—Ru3—C9	17.2 (5)	C7—Ru3—C10—O10	31 (21)
C5—Ru2—Ru3—C9	108.5 (5)	C9—Ru3—C10—O10	−154 (21)
C4—Ru2—Ru3—C9	−114 (3)	Ru2—Ru3—C10—O10	114 (20)
N2—Ru2—Ru3—C9	−156.5 (4)	Ru1—Ru3—C10—O10	116 (21)
Ru1—Ru2—Ru3—C9	−90.1 (4)	C12—Ru4—C11—O11	73 (21)
C6—Ru2—Ru3—Ru1	107.4 (3)	C13—Ru4—C11—O11	−24 (21)
C5—Ru2—Ru3—Ru1	−161.4 (3)	N3—Ru4—C11—O11	−145 (20)
C4—Ru2—Ru3—Ru1	−24 (3)	Ru6—Ru4—C11—O11	161 (21)
N2—Ru2—Ru3—Ru1	−66.4 (2)	Ru5—Ru4—C11—O11	−142 (21)
C1—Ru1—Ru3—C10	72.5 (5)	C11—Ru4—C12—O12	104 (100)
C2—Ru1—Ru3—C10	−20.3 (5)	C13—Ru4—C12—O12	−163 (100)
C3—Ru1—Ru3—C10	−153 (5)	N3—Ru4—C12—O12	−72 (100)
N1—Ru1—Ru3—C10	−114.4 (4)	Ru6—Ru4—C12—O12	17 (100)
Ru2—Ru1—Ru3—C10	−179.3 (3)	Ru5—Ru4—C12—O12	−13 (100)
C1—Ru1—Ru3—C8	−117.0 (9)	C11—Ru4—C13—O13	24 (15)
C2—Ru1—Ru3—C8	150.2 (9)	C12—Ru4—C13—O13	−68 (15)
C3—Ru1—Ru3—C8	18 (5)	N3—Ru4—C13—O13	−162 (15)
N1—Ru1—Ru3—C8	56.1 (9)	Ru6—Ru4—C13—O13	116 (15)
Ru2—Ru1—Ru3—C8	−8.8 (9)	Ru5—Ru4—C13—O13	132 (15)
C1—Ru1—Ru3—C7	162.9 (4)	C16—Ru5—C14—O14	−52 (15)
C2—Ru1—Ru3—C7	70.1 (4)	C15—Ru5—C14—O14	39 (15)
C3—Ru1—Ru3—C7	−62 (5)	H2—Ru5—C14—O14	−145.8
N1—Ru1—Ru3—C7	−24.0 (4)	N4—Ru5—C14—O14	135 (15)
Ru2—Ru1—Ru3—C7	−88.9 (3)	Ru6—Ru5—C14—O14	174 (10)
C1—Ru1—Ru3—C9	−19.1 (4)	Ru4—Ru5—C14—O14	−161 (15)
C2—Ru1—Ru3—C9	−111.9 (4)	C16—Ru5—C15—O15	−10 (36)
C3—Ru1—Ru3—C9	116 (5)	H2—Ru5—C15—O15	104.5
N1—Ru1—Ru3—C9	154.0 (4)	C14—Ru5—C15—O15	−101 (36)
Ru2—Ru1—Ru3—C9	89.1 (3)	N4—Ru5—C15—O15	169 (36)
C1—Ru1—Ru3—Ru2	−108.2 (3)	Ru6—Ru5—C15—O15	82 (36)
C2—Ru1—Ru3—Ru2	159.0 (3)	Ru4—Ru5—C15—O15	107 (36)
C3—Ru1—Ru3—Ru2	26 (5)	C15—Ru5—C16—O16	−109 (14)
N1—Ru1—Ru3—Ru2	64.9 (2)	H2—Ru5—C16—O16	81.5
C11—Ru4—Ru5—C16	5.2 (5)	C14—Ru5—C16—O16	−10 (14)
C12—Ru4—Ru5—C16	117.3 (7)	N4—Ru5—C16—O16	82 (15)
C13—Ru4—Ru5—C16	−96.0 (5)	Ru6—Ru5—C16—O16	167 (14)
N3—Ru4—Ru5—C16	−175.2 (4)	Ru4—Ru5—C16—O16	108 (14)
Ru6—Ru4—Ru5—C16	82.3 (3)	C20—Ru6—C17—O17	42 (9)
C11—Ru4—Ru5—C15	−106.1 (6)	C18—Ru6—C17—O17	−56 (9)
C12—Ru4—Ru5—C15	6.0 (8)	C19—Ru6—C17—O17	170 (8)
C13—Ru4—Ru5—C15	152.7 (6)	Ru5—Ru6—C17—O17	−158 (9)
N3—Ru4—Ru5—C15	73.5 (6)	Ru4—Ru6—C17—O17	140 (9)
Ru6—Ru4—Ru5—C15	−29.0 (5)	C20—Ru6—C18—O18	−23 (22)
C11—Ru4—Ru5—H2	73.0	C19—Ru6—C18—O18	−116 (22)
C12—Ru4—Ru5—H2	−174.9	C17—Ru6—C18—O18	70 (22)
C13—Ru4—Ru5—H2	−28.2	Ru5—Ru6—C18—O18	158 (22)
N3—Ru4—Ru5—H2	−107.4	Ru4—Ru6—C18—O18	148 (21)
Ru6—Ru4—Ru5—H2	150.1	C20—Ru6—C19—O19	−25 (10)
C11—Ru4—Ru5—C14	104.6 (6)	C18—Ru6—C19—O19	73 (10)
C12—Ru4—Ru5—C14	−143.3 (8)	C17—Ru6—C19—O19	−154 (9)
C13—Ru4—Ru5—C14	3.4 (6)	Ru5—Ru6—C19—O19	174 (100)
N3—Ru4—Ru5—C14	−75.8 (5)	Ru4—Ru6—C19—O19	−124 (10)
Ru6—Ru4—Ru5—C14	−178.2 (4)	C18—Ru6—C20—O20	−12 (100)
C11—Ru4—Ru5—N4	−178.2 (4)	C19—Ru6—C20—O20	81 (100)
C12—Ru4—Ru5—N4	−66.1 (7)	C17—Ru6—C20—O20	−105 (100)
C13—Ru4—Ru5—N4	80.5 (4)	Ru5—Ru6—C20—O20	167 (100)
N3—Ru4—Ru5—N4	1.4 (4)	Ru4—Ru6—C20—O20	171 (100)
Ru6—Ru4—Ru5—N4	−101.1 (3)	N1—C21—C22—C23	0.8 (12)
C11—Ru4—Ru5—Ru6	−77.1 (3)	C21—C22—C23—N2	−0.2 (11)
C12—Ru4—Ru5—Ru6	35.0 (6)	N3—C24—C25—C26	−0.1 (14)
C13—Ru4—Ru5—Ru6	−178.3 (4)	C24—C25—C26—N4	0.0 (14)
N3—Ru4—Ru5—Ru6	102.5 (3)	C29ⁱ—C27—C28—C29	45 (3)
C16—Ru5—Ru6—C20	−102.8 (11)	C27—C28—C29—C27ⁱ	−54 (3)
C15—Ru5—Ru6—C20	166.0 (11)	C22—C21—N1—N2	−1.2 (11)
H2—Ru5—Ru6—C20	−9.6	C22—C21—N1—Ru1	178.8 (7)
C14—Ru5—Ru6—C20	31 (6)	C1—Ru1—N1—C21	−147 (3)
N4—Ru5—Ru6—C20	70.0 (11)	C2—Ru1—N1—C21	41.4 (11)
Ru4—Ru5—Ru6—C20	4.6 (10)	C3—Ru1—N1—C21	−56.0 (10)
C16—Ru5—Ru6—C18	75.7 (5)	Ru3—Ru1—N1—C21	126.2 (10)
C15—Ru5—Ru6—C18	−15.4 (5)	Ru2—Ru1—N1—C21	−176.7 (11)
H2—Ru5—Ru6—C18	169.0	C1—Ru1—N1—N2	33 (3)
C14—Ru5—Ru6—C18	−151 (6)	C2—Ru1—N1—N2	−138.7 (6)
N4—Ru5—Ru6—C18	−111.4 (4)	C3—Ru1—N1—N2	124.0 (6)
Ru4—Ru5—Ru6—C18	−176.9 (3)	Ru3—Ru1—N1—N2	−53.8 (6)
C16—Ru5—Ru6—C19	−15.9 (5)	Ru2—Ru1—N1—N2	3.3 (5)
C15—Ru5—Ru6—C19	−107.0 (5)	C21—N1—N2—C23	1.1 (10)
H2—Ru5—Ru6—C19	77.4	Ru1—N1—N2—C23	−178.9 (6)
C14—Ru5—Ru6—C19	118 (6)	C21—N1—N2—Ru2	175.4 (6)
N4—Ru5—Ru6—C19	157.0 (4)	Ru1—N1—N2—Ru2	−4.6 (7)
Ru4—Ru5—Ru6—C19	91.5 (3)	C22—C23—N2—N1	−0.5 (11)
C16—Ru5—Ru6—C17	168.3 (5)	C22—C23—N2—Ru2	−172.2 (8)
C15—Ru5—Ru6—C17	77.2 (5)	C6—Ru2—N2—N1	−6 (4)
H2—Ru5—Ru6—C17	−98.4	C5—Ru2—N2—N1	147.2 (6)
C14—Ru5—Ru6—C17	−58 (6)	C4—Ru2—N2—N1	−114.9 (6)
N4—Ru5—Ru6—C17	−18.8 (4)	Ru3—Ru2—N2—N1	61.3 (6)
Ru4—Ru5—Ru6—C17	−84.3 (3)	Ru1—Ru2—N2—N1	3.3 (5)
C16—Ru5—Ru6—Ru4	−107.4 (3)	C6—Ru2—N2—C23	165 (3)
C15—Ru5—Ru6—Ru4	161.5 (3)	C5—Ru2—N2—C23	−41.4 (11)
H2—Ru5—Ru6—Ru4	−14.1	C4—Ru2—N2—C23	56.5 (11)
C14—Ru5—Ru6—Ru4	26 (6)	Ru3—Ru2—N2—C23	−127.3 (11)
N4—Ru5—Ru6—Ru4	65.5 (2)	Ru1—Ru2—N2—C23	174.7 (11)
C11—Ru4—Ru6—C20	−69.3 (5)	C25—C24—N3—N4	0.1 (13)
C12—Ru4—Ru6—C20	22.4 (5)	C25—C24—N3—Ru4	179.9 (9)
C13—Ru4—Ru6—C20	−162 (4)	C11—Ru4—N3—N4	1 (4)
N3—Ru4—Ru6—C20	116.4 (4)	C12—Ru4—N3—N4	142.8 (7)
Ru5—Ru4—Ru6—C20	−178.4 (4)	C13—Ru4—N3—N4	−120.1 (7)
C11—Ru4—Ru6—C18	119.9 (12)	Ru6—Ru4—N3—N4	54.7 (7)
C12—Ru4—Ru6—C18	−148.3 (12)	Ru5—Ru4—N3—N4	−2.1 (6)
C13—Ru4—Ru6—C18	27 (4)	C11—Ru4—N3—C24	−179 (84)
N3—Ru4—Ru6—C18	−54.4 (11)	C12—Ru4—N3—C24	−37.0 (12)
Ru5—Ru4—Ru6—C18	10.8 (11)	C13—Ru4—N3—C24	60.2 (12)
C11—Ru4—Ru6—C19	23.4 (5)	Ru6—Ru4—N3—C24	−125.0 (12)
C12—Ru4—Ru6—C19	115.2 (5)	Ru5—Ru4—N3—C24	178.1 (12)
C13—Ru4—Ru6—C19	−69 (4)	C25—C26—N4—N3	0.0 (13)
N3—Ru4—Ru6—C19	−150.9 (4)	C25—C26—N4—Ru5	176.0 (9)
Ru5—Ru4—Ru6—C19	−85.7 (3)	C24—N3—N4—C26	−0.1 (12)
C11—Ru4—Ru6—C17	−160.6 (5)	Ru4—N3—N4—C26	−179.9 (7)
C12—Ru4—Ru6—C17	−68.8 (5)	C24—N3—N4—Ru5	−177.3 (7)
C13—Ru4—Ru6—C17	107 (4)	Ru4—N3—N4—Ru5	2.9 (8)
N3—Ru4—Ru6—C17	25.1 (4)	C16—Ru5—N4—C26	−150 (3)
Ru5—Ru4—Ru6—C17	90.3 (3)	C15—Ru5—N4—C26	40.6 (12)
C11—Ru4—Ru6—Ru5	109.1 (4)	H2—Ru5—N4—C26	−150.0
C12—Ru4—Ru6—Ru5	−159.1 (4)	C14—Ru5—N4—C26	−57.9 (12)
C13—Ru4—Ru6—Ru5	17 (4)	Ru6—Ru5—N4—C26	124.3 (12)
N3—Ru4—Ru6—Ru5	−65.2 (2)	Ru4—Ru5—N4—C26	−178.0 (12)
C2—Ru1—C1—O1	−119 (15)	C16—Ru5—N4—N3	26 (4)
C3—Ru1—C1—O1	−22 (15)	C15—Ru5—N4—N3	−143.5 (7)
N1—Ru1—C1—O1	69 (16)	H2—Ru5—N4—N3	26.0
Ru3—Ru1—C1—O1	156 (15)	C14—Ru5—N4—N3	118.0 (7)
Ru2—Ru1—C1—O1	98 (15)	Ru6—Ru5—N4—N3	−59.7 (6)
C1—Ru1—C2—O2	−26 (100)	Ru4—Ru5—N4—N3	−2.1 (6)
C3—Ru1—C2—O2	−118 (100)

Symmetry code: (i) −x+1/2, −y+5/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Ru₃H(C₃H₃N₂)(CO)₁₀]·C_1.50H₃
M_r	672.43
Crystal system, space group	Monoclinic, I2/a
Temperature (K)	153
a, b, c (Å)	14.2248 (11), 9.1670 (5), 59.834 (5)
β (°)	90.380 (9)
V (Å³)	7802.1 (10)
Z	16
Radiation type	Mo Kα
µ (mm⁻¹)	2.35
Crystal size (mm)	0.50 × 0.45 × 0.40

Data collection
Diffractometer	Stoe IPDS diffractometer
Absorption correction	Multi-scan (Blessing, 1995)
T_min, T_max	0.224, 0.251
No. of measured, independent and observed [I > 2σ(I)] reflections	18544, 4743, 4474
R_int	0.041
θ_max (°)	22.3
(sin θ/λ)_max (Å⁻¹)	0.535

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.107, 1.36
No. of reflections	4743
No. of parameters	532
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
	w = 1/[σ²(F_o²) + 252.1712P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.00, −0.81

Computer programs: EXPOSE (Stoe & Cie, 2000), CELL (Stoe & Cie, 2000), INTEGRATE (Stoe & Cie, 2000), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.

Selected geometric parameters (Å, º) top

Ru1—N1	2.097 (8)	Ru4—H2	1.55
Ru1—Ru3	2.8544 (12)	Ru5—N4	2.115 (9)
Ru1—Ru2	2.8992 (11)	Ru5—Ru6	2.8357 (12)
Ru1—H1	1.69	Ru5—H2	1.92
Ru2—N2	2.103 (8)	C21—N1	1.336 (13)
Ru2—Ru3	2.8509 (11)	C23—N2	1.356 (13)
Ru2—H1	1.75	C24—N3	1.344 (14)
Ru4—N3	2.094 (9)	C26—N4	1.338 (15)
Ru4—Ru6	2.8457 (12)	N1—N2	1.351 (11)
Ru4—Ru5	2.9124 (12)	N3—N4	1.344 (12)

N1—Ru1—Ru2	68.1 (2)	N4—Ru5—Ru4	67.9 (2)
Ru3—Ru1—Ru2	59.40 (3)	Ru6—Ru5—Ru4	59.33 (3)
N2—Ru2—Ru1	68.6 (2)	Ru5—Ru6—Ru4	61.68 (3)
Ru3—Ru2—Ru1	59.52 (3)	N2—N1—Ru1	112.3 (6)
Ru2—Ru3—Ru1	61.08 (3)	N1—N2—Ru2	110.8 (6)
N3—Ru4—Ru5	68.3 (2)	N4—N3—Ru4	112.2 (6)
Ru6—Ru4—Ru5	58.99 (3)	N3—N4—Ru5	111.5 (7)

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