Structural and electrochemical comparison of trinuclear ruthenium oxo clusters [Ru₃(OAc)₆O(L)₃]⁺ and [Ru₃(OAc)₆O(L)₂(CO)] (L = imidazole, benz­imidazole, and 4-phenyl­pyridine)

The triruthenium oxo clusters [Ru₃(OAc)₆O(L)₃]⁺ and [Ru₃(OAc)₆O(L)₂(CO)] possess unique electronic characteristics that vary based on the ligands L. Here we report an investigation of the structural, electrochemical, and optical properties of clusters with imidazole, benzimidazole, and 4-phenyl­pyridine ligands. The complexes [Ru₃(OAc)₆O(L)₃]⁺ [1⁺: L = imidazole (im); 2⁺: L = benzimidazole (benzim); 3⁺: L = 4-phenyl­pyridine (4PP)] and [Ru₃(OAc)₆O(L)₂(CO)] (1-CO and 3-CO) were synthesized by reaction of either [Ru₃(OAc)₆O(MeOH)₃]⁺ or [Ru₃(OAc)₆O(MeOH)₂(CO)], respectively, with the corresponding heterocycle. We further discovered that [3]OAc could be reduced to the mixed-valence neutral state 3 by refluxing the complex under nitro­gen in methanol. Single-crystal X-ray structure analysis of hexa-μ₂-acetato-μ₃-oxido-tris­(1H-imidazole)­triruthenium hexa­fluoro­phosphate aceto­nitrile hemisolvate, [Ru₃(C₂H₃O₂)₆O(C₃H₄N₂)₃]PF₆·0.5CH₃CN, [1]PF₆, hexa-μ₂-ace­tato-carbonyl­bis­(1H-imidazole)-μ₃-oxido-triruthenium methanol monosolvate, [Ru₃(C₂H₃O₂)₆O(C₃H₄N₂)(CO)]·CH₃OH, 1-CO, hexa-μ₂-acetato-μ₃-oxido-tris­(4-phenyl­pyridine)­triruthenium penta­hydrate, [Ru₃(C₂H₃O₂)₆O(C₁₁H₉N)₃]·5H₂O, 3, and hexa-μ₂-acetato-carbonyl-μ₃-oxido-bis­(4-phenyl­pyridine)­tri­ru­thenium methanol monosolvate, [Ru₃(C₂H₃O₂)₆O(C₁₁H₉N)₂(CO)]·CH₃OH, 3-CO, show the expected triruthenium μ₃-oxo core and N-coordination of the ligands. Cyclic voltammetry revealed quasi-reversible and irreversible redox couples in [1]PF₆, 1-CO, and [2]PF₆, while [3]PF₆ and 3-CO exhibit reversible redox couples. The optical properties of these richly colored species were investigated using UV–Vis spectroscopy.

Computing details

For all structures, data collection: COSMO (Bruker, 2009); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXT (Sheldrick, 2015a). Program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015b) for ae218b; SHELXL2014 (Sheldrick, 2015b) for ae218d, ae418a; SHELXL2014 (Sheldrick, 2015a) for ae817a. For all structures, molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Hexa-µ₂-acetato-carbonylbis(1H-imidazole)-µ₃-oxido-triruthenium (ae218b)

Crystal data

[Ru3(C2H3O2)6O(C3H4N2)(CO)]·CH4O	F(000) = 1720
Mr = 869.69	Dx = 1.789 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 9.6807 (6) Å	Cell parameters from 9874 reflections
b = 18.5596 (12) Å	θ = 2.2–27.5°
c = 18.5805 (12) Å	µ = 1.45 mm^−1
β = 104.746 (1)°	T = 173 K
V = 3228.4 (4) Å^3	Plate, blue
Z = 4	0.24 × 0.22 × 0.05 mm

Data collection

Bruker APEXII CCD diffractometer	7410 independent reflections
Radiation source: sealed tube	6119 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.051
Detector resolution: 8.36 pixels mm^-1	θmax = 27.5°, θmin = 1.6°
ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −24→24
Tmin = 0.024, Tmax = 0.047	l = −24→24
59780 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.042	H-atom parameters constrained
wR(F^2) = 0.123	w = 1/[σ^2(Fo^2) + (0.0731P)^2 + 3.9385P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max = 0.001
7410 reflections	Δρmax = 2.15 e Å^−3
407 parameters	Δρmin = −0.56 e Å^−3
0 restraints

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. The structure was refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008) incorporated in Olex2 (Dolomanov et al., 2009). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ru1	0.47767 (4)	0.62811 (2)	0.66768 (2)	0.02732 (10)
Ru2	0.40818 (3)	0.58165 (2)	0.82543 (2)	0.02553 (10)
Ru3	0.72472 (3)	0.52985 (2)	0.79256 (2)	0.02673 (10)
O1	0.5332 (3)	0.58171 (14)	0.76191 (15)	0.0261 (6)
O2	0.2933 (3)	0.56822 (17)	0.63426 (16)	0.0354 (7)
O3	0.2238 (3)	0.57232 (17)	0.74073 (17)	0.0343 (6)
O4	0.3600 (3)	0.70884 (15)	0.70121 (16)	0.0327 (6)
O5	0.3897 (3)	0.69139 (15)	0.82375 (15)	0.0312 (6)
O6	0.5647 (3)	0.59419 (17)	0.92281 (16)	0.0337 (6)
O7	0.7761 (3)	0.58444 (16)	0.89450 (16)	0.0336 (6)
O8	0.4082 (3)	0.47271 (15)	0.83557 (18)	0.0349 (7)
O9	0.6338 (3)	0.44319 (15)	0.83507 (16)	0.0317 (6)
O10	0.8271 (3)	0.61362 (17)	0.75165 (18)	0.0359 (7)
O11	0.6565 (3)	0.69120 (16)	0.69124 (17)	0.0356 (7)
O12	0.6819 (3)	0.47445 (15)	0.69239 (16)	0.0344 (7)
O13	0.5794 (3)	0.55993 (16)	0.61050 (16)	0.0355 (7)
O14	0.9880 (4)	0.4380 (2)	0.8278 (2)	0.0527 (9)
N1	0.4155 (4)	0.68289 (19)	0.56596 (19)	0.0354 (8)
N2	0.4148 (6)	0.7414 (2)	0.4649 (2)	0.0568 (13)
H2	0.4460	0.7611	0.4289	0.068*
N3	0.2692 (4)	0.58160 (18)	0.89548 (19)	0.0293 (7)
N4	0.0713 (4)	0.5896 (2)	0.9314 (2)	0.0339 (8)
H4	−0.0193	0.5968	0.9296	0.041*
C1	0.4944 (6)	0.7033 (3)	0.5223 (2)	0.0443 (12)
H1	0.5932	0.6928	0.5298	0.053*
C2	0.2809 (8)	0.7443 (3)	0.4714 (3)	0.0562 (15)
H2A	0.2016	0.7669	0.4384	0.067*
C3	0.2816 (6)	0.7086 (3)	0.5344 (3)	0.0488 (13)
H3	0.2009	0.7022	0.5541	0.059*
C4	0.1315 (4)	0.5954 (2)	0.8741 (2)	0.0318 (9)
H4A	0.0814	0.6078	0.8247	0.038*
C5	0.1760 (5)	0.5704 (3)	0.9933 (3)	0.0368 (10)
H5	0.1655	0.5621	1.0420	0.044*
C6	0.2973 (5)	0.5658 (3)	0.9701 (2)	0.0365 (9)
H6	0.3885	0.5534	1.0009	0.044*
C7	0.2031 (5)	0.5606 (3)	0.6725 (3)	0.0375 (10)
C8	0.0559 (6)	0.5354 (4)	0.6320 (3)	0.0573 (15)
H8A	0.0583	0.4836	0.6221	0.086*
H8B	0.0243	0.5614	0.5848	0.086*
H8C	−0.0107	0.5447	0.6628	0.086*
C9	0.3494 (4)	0.7287 (2)	0.7633 (2)	0.0310 (8)
C10	0.2831 (6)	0.8011 (2)	0.7690 (3)	0.0401 (10)
H10A	0.2077	0.7959	0.7952	0.060*
H10B	0.2420	0.8201	0.7189	0.060*
H10C	0.3564	0.8343	0.7965	0.060*
C11	0.6983 (5)	0.5996 (2)	0.9375 (2)	0.0317 (9)
C12	0.7727 (5)	0.6259 (3)	1.0145 (3)	0.0488 (13)
H12A	0.8763	0.6212	1.0222	0.073*
H12B	0.7416	0.5971	1.0517	0.073*
H12C	0.7485	0.6766	1.0195	0.073*
C13	0.5108 (5)	0.4288 (2)	0.8420 (2)	0.0336 (9)
C14	0.4822 (6)	0.3524 (2)	0.8607 (3)	0.0421 (11)
H14A	0.5366	0.3194	0.8371	0.063*
H14B	0.3800	0.3420	0.8425	0.063*
H14C	0.5115	0.3458	0.9148	0.063*
C15	0.7835 (5)	0.6713 (2)	0.7189 (3)	0.0381 (10)
C16	0.8979 (7)	0.7244 (4)	0.7108 (4)	0.072 (2)
H16A	0.9459	0.7439	0.7598	0.108*
H16B	0.8537	0.7638	0.6778	0.108*
H16C	0.9678	0.6997	0.6896	0.108*
C17	0.6406 (5)	0.5005 (2)	0.6282 (2)	0.0323 (9)
C18	0.6709 (6)	0.4565 (3)	0.5655 (3)	0.0434 (11)
H18A	0.7254	0.4856	0.5384	0.065*
H18B	0.5805	0.4415	0.5315	0.065*
H18C	0.7265	0.4137	0.5860	0.065*
C19	0.8921 (5)	0.4766 (2)	0.8162 (2)	0.0342 (9)
O15	0.8235 (14)	0.8141 (6)	1.0013 (7)	0.097 (4)	0.5
H15	0.7702	0.8476	0.9801	0.145*	0.5
C21	0.9033 (18)	0.7871 (10)	0.9528 (16)	0.141 (10)	0.5
H21A	0.8402	0.7812	0.9028	0.211*	0.5
H21B	0.9449	0.7404	0.9712	0.211*	0.5
H21C	0.9798	0.8210	0.9510	0.211*	0.5
O16	0.6812 (9)	0.9193 (4)	0.9102 (4)	0.0494 (18)	0.5
H16	0.7457	0.9505	0.9148	0.074*	0.5
C22	0.6546 (13)	0.8890 (6)	0.8402 (6)	0.053 (3)	0.5
H22A	0.5612	0.9052	0.8103	0.080*	0.5
H22B	0.6548	0.8364	0.8444	0.080*	0.5
H22C	0.7290	0.9040	0.8160	0.080*	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.03264 (19)	0.02588 (17)	0.02346 (17)	0.00168 (12)	0.00718 (13)	0.00102 (11)
Ru2	0.02497 (17)	0.02691 (17)	0.02479 (17)	0.00049 (11)	0.00646 (13)	0.00183 (11)
Ru3	0.02659 (18)	0.02874 (18)	0.02511 (17)	0.00108 (12)	0.00703 (13)	0.00105 (12)
O1	0.0274 (14)	0.0275 (13)	0.0236 (13)	0.0001 (11)	0.0071 (11)	−0.0001 (10)
O2	0.0383 (17)	0.0388 (16)	0.0285 (15)	−0.0011 (13)	0.0072 (13)	−0.0043 (12)
O3	0.0303 (15)	0.0406 (17)	0.0299 (15)	−0.0001 (12)	0.0037 (12)	0.0000 (13)
O4	0.0403 (17)	0.0311 (15)	0.0272 (14)	0.0041 (12)	0.0094 (12)	−0.0004 (12)
O5	0.0405 (17)	0.0273 (14)	0.0269 (14)	−0.0017 (12)	0.0103 (12)	−0.0012 (11)
O6	0.0278 (15)	0.0460 (17)	0.0265 (14)	0.0007 (13)	0.0055 (12)	0.0015 (13)
O7	0.0296 (15)	0.0424 (17)	0.0291 (15)	0.0003 (12)	0.0080 (12)	−0.0061 (12)
O8	0.0319 (16)	0.0277 (15)	0.0477 (18)	0.0014 (11)	0.0147 (14)	0.0056 (13)
O9	0.0337 (16)	0.0272 (14)	0.0353 (16)	0.0025 (12)	0.0106 (12)	0.0058 (12)
O10	0.0318 (16)	0.0381 (16)	0.0396 (17)	−0.0018 (13)	0.0124 (13)	0.0068 (13)
O11	0.0365 (17)	0.0314 (15)	0.0392 (17)	−0.0002 (13)	0.0099 (13)	0.0046 (13)
O12	0.0438 (18)	0.0314 (15)	0.0287 (15)	0.0075 (13)	0.0107 (13)	0.0003 (12)
O13	0.0467 (18)	0.0337 (15)	0.0275 (15)	0.0089 (14)	0.0118 (13)	−0.0005 (12)
O14	0.0367 (19)	0.052 (2)	0.066 (2)	0.0146 (16)	0.0059 (17)	−0.0010 (18)
N1	0.054 (2)	0.0270 (17)	0.0252 (17)	0.0045 (16)	0.0101 (16)	−0.0004 (14)
N2	0.099 (4)	0.041 (2)	0.028 (2)	−0.011 (2)	0.012 (2)	0.0075 (17)
N3	0.0280 (17)	0.0326 (18)	0.0275 (17)	0.0006 (13)	0.0075 (14)	0.0022 (14)
N4	0.0236 (17)	0.045 (2)	0.0331 (19)	−0.0027 (15)	0.0081 (14)	−0.0026 (16)
C1	0.068 (3)	0.037 (2)	0.027 (2)	−0.009 (2)	0.009 (2)	0.0003 (18)
C2	0.082 (4)	0.044 (3)	0.036 (3)	0.017 (3)	0.002 (3)	0.005 (2)
C3	0.061 (3)	0.051 (3)	0.033 (2)	0.020 (2)	0.007 (2)	0.005 (2)
C4	0.028 (2)	0.034 (2)	0.032 (2)	0.0011 (16)	0.0064 (17)	0.0010 (17)
C5	0.034 (2)	0.045 (3)	0.033 (2)	−0.0017 (19)	0.0122 (18)	0.0064 (19)
C6	0.033 (2)	0.046 (2)	0.032 (2)	0.0045 (19)	0.0119 (18)	0.0061 (19)
C7	0.036 (2)	0.038 (2)	0.035 (2)	−0.0006 (19)	0.0037 (19)	−0.0024 (18)
C8	0.042 (3)	0.083 (4)	0.043 (3)	−0.009 (3)	0.002 (2)	−0.007 (3)
C9	0.031 (2)	0.030 (2)	0.033 (2)	−0.0007 (16)	0.0090 (17)	−0.0001 (16)
C10	0.055 (3)	0.033 (2)	0.038 (2)	0.007 (2)	0.022 (2)	0.0027 (18)
C11	0.029 (2)	0.037 (2)	0.028 (2)	0.0009 (17)	0.0047 (16)	0.0005 (17)
C12	0.031 (2)	0.077 (4)	0.036 (3)	−0.001 (2)	0.005 (2)	−0.020 (2)
C13	0.043 (2)	0.031 (2)	0.029 (2)	0.0007 (18)	0.0135 (18)	0.0015 (16)
C14	0.051 (3)	0.028 (2)	0.053 (3)	0.0017 (19)	0.024 (2)	0.005 (2)
C15	0.042 (3)	0.036 (2)	0.037 (2)	−0.0046 (19)	0.0117 (19)	0.0029 (19)
C16	0.048 (3)	0.062 (4)	0.106 (5)	−0.010 (3)	0.017 (3)	0.034 (4)
C17	0.034 (2)	0.033 (2)	0.029 (2)	−0.0045 (17)	0.0066 (17)	−0.0034 (17)
C18	0.056 (3)	0.040 (2)	0.033 (2)	0.011 (2)	0.009 (2)	−0.0066 (19)
C19	0.034 (2)	0.036 (2)	0.033 (2)	0.0018 (18)	0.0096 (18)	0.0000 (17)
O15	0.102 (9)	0.082 (7)	0.106 (9)	0.021 (6)	0.027 (7)	0.044 (6)
C21	0.065 (10)	0.100 (13)	0.28 (3)	0.028 (9)	0.088 (16)	0.081 (17)
O16	0.067 (5)	0.035 (4)	0.046 (4)	−0.001 (3)	0.015 (4)	0.010 (3)
C22	0.057 (7)	0.057 (6)	0.045 (6)	−0.015 (5)	0.014 (5)	−0.016 (5)

Geometric parameters (Å, º)

Ru1—O1	1.902 (3)	C2—H2A	0.9500
Ru1—O2	2.060 (3)	C2—C3	1.344 (7)
Ru1—O4	2.072 (3)	C3—H3	0.9500
Ru1—O11	2.043 (3)	C4—H4A	0.9500
Ru1—O13	2.057 (3)	C5—H5	0.9500
Ru1—N1	2.095 (4)	C5—C6	1.352 (6)
Ru2—O1	1.893 (3)	C6—H6	0.9500
Ru2—O3	2.064 (3)	C7—C8	1.506 (7)
Ru2—O5	2.044 (3)	C8—H8A	0.9800
Ru2—O6	2.056 (3)	C8—H8B	0.9800
Ru2—O8	2.031 (3)	C8—H8C	0.9800
Ru2—N3	2.097 (3)	C9—C10	1.504 (6)
Ru3—O1	2.038 (3)	C10—H10A	0.9800
Ru3—O7	2.093 (3)	C10—H10B	0.9800
Ru3—O9	2.083 (3)	C10—H10C	0.9800
Ru3—O10	2.088 (3)	C11—C12	1.510 (6)
Ru3—O12	2.074 (3)	C12—H12A	0.9800
Ru3—C19	1.853 (5)	C12—H12B	0.9800
O2—C7	1.267 (6)	C12—H12C	0.9800
O3—C7	1.251 (5)	C13—C14	1.503 (6)
O4—C9	1.241 (5)	C14—H14A	0.9800
O5—C9	1.292 (5)	C14—H14B	0.9800
O6—C11	1.256 (5)	C14—H14C	0.9800
O7—C11	1.261 (5)	C15—C16	1.517 (7)
O8—C13	1.267 (5)	C16—H16A	0.9800
O9—C13	1.259 (5)	C16—H16B	0.9800
O10—C15	1.251 (5)	C16—H16C	0.9800
O11—C15	1.261 (6)	C17—C18	1.512 (6)
O12—C17	1.254 (5)	C18—H18A	0.9800
O13—C17	1.255 (5)	C18—H18B	0.9800
O14—C19	1.148 (6)	C18—H18C	0.9800
N1—C1	1.305 (6)	O15—H15	0.8400
N1—C3	1.365 (7)	O15—C21	1.42 (2)
N2—H2	0.8800	C21—H21A	0.9800
N2—C1	1.346 (7)	C21—H21B	0.9800
N2—C2	1.333 (8)	C21—H21C	0.9800
N3—C4	1.316 (5)	O16—H16	0.8400
N3—C6	1.375 (5)	O16—C22	1.380 (12)
N4—H4	0.8800	C22—H22A	0.9800
N4—C4	1.342 (6)	C22—H22B	0.9800
N4—C5	1.372 (6)	C22—H22C	0.9800
C1—H1	0.9500
O1—Ru1—O2	93.06 (12)	C2—C3—H3	125.1
O1—Ru1—O4	95.67 (11)	N3—C4—N4	110.8 (4)
O1—Ru1—O11	92.12 (12)	N3—C4—H4A	124.6
O1—Ru1—O13	97.86 (11)	N4—C4—H4A	124.6
O1—Ru1—N1	177.80 (12)	N4—C5—H5	127.3
O2—Ru1—O4	88.87 (12)	C6—C5—N4	105.4 (4)
O2—Ru1—N1	87.81 (14)	C6—C5—H5	127.3
O4—Ru1—N1	82.33 (13)	N3—C6—H6	125.0
O11—Ru1—O2	174.79 (12)	C5—C6—N3	110.0 (4)
O11—Ru1—O4	91.26 (12)	C5—C6—H6	125.0
O11—Ru1—O13	88.40 (13)	O2—C7—C8	117.0 (4)
O11—Ru1—N1	87.04 (14)	O3—C7—O2	126.4 (4)
O13—Ru1—O2	90.26 (13)	O3—C7—C8	116.6 (4)
O13—Ru1—O4	166.47 (12)	C7—C8—H8A	109.5
O13—Ru1—N1	84.15 (13)	C7—C8—H8B	109.5
O1—Ru2—O3	95.19 (12)	C7—C8—H8C	109.5
O1—Ru2—O5	93.27 (11)	H8A—C8—H8B	109.5
O1—Ru2—O6	95.97 (12)	H8A—C8—H8C	109.5
O1—Ru2—O8	94.23 (12)	H8B—C8—H8C	109.5
O1—Ru2—N3	179.81 (13)	O4—C9—O5	124.8 (4)
O3—Ru2—N3	84.63 (13)	O4—C9—C10	117.9 (4)
O5—Ru2—O3	90.95 (12)	O5—C9—C10	117.2 (4)
O5—Ru2—O6	86.71 (12)	C9—C10—H10A	109.5
O5—Ru2—N3	86.71 (12)	C9—C10—H10B	109.5
O6—Ru2—O3	168.72 (12)	C9—C10—H10C	109.5
O6—Ru2—N3	84.22 (13)	H10A—C10—H10B	109.5
O8—Ru2—O3	88.10 (13)	H10A—C10—H10C	109.5
O8—Ru2—O5	172.50 (12)	H10B—C10—H10C	109.5
O8—Ru2—O6	92.78 (13)	O6—C11—O7	126.4 (4)
O8—Ru2—N3	85.80 (13)	O6—C11—C12	116.6 (4)
O1—Ru3—O7	90.81 (11)	O7—C11—C12	117.0 (4)
O1—Ru3—O9	91.64 (11)	C11—C12—H12A	109.5
O1—Ru3—O10	91.65 (11)	C11—C12—H12B	109.5
O1—Ru3—O12	91.35 (11)	C11—C12—H12C	109.5
O9—Ru3—O7	93.26 (12)	H12A—C12—H12B	109.5
O9—Ru3—O10	176.71 (12)	H12A—C12—H12C	109.5
O10—Ru3—O7	86.76 (12)	H12B—C12—H12C	109.5
O12—Ru3—O7	177.79 (12)	O8—C13—C14	116.3 (4)
O12—Ru3—O9	87.15 (12)	O9—C13—O8	126.4 (4)
O12—Ru3—O10	92.71 (12)	O9—C13—C14	117.3 (4)
C19—Ru3—O1	175.54 (16)	C13—C14—H14A	109.5
C19—Ru3—O7	92.95 (16)	C13—C14—H14B	109.5
C19—Ru3—O9	85.75 (16)	C13—C14—H14C	109.5
C19—Ru3—O10	90.96 (16)	H14A—C14—H14B	109.5
C19—Ru3—O12	84.91 (16)	H14A—C14—H14C	109.5
Ru1—O1—Ru3	119.67 (14)	H14B—C14—H14C	109.5
Ru2—O1—Ru1	119.92 (14)	O10—C15—O11	128.4 (4)
Ru2—O1—Ru3	120.39 (14)	O10—C15—C16	116.1 (4)
C7—O2—Ru1	124.0 (3)	O11—C15—C16	115.5 (4)
C7—O3—Ru2	132.2 (3)	C15—C16—H16A	109.5
C9—O4—Ru1	132.6 (3)	C15—C16—H16B	109.5
C9—O5—Ru2	123.6 (3)	C15—C16—H16C	109.5
C11—O6—Ru2	133.4 (3)	H16A—C16—H16B	109.5
C11—O7—Ru3	129.7 (3)	H16A—C16—H16C	109.5
C13—O8—Ru2	129.1 (3)	H16B—C16—H16C	109.5
C13—O9—Ru3	134.8 (3)	O12—C17—O13	127.1 (4)
C15—O10—Ru3	133.0 (3)	O12—C17—C18	116.5 (4)
C15—O11—Ru1	127.2 (3)	O13—C17—C18	116.4 (4)
C17—O12—Ru3	127.2 (3)	C17—C18—H18A	109.5
C17—O13—Ru1	131.4 (3)	C17—C18—H18B	109.5
C1—N1—Ru1	128.5 (4)	C17—C18—H18C	109.5
C1—N1—C3	105.9 (4)	H18A—C18—H18B	109.5
C3—N1—Ru1	125.5 (3)	H18A—C18—H18C	109.5
C1—N2—H2	125.6	H18B—C18—H18C	109.5
C2—N2—H2	125.6	O14—C19—Ru3	173.5 (4)
C2—N2—C1	108.9 (5)	C21—O15—H15	109.5
C4—N3—Ru2	125.0 (3)	O15—C21—H21A	109.5
C4—N3—C6	105.8 (4)	O15—C21—H21B	109.5
C6—N3—Ru2	129.2 (3)	O15—C21—H21C	109.5
C4—N4—H4	126.0	H21A—C21—H21B	109.5
C4—N4—C5	108.0 (4)	H21A—C21—H21C	109.5
C5—N4—H4	126.0	H21B—C21—H21C	109.5
N1—C1—N2	109.7 (5)	C22—O16—H16	109.5
N1—C1—H1	125.2	O16—C22—H22A	109.5
N2—C1—H1	125.2	O16—C22—H22B	109.5
N2—C2—H2A	127.2	O16—C22—H22C	109.5
N2—C2—C3	105.7 (5)	H22A—C22—H22B	109.5
C3—C2—H2A	127.2	H22A—C22—H22C	109.5
N1—C3—H3	125.1	H22B—C22—H22C	109.5
C2—C3—N1	109.8 (5)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···O5^i	0.88	2.09	2.858 (5)	146
N4—H4···O7^ii	0.88	1.93	2.766 (5)	157
O15—H15···O16	0.84	1.91	2.719 (12)	163

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x−1, y, z.

Hexa-µ₂-acetato-µ₃-oxido-tris(4-phenylpyridine)triruthenium pentahydrate (ae218d)

Crystal data

[Ru3(C2H3O2)6O(C11H9N)3]·5H2O	Z = 2
Mr = 1229.13	F(000) = 1244
Triclinic, P1	Dx = 1.572 Mg m^−3
a = 11.700 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 15.033 (5) Å	Cell parameters from 5429 reflections
c = 16.180 (5) Å	θ = 2.5–22.4°
α = 78.256 (4)°	µ = 0.93 mm^−1
β = 71.422 (3)°	T = 173 K
γ = 76.364 (3)°	Plate, brown
V = 2596.0 (14) Å^3	0.28 × 0.02 × 0.002 mm

Data collection

Bruker APEXII CCD diffractometer	10222 independent reflections
Radiation source: sealed tube	5227 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.155
Detector resolution: 8.36 pixels mm^-1	θmax = 26.2°, θmin = 1.3°
ω scans	h = −14→14
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −18→18
Tmin = 0.534, Tmax = 0.745	l = −19→20
43041 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.083	H-atom parameters constrained
wR(F^2) = 0.254	w = 1/[σ^2(Fo^2) + (0.1342P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.98	(Δ/σ)max < 0.001
10222 reflections	Δρmax = 2.45 e Å^−3
628 parameters	Δρmin = −1.13 e Å^−3
0 restraints

Special details

Experimental. Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a nylon loop using Paratone oil. Data were measured using omega scans of 0.5° per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 0.83Å to 100%. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick. The structures are solved by the direct method using the SHELXS-97 program and refined by least squares method on F2, SHELXL-97, incorporated in OLEX2.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. The structure was refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008) incorporated in Olex2 (Dolomanov et al., 2009). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ru1	0.51924 (8)	0.71860 (6)	0.59071 (6)	0.0388 (3)
Ru2	0.36729 (7)	0.63005 (6)	0.78939 (6)	0.0381 (3)
Ru3	0.27149 (8)	0.84710 (6)	0.70788 (6)	0.0397 (3)
O1	0.3867 (6)	0.7319 (4)	0.6981 (4)	0.0359 (16)
O2	0.6533 (6)	0.6838 (5)	0.6568 (5)	0.0436 (18)
O3	0.5549 (6)	0.5904 (5)	0.7749 (5)	0.0404 (17)
O4	0.5311 (6)	0.5779 (5)	0.5929 (4)	0.0403 (17)
O5	0.3690 (7)	0.5414 (5)	0.7056 (5)	0.0464 (18)
O6	0.3618 (6)	0.7050 (5)	0.8864 (5)	0.0445 (18)
O7	0.2563 (7)	0.8444 (5)	0.8404 (5)	0.0475 (18)
O8	0.1770 (7)	0.6529 (5)	0.8212 (5)	0.0469 (19)
O9	0.1206 (6)	0.7862 (5)	0.7384 (5)	0.0479 (19)
O10	0.4088 (7)	0.9242 (5)	0.6797 (5)	0.0459 (18)
O11	0.5471 (6)	0.8545 (5)	0.5679 (5)	0.0428 (17)
O12	0.2610 (7)	0.8671 (5)	0.5783 (5)	0.0480 (19)
O13	0.3970 (6)	0.7468 (5)	0.5165 (4)	0.0446 (18)
N1	0.6602 (8)	0.7064 (6)	0.4701 (5)	0.039 (2)
N2	0.3478 (8)	0.5096 (6)	0.8843 (6)	0.044 (2)
N3	0.1417 (8)	0.9715 (6)	0.7188 (6)	0.047 (2)
C1	0.7576 (10)	0.6368 (8)	0.4554 (7)	0.046 (3)
H1	0.7692	0.5919	0.5040	0.055*
C2	0.8406 (10)	0.6269 (8)	0.3752 (8)	0.052 (3)
H2	0.9075	0.5763	0.3695	0.063*
C3	0.8279 (8)	0.6912 (7)	0.3004 (7)	0.039 (3)
C4	0.7273 (10)	0.7623 (8)	0.3145 (7)	0.047 (3)
H4	0.7115	0.8059	0.2662	0.057*
C5	0.6482 (10)	0.7705 (8)	0.3999 (8)	0.052 (3)
H5	0.5841	0.8229	0.4085	0.063*
C6	0.9108 (10)	0.6812 (9)	0.2103 (8)	0.051 (3)
C7	0.9755 (11)	0.5935 (9)	0.1879 (8)	0.054 (3)
H7	0.9661	0.5404	0.2310	0.064*
C8	1.0519 (11)	0.5839 (10)	0.1046 (8)	0.059 (3)
H8	1.0934	0.5241	0.0906	0.071*
C9	1.0693 (12)	0.6592 (12)	0.0415 (9)	0.071 (4)
H9	1.1242	0.6517	−0.0153	0.085*
C10	1.0072 (12)	0.7460 (10)	0.0602 (8)	0.064 (4)
H10	1.0184	0.7982	0.0161	0.077*
C11	0.9272 (11)	0.7575 (9)	0.1447 (8)	0.060 (3)
H11	0.8840	0.8174	0.1573	0.072*
C12	0.4264 (10)	0.4731 (8)	0.9323 (7)	0.048 (3)
H12	0.4857	0.5078	0.9302	0.057*
C13	0.4269 (10)	0.3880 (8)	0.9850 (8)	0.049 (3)
H13	0.4836	0.3675	1.0189	0.059*
C14	0.3453 (10)	0.3322 (8)	0.9888 (7)	0.046 (3)
C15	0.2611 (10)	0.3705 (8)	0.9394 (8)	0.050 (3)
H15	0.2009	0.3368	0.9412	0.060*
C16	0.2646 (10)	0.4556 (8)	0.8889 (7)	0.049 (3)
H16	0.2073	0.4785	0.8557	0.059*
C17	0.3482 (10)	0.2380 (7)	1.0414 (8)	0.047 (3)
C18	0.3201 (14)	0.1675 (9)	1.0110 (11)	0.077 (4)
H18	0.2966	0.1802	0.9581	0.093*
C19	0.326 (2)	0.0794 (11)	1.0576 (15)	0.140 (9)
H19	0.3103	0.0306	1.0362	0.168*
C20	0.358 (2)	0.0632 (13)	1.1384 (17)	0.156 (11)
H20	0.3593	0.0035	1.1721	0.188*
C21	0.3846 (15)	0.1304 (10)	1.1676 (11)	0.096 (6)
H21	0.4068	0.1184	1.2209	0.115*
C22	0.3799 (12)	0.2172 (10)	1.1195 (9)	0.066 (4)
H22	0.3990	0.2647	1.1407	0.080*
C23	0.1461 (10)	1.0449 (7)	0.6510 (8)	0.050 (3)
H23	0.2158	1.0435	0.6007	0.060*
C24	0.0504 (10)	1.1209 (8)	0.6551 (8)	0.051 (3)
H24	0.0540	1.1687	0.6063	0.061*
C25	−0.0512 (10)	1.1280 (8)	0.7300 (8)	0.048 (3)
C26	−0.0488 (11)	1.0559 (9)	0.7972 (9)	0.059 (3)
H26	−0.1147	1.0589	0.8498	0.070*
C27	0.0428 (10)	0.9804 (8)	0.7926 (8)	0.049 (3)
H27	0.0383	0.9327	0.8415	0.059*
C28	−0.1536 (11)	1.2082 (8)	0.7346 (8)	0.054 (3)
C29	−0.1417 (13)	1.2919 (9)	0.6853 (10)	0.067 (4)
H29	−0.0637	1.2982	0.6451	0.080*
C30	−0.2349 (15)	1.3686 (11)	0.6892 (13)	0.095 (5)
H30	−0.2211	1.4262	0.6544	0.114*
C31	−0.3525 (17)	1.3575 (12)	0.7476 (12)	0.091 (5)
H31	−0.4190	1.4085	0.7517	0.109*
C32	−0.3713 (13)	1.2727 (13)	0.7990 (10)	0.090 (5)
H32	−0.4496	1.2662	0.8386	0.108*
C33	−0.2733 (13)	1.1969 (10)	0.7917 (9)	0.071 (4)
H33	−0.2863	1.1382	0.8245	0.085*
C34	0.6488 (10)	0.6221 (8)	0.7255 (8)	0.044 (3)
C35	0.7681 (11)	0.5877 (9)	0.7504 (9)	0.066 (4)
H35A	0.8315	0.5601	0.7016	0.099*
H35B	0.7554	0.5411	0.8029	0.099*
H35C	0.7944	0.6396	0.7627	0.099*
C36	0.4566 (11)	0.5238 (7)	0.6371 (7)	0.044 (3)
C37	0.4713 (11)	0.4344 (7)	0.6075 (7)	0.051 (3)
H37A	0.4393	0.4440	0.5567	0.076*
H37B	0.4261	0.3933	0.6555	0.076*
H37C	0.5585	0.4062	0.5907	0.076*
C38	0.3054 (9)	0.7872 (8)	0.8945 (7)	0.044 (3)
C39	0.2988 (12)	0.8201 (8)	0.9784 (8)	0.058 (3)
H39A	0.2911	0.7685	1.0267	0.087*
H39B	0.2274	0.8697	0.9925	0.087*
H39C	0.3737	0.8434	0.9705	0.087*
C40	0.1004 (10)	0.7131 (9)	0.7899 (8)	0.048 (3)
C41	−0.0304 (11)	0.6948 (10)	0.8191 (11)	0.080 (4)
H41A	−0.0872	0.7482	0.8441	0.119*
H41B	−0.0365	0.6399	0.8636	0.119*
H41C	−0.0514	0.6846	0.7682	0.119*
C42	0.5070 (10)	0.9162 (7)	0.6177 (7)	0.040 (2)
C43	0.5857 (11)	0.9889 (8)	0.6024 (8)	0.052 (3)
H43A	0.5834	1.0295	0.5471	0.079*
H43B	0.6705	0.9583	0.5992	0.079*
H43C	0.5539	1.0256	0.6512	0.079*
C44	0.3064 (10)	0.8120 (8)	0.5209 (8)	0.048 (3)
C45	0.2407 (11)	0.8278 (8)	0.4492 (8)	0.057 (3)
H45A	0.1592	0.8113	0.4754	0.085*
H45B	0.2887	0.7891	0.4033	0.085*
H45C	0.2321	0.8930	0.4232	0.085*
O17	−0.0382 (6)	0.9449 (5)	0.5641 (4)	0.167 (16)	0.5
O16	0.0212 (6)	0.5798 (5)	0.5311 (4)	0.140 (5)
H16A	−0.0047	0.5446	0.5803	0.210*
H16B	0.0744	0.5463	0.4929	0.210*
O14	0.8753 (6)	0.7597 (5)	0.5557 (4)	0.113 (4)
H14A	0.8362	0.8019	0.5895	0.170*
H14B	0.9479	0.7448	0.5635	0.170*
O15	0.2106 (6)	0.6072 (5)	0.5875 (4)	0.149 (14)	0.5
H15A	0.1795	0.6150	0.5438	0.224*	0.5
H15B	0.2665	0.6416	0.5692	0.224*	0.5
O18	0.3175 (6)	1.0352 (5)	0.8261 (4)	0.208 (8)
H18A	0.3164	0.9917	0.8708	0.311*
H18B	0.2575	1.0790	0.8463	0.311*
O17A	−0.0478 (6)	0.8844 (5)	0.6228 (4)	0.127 (11)	0.5
H17C	−0.0125	0.8269	0.6196	0.190*	0.5
H17D	−0.0848	0.8861	0.6786	0.190*	0.5
O15A	0.1481 (6)	0.6046 (5)	0.6360 (4)	0.24 (3)	0.5
H17A	−0.0131	0.9888	0.5773	0.366*	0.5
H17B	0.0242	0.8995	0.5584	0.366*	0.5
H15C	0.1291	0.5539	0.6693	0.366*	0.5
H15D	0.1410	0.6459	0.6688	0.366*	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.0379 (5)	0.0391 (5)	0.0462 (5)	−0.0119 (4)	−0.0126 (4)	−0.0141 (4)
Ru2	0.0362 (5)	0.0385 (5)	0.0465 (5)	−0.0113 (4)	−0.0144 (4)	−0.0122 (4)
Ru3	0.0366 (5)	0.0392 (5)	0.0486 (6)	−0.0084 (4)	−0.0144 (4)	−0.0131 (4)
O1	0.037 (4)	0.042 (4)	0.037 (4)	−0.013 (3)	−0.012 (3)	−0.015 (3)
O2	0.038 (4)	0.047 (4)	0.054 (5)	−0.015 (3)	−0.015 (4)	−0.014 (4)
O3	0.041 (4)	0.041 (4)	0.047 (4)	−0.013 (3)	−0.016 (3)	−0.011 (3)
O4	0.043 (4)	0.039 (4)	0.048 (4)	−0.012 (3)	−0.018 (3)	−0.014 (3)
O5	0.051 (5)	0.049 (5)	0.046 (5)	−0.017 (4)	−0.011 (4)	−0.016 (4)
O6	0.045 (4)	0.049 (5)	0.047 (4)	−0.012 (4)	−0.017 (4)	−0.014 (4)
O7	0.048 (4)	0.041 (4)	0.056 (5)	−0.005 (4)	−0.018 (4)	−0.010 (4)
O8	0.041 (4)	0.049 (5)	0.058 (5)	−0.017 (4)	−0.014 (4)	−0.013 (4)
O9	0.044 (4)	0.042 (4)	0.068 (5)	−0.015 (4)	−0.023 (4)	−0.010 (4)
O10	0.045 (4)	0.040 (4)	0.060 (5)	−0.015 (3)	−0.012 (4)	−0.017 (4)
O11	0.040 (4)	0.044 (4)	0.049 (4)	−0.013 (3)	−0.010 (3)	−0.012 (4)
O12	0.047 (4)	0.042 (4)	0.064 (5)	−0.002 (4)	−0.024 (4)	−0.018 (4)
O13	0.043 (4)	0.056 (5)	0.045 (4)	−0.014 (4)	−0.014 (3)	−0.020 (4)
N1	0.051 (6)	0.035 (5)	0.039 (5)	−0.016 (4)	−0.012 (4)	−0.014 (4)
N2	0.036 (5)	0.054 (6)	0.046 (5)	−0.009 (4)	−0.013 (4)	−0.011 (4)
N3	0.043 (5)	0.042 (5)	0.062 (6)	−0.006 (4)	−0.016 (5)	−0.016 (5)
C1	0.037 (6)	0.060 (8)	0.045 (7)	−0.006 (6)	−0.015 (5)	−0.015 (6)
C2	0.039 (6)	0.059 (8)	0.067 (8)	−0.015 (6)	−0.020 (6)	−0.012 (6)
C3	0.021 (5)	0.047 (6)	0.057 (7)	−0.014 (5)	−0.013 (5)	−0.010 (5)
C4	0.046 (7)	0.060 (7)	0.045 (7)	−0.031 (6)	−0.010 (5)	−0.007 (6)
C5	0.048 (7)	0.055 (8)	0.056 (8)	−0.006 (6)	−0.005 (6)	−0.030 (6)
C6	0.035 (6)	0.075 (9)	0.056 (8)	−0.023 (6)	−0.016 (5)	−0.019 (7)
C7	0.056 (7)	0.060 (8)	0.055 (8)	−0.022 (6)	−0.020 (6)	−0.012 (6)
C8	0.051 (7)	0.076 (9)	0.050 (8)	−0.018 (7)	−0.006 (6)	−0.016 (7)
C9	0.051 (8)	0.109 (12)	0.063 (9)	−0.029 (8)	−0.012 (7)	−0.026 (9)
C10	0.064 (8)	0.082 (10)	0.048 (8)	−0.030 (8)	−0.006 (7)	−0.007 (7)
C11	0.058 (8)	0.071 (9)	0.063 (9)	−0.032 (7)	−0.014 (7)	−0.019 (7)
C12	0.049 (7)	0.054 (7)	0.049 (7)	−0.025 (6)	−0.014 (6)	−0.007 (6)
C13	0.055 (7)	0.046 (7)	0.058 (7)	−0.017 (6)	−0.027 (6)	−0.010 (6)
C14	0.040 (6)	0.060 (7)	0.046 (7)	−0.018 (5)	−0.011 (5)	−0.015 (6)
C15	0.045 (7)	0.053 (7)	0.059 (8)	−0.020 (6)	−0.019 (6)	−0.006 (6)
C16	0.049 (7)	0.055 (7)	0.053 (7)	−0.023 (6)	−0.021 (6)	−0.002 (6)
C17	0.046 (7)	0.043 (7)	0.058 (8)	−0.025 (5)	−0.016 (6)	−0.001 (6)
C18	0.096 (11)	0.053 (8)	0.110 (12)	−0.030 (8)	−0.061 (10)	−0.001 (8)
C19	0.22 (2)	0.059 (11)	0.20 (2)	−0.075 (13)	−0.13 (2)	0.033 (12)
C20	0.24 (3)	0.082 (14)	0.21 (2)	−0.079 (16)	−0.16 (2)	0.061 (15)
C21	0.126 (14)	0.070 (10)	0.119 (14)	−0.058 (10)	−0.080 (12)	0.044 (10)
C22	0.067 (9)	0.080 (10)	0.063 (9)	−0.038 (7)	−0.024 (7)	0.003 (7)
C23	0.048 (7)	0.038 (6)	0.080 (9)	0.000 (5)	−0.040 (6)	−0.020 (6)
C24	0.051 (7)	0.049 (7)	0.057 (8)	−0.015 (6)	−0.020 (6)	−0.005 (6)
C25	0.045 (7)	0.042 (7)	0.068 (8)	−0.004 (5)	−0.026 (6)	−0.023 (6)
C26	0.050 (7)	0.066 (9)	0.072 (9)	−0.009 (7)	−0.024 (6)	−0.028 (7)
C27	0.047 (7)	0.042 (7)	0.063 (8)	−0.001 (6)	−0.030 (6)	0.000 (6)
C28	0.061 (8)	0.044 (7)	0.065 (8)	0.014 (6)	−0.035 (7)	−0.025 (6)
C29	0.076 (9)	0.048 (8)	0.093 (10)	−0.003 (7)	−0.048 (8)	−0.021 (7)
C30	0.077 (11)	0.064 (10)	0.151 (16)	0.022 (9)	−0.048 (12)	−0.047 (10)
C31	0.106 (14)	0.090 (12)	0.090 (12)	0.033 (10)	−0.067 (11)	−0.039 (10)
C32	0.057 (9)	0.143 (16)	0.057 (9)	0.032 (10)	−0.024 (7)	−0.032 (10)
C33	0.076 (10)	0.072 (9)	0.065 (9)	0.015 (8)	−0.029 (8)	−0.031 (7)
C34	0.037 (6)	0.051 (7)	0.052 (7)	−0.008 (5)	−0.014 (5)	−0.021 (6)
C35	0.055 (8)	0.074 (9)	0.083 (10)	−0.014 (7)	−0.040 (7)	−0.004 (7)
C36	0.060 (7)	0.031 (6)	0.049 (7)	−0.014 (5)	−0.019 (6)	−0.015 (5)
C37	0.062 (7)	0.044 (7)	0.049 (7)	−0.009 (6)	−0.017 (6)	−0.013 (5)
C38	0.034 (6)	0.046 (7)	0.055 (7)	−0.014 (5)	−0.009 (5)	−0.011 (6)
C39	0.068 (8)	0.058 (8)	0.059 (8)	−0.016 (6)	−0.019 (6)	−0.027 (6)
C40	0.038 (6)	0.049 (7)	0.062 (8)	−0.002 (6)	−0.017 (6)	−0.020 (6)
C41	0.044 (7)	0.073 (9)	0.125 (13)	−0.029 (7)	−0.022 (8)	−0.005 (9)
C42	0.038 (6)	0.039 (6)	0.049 (7)	−0.010 (5)	−0.018 (5)	−0.009 (5)
C43	0.057 (7)	0.048 (7)	0.068 (8)	−0.019 (6)	−0.028 (6)	−0.017 (6)
C44	0.043 (7)	0.041 (7)	0.065 (8)	−0.011 (6)	−0.015 (6)	−0.015 (6)
C45	0.063 (8)	0.063 (8)	0.059 (8)	−0.011 (6)	−0.033 (6)	−0.017 (6)
O17	0.073 (18)	0.18 (3)	0.28 (4)	0.016 (18)	−0.05 (2)	−0.15 (3)
O16	0.139 (11)	0.148 (12)	0.157 (13)	−0.033 (9)	−0.084 (10)	0.002 (10)
O14	0.072 (7)	0.152 (11)	0.110 (9)	−0.044 (7)	−0.018 (6)	0.009 (8)
O15	0.21 (3)	0.09 (2)	0.22 (3)	−0.06 (2)	−0.17 (3)	0.012 (19)
O18	0.29 (2)	0.112 (12)	0.24 (2)	−0.010 (14)	−0.116 (18)	−0.040 (12)
O17A	0.101 (19)	0.14 (3)	0.17 (3)	−0.021 (17)	−0.064 (19)	−0.06 (2)
O15A	0.39 (7)	0.10 (3)	0.22 (4)	−0.05 (3)	−0.02 (4)	−0.08 (3)

Geometric parameters (Å, º)

Ru1—O1	1.934 (6)	C18—H18	0.9500
Ru1—O2	2.082 (7)	C18—C19	1.38 (2)
Ru1—O4	2.080 (7)	C19—H19	0.9500
Ru1—O11	2.084 (7)	C19—C20	1.43 (3)
Ru1—O13	2.066 (7)	C20—H20	0.9500
Ru1—N1	2.124 (8)	C20—C21	1.34 (2)
Ru2—O1	1.899 (6)	C21—H21	0.9500
Ru2—O3	2.083 (7)	C21—C22	1.375 (17)
Ru2—O5	2.078 (7)	C22—H22	0.9500
Ru2—O6	2.087 (7)	C23—H23	0.9500
Ru2—O8	2.079 (7)	C23—C24	1.394 (15)
Ru2—N2	2.128 (9)	C24—H24	0.9500
Ru3—O1	1.928 (6)	C24—C25	1.403 (16)
Ru3—O7	2.088 (8)	C25—C26	1.371 (16)
Ru3—O9	2.055 (7)	C25—C28	1.481 (15)
Ru3—O10	2.080 (7)	C26—H26	0.9500
Ru3—O12	2.096 (8)	C26—C27	1.361 (16)
Ru3—N3	2.111 (9)	C27—H27	0.9500
O2—C34	1.289 (13)	C28—C29	1.357 (17)
O3—C34	1.267 (12)	C28—C33	1.439 (18)
O4—C36	1.279 (12)	C29—H29	0.9500
O5—C36	1.272 (13)	C29—C30	1.385 (18)
O6—C38	1.268 (12)	C30—H30	0.9500
O7—C38	1.271 (12)	C30—C31	1.42 (2)
O8—C40	1.265 (13)	C31—H31	0.9500
O9—C40	1.258 (13)	C31—C32	1.40 (2)
O10—C42	1.261 (12)	C32—H32	0.9500
O11—C42	1.262 (12)	C32—C33	1.407 (18)
O12—C44	1.273 (13)	C33—H33	0.9500
O13—C44	1.257 (13)	C34—C35	1.521 (15)
N1—C1	1.348 (13)	C35—H35A	0.9800
N1—C5	1.353 (14)	C35—H35B	0.9800
N2—C12	1.340 (13)	C35—H35C	0.9800
N2—C16	1.384 (13)	C36—C37	1.472 (14)
N3—C23	1.387 (14)	C37—H37A	0.9800
N3—C27	1.377 (14)	C37—H37B	0.9800
C1—H1	0.9500	C37—H37C	0.9800
C1—C2	1.363 (15)	C38—C39	1.511 (15)
C2—H2	0.9500	C39—H39A	0.9800
C2—C3	1.411 (15)	C39—H39B	0.9800
C3—C4	1.384 (15)	C39—H39C	0.9800
C3—C6	1.487 (15)	C40—C41	1.525 (15)
C4—H4	0.9500	C41—H41A	0.9800
C4—C5	1.407 (15)	C41—H41B	0.9800
C5—H5	0.9500	C41—H41C	0.9800
C6—C7	1.411 (16)	C42—C43	1.524 (14)
C6—C11	1.398 (16)	C43—H43A	0.9800
C7—H7	0.9500	C43—H43B	0.9800
C7—C8	1.373 (16)	C43—H43C	0.9800
C8—H8	0.9500	C44—C45	1.539 (15)
C8—C9	1.367 (18)	C45—H45A	0.9800
C9—H9	0.9500	C45—H45B	0.9800
C9—C10	1.376 (19)	C45—H45C	0.9800
C10—H10	0.9500	O17—H17A	0.8699
C10—C11	1.407 (17)	O17—H17B	0.8700
C11—H11	0.9500	O16—H16A	0.8695
C12—H12	0.9500	O16—H16B	0.8700
C12—C13	1.385 (15)	O14—H14A	0.8699
C13—H13	0.9500	O14—H14B	0.8693
C13—C14	1.391 (14)	O15—H15A	0.8700
C14—C15	1.410 (15)	O15—H15B	0.8700
C14—C17	1.496 (15)	O18—H18A	0.8698
C15—H15	0.9500	O18—H18B	0.8698
C15—C16	1.373 (15)	O17A—H17C	0.8701
C16—H16	0.9500	O17A—H17D	0.8700
C17—C18	1.396 (16)	O15A—H15C	0.8700
C17—C22	1.385 (16)	O15A—H15D	0.8698
O1—Ru1—O2	93.1 (3)	C15—C16—N2	122.9 (10)
O1—Ru1—O4	96.9 (3)	C15—C16—H16	118.6
O1—Ru1—O11	95.7 (3)	C18—C17—C14	119.8 (11)
O1—Ru1—O13	91.5 (3)	C22—C17—C14	122.0 (10)
O1—Ru1—N1	177.9 (3)	C22—C17—C18	118.2 (11)
O2—Ru1—O11	87.7 (3)	C17—C18—H18	119.9
O2—Ru1—N1	89.0 (3)	C19—C18—C17	120.3 (14)
O4—Ru1—O2	87.9 (3)	C19—C18—H18	119.9
O4—Ru1—O11	166.8 (3)	C18—C19—H19	120.7
O4—Ru1—N1	83.6 (3)	C18—C19—C20	118.6 (16)
O11—Ru1—N1	83.9 (3)	C20—C19—H19	120.7
O13—Ru1—O2	175.0 (3)	C19—C20—H20	119.4
O13—Ru1—O4	89.4 (3)	C21—C20—C19	121.2 (16)
O13—Ru1—O11	94.0 (3)	C21—C20—H20	119.4
O13—Ru1—N1	86.5 (3)	C20—C21—H21	120.4
O1—Ru2—O3	93.6 (3)	C20—C21—C22	119.2 (16)
O1—Ru2—O5	93.3 (3)	C22—C21—H21	120.4
O1—Ru2—O6	94.0 (3)	C17—C22—H22	118.8
O1—Ru2—O8	95.6 (3)	C21—C22—C17	122.5 (13)
O1—Ru2—N2	175.7 (3)	C21—C22—H22	118.8
O3—Ru2—O6	86.5 (3)	N3—C23—H23	119.3
O3—Ru2—N2	86.1 (3)	N3—C23—C24	121.3 (11)
O5—Ru2—O3	93.4 (3)	C24—C23—H23	119.3
O5—Ru2—O6	172.7 (3)	C23—C24—H24	119.5
O5—Ru2—O8	86.9 (3)	C23—C24—C25	121.1 (11)
O5—Ru2—N2	82.5 (3)	C25—C24—H24	119.5
O6—Ru2—N2	90.2 (3)	C24—C25—C28	121.4 (11)
O8—Ru2—O3	170.7 (3)	C26—C25—C24	115.5 (11)
O8—Ru2—O6	92.1 (3)	C26—C25—C28	123.1 (12)
O8—Ru2—N2	84.8 (3)	C25—C26—H26	118.2
O1—Ru3—O7	93.9 (3)	C27—C26—C25	123.7 (12)
O1—Ru3—O9	94.1 (3)	C27—C26—H26	118.2
O1—Ru3—O10	93.0 (3)	N3—C27—H27	119.2
O1—Ru3—O12	95.3 (3)	C26—C27—N3	121.5 (11)
O1—Ru3—N3	178.5 (3)	C26—C27—H27	119.2
O7—Ru3—O12	170.5 (3)	C29—C28—C25	123.4 (12)
O7—Ru3—N3	86.4 (3)	C29—C28—C33	117.7 (12)
O9—Ru3—O7	92.3 (3)	C33—C28—C25	118.9 (11)
O9—Ru3—O10	172.8 (3)	C28—C29—H29	117.6
O9—Ru3—O12	84.8 (3)	C28—C29—C30	124.8 (16)
O9—Ru3—N3	84.4 (3)	C30—C29—H29	117.6
O10—Ru3—O7	86.6 (3)	C29—C30—H30	121.4
O10—Ru3—O12	95.1 (3)	C29—C30—C31	117.2 (17)
O10—Ru3—N3	88.4 (3)	C31—C30—H30	121.4
O12—Ru3—N3	84.3 (3)	C30—C31—H31	119.6
Ru2—O1—Ru1	119.8 (3)	C32—C31—C30	120.8 (14)
Ru2—O1—Ru3	121.1 (3)	C32—C31—H31	119.6
Ru3—O1—Ru1	119.0 (3)	C31—C32—H32	120.2
C34—O2—Ru1	123.3 (6)	C31—C32—C33	119.5 (15)
C34—O3—Ru2	134.2 (7)	C33—C32—H32	120.2
C36—O4—Ru1	130.9 (7)	C28—C33—H33	120.0
C36—O5—Ru2	124.0 (6)	C32—C33—C28	119.9 (14)
C38—O6—Ru2	125.6 (7)	C32—C33—H33	120.0
C38—O7—Ru3	132.7 (7)	O2—C34—C35	115.7 (10)
C40—O8—Ru2	132.3 (7)	O3—C34—O2	126.5 (10)
C40—O9—Ru3	127.4 (7)	O3—C34—C35	117.8 (11)
C42—O10—Ru3	125.7 (7)	C34—C35—H35A	109.5
C42—O11—Ru1	130.2 (7)	C34—C35—H35B	109.5
C44—O12—Ru3	128.8 (7)	C34—C35—H35C	109.5
C44—O13—Ru1	126.6 (7)	H35A—C35—H35B	109.5
C1—N1—Ru1	125.7 (7)	H35A—C35—H35C	109.5
C1—N1—C5	116.3 (9)	H35B—C35—H35C	109.5
C5—N1—Ru1	117.8 (7)	O4—C36—C37	118.6 (10)
C12—N2—Ru2	122.9 (7)	O5—C36—O4	124.7 (9)
C12—N2—C16	115.5 (9)	O5—C36—C37	116.7 (10)
C16—N2—Ru2	120.7 (7)	C36—C37—H37A	109.5
C23—N3—Ru3	122.6 (8)	C36—C37—H37B	109.5
C27—N3—Ru3	120.5 (7)	C36—C37—H37C	109.5
C27—N3—C23	116.8 (9)	H37A—C37—H37B	109.5
N1—C1—H1	117.9	H37A—C37—H37C	109.5
N1—C1—C2	124.2 (11)	H37B—C37—H37C	109.5
C2—C1—H1	117.9	O6—C38—O7	127.9 (10)
C1—C2—H2	119.7	O6—C38—C39	114.9 (10)
C1—C2—C3	120.5 (11)	O7—C38—C39	117.2 (10)
C3—C2—H2	119.7	C38—C39—H39A	109.5
C2—C3—C6	123.2 (10)	C38—C39—H39B	109.5
C4—C3—C2	115.8 (10)	C38—C39—H39C	109.5
C4—C3—C6	120.9 (10)	H39A—C39—H39B	109.5
C3—C4—H4	119.7	H39A—C39—H39C	109.5
C3—C4—C5	120.6 (11)	H39B—C39—H39C	109.5
C5—C4—H4	119.7	O8—C40—C41	115.9 (11)
N1—C5—C4	122.4 (11)	O9—C40—O8	127.0 (10)
N1—C5—H5	118.8	O9—C40—C41	117.1 (10)
C4—C5—H5	118.8	C40—C41—H41A	109.5
C7—C6—C3	120.7 (11)	C40—C41—H41B	109.5
C11—C6—C3	121.7 (11)	C40—C41—H41C	109.5
C11—C6—C7	117.6 (11)	H41A—C41—H41B	109.5
C6—C7—H7	119.6	H41A—C41—H41C	109.5
C8—C7—C6	120.9 (12)	H41B—C41—H41C	109.5
C8—C7—H7	119.6	O10—C42—O11	127.0 (9)
C7—C8—H8	119.5	O10—C42—C43	116.1 (10)
C9—C8—C7	121.0 (13)	O11—C42—C43	116.9 (10)
C9—C8—H8	119.5	C42—C43—H43A	109.5
C8—C9—H9	119.9	C42—C43—H43B	109.5
C8—C9—C10	120.1 (13)	C42—C43—H43C	109.5
C10—C9—H9	119.9	H43A—C43—H43B	109.5
C9—C10—H10	120.0	H43A—C43—H43C	109.5
C9—C10—C11	120.0 (13)	H43B—C43—H43C	109.5
C11—C10—H10	120.0	O12—C44—C45	115.2 (10)
C6—C11—C10	120.4 (13)	O13—C44—O12	127.9 (11)
C6—C11—H11	119.8	O13—C44—C45	116.9 (10)
C10—C11—H11	119.8	C44—C45—H45A	109.5
N2—C12—H12	117.9	C44—C45—H45B	109.5
N2—C12—C13	124.3 (10)	C44—C45—H45C	109.5
C13—C12—H12	117.9	H45A—C45—H45B	109.5
C12—C13—H13	119.6	H45A—C45—H45C	109.5
C12—C13—C14	120.8 (10)	H45B—C45—H45C	109.5
C14—C13—H13	119.6	H17A—O17—H17B	104.5
C13—C14—C15	115.4 (10)	H16A—O16—H16B	109.6
C13—C14—C17	121.9 (10)	H14A—O14—H14B	104.5
C15—C14—C17	122.7 (10)	H15A—O15—H15B	104.5
C14—C15—H15	119.4	H18A—O18—H18B	104.5
C16—C15—C14	121.1 (10)	H17C—O17A—H17D	104.5
C16—C15—H15	119.4	H15C—O15A—H15D	109.5
N2—C16—H16	118.6

Hexa-µ₂-acetato-µ₃-oxido-tris(1H-imidazole)triruthenium hexafluorophosphate acetonitrile hemisolvate (ae418a)

Crystal data

[Ru3(C2H3O2)6O(C3H4N2)3]PF6·0.5C2H3N	Mo Kα radiation, λ = 0.71073 Å
Mr = 1043.23	Cell parameters from 9943 reflections
Cubic, Pa3	θ = 2.4–25.3°
a = 19.2946 (13) Å	µ = 1.39 mm^−1
V = 7183.0 (15) Å^3	T = 173 K
Z = 8.0	Plate, black
F(000) = 4112	0.34 × 0.20 × 0.03 mm
Dx = 1.929 Mg m^−3

Data collection

Bruker APEXII CCD diffractometer	2203 independent reflections
Radiation source: sealed tube	1841 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.093
Detector resolution: 8.36 pixels mm^-1	θmax = 25.4°, θmin = 1.8°
ω scans	h = −23→23
Absorption correction: multi-scan (TWINABS; Bruker, 2012)	k = −23→23
Tmin = 0.655, Tmax = 0.745	l = −23→23
110680 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.043	H-atom parameters constrained
wR(F^2) = 0.111	w = 1/[σ^2(Fo^2) + (0.0602P)^2 + 16.5814P] where P = (Fo^2 + 2Fc^2)/3
S = 1.13	(Δ/σ)max = 0.001
2203 reflections	Δρmax = 1.70 e Å^−3
180 parameters	Δρmin = −0.44 e Å^−3
0 restraints

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ru1	0.67622 (2)	0.46270 (2)	0.91302 (2)	0.02005 (17)
P1B	0.7438 (3)	0.7438 (3)	0.7438 (3)	0.045 (2)	0.5
O1	0.60126 (15)	0.39874 (15)	0.89874 (15)	0.0181 (10)
O2	0.74925 (16)	0.38654 (16)	0.91384 (15)	0.0251 (7)
O3	0.69122 (16)	0.30476 (16)	0.97439 (16)	0.0272 (7)
O5	0.53899 (15)	0.51922 (15)	0.82687 (15)	0.0217 (7)
O4	0.61256 (16)	0.54609 (15)	0.91362 (16)	0.0248 (7)
N1	0.75597 (19)	0.53466 (18)	0.9283 (2)	0.0236 (8)
N2	0.8190 (2)	0.6284 (2)	0.9196 (2)	0.0340 (10)
H2	0.8355	0.6678	0.9036	0.041*
C6	0.5676 (2)	0.5613 (2)	0.8690 (2)	0.0226 (9)
C1	0.7675 (2)	0.5911 (2)	0.8914 (3)	0.0301 (11)
H1	0.7428	0.6035	0.8506	0.036*
C7	0.5477 (2)	0.6360 (2)	0.8643 (2)	0.0284 (10)
H7A	0.5783	0.6596	0.8314	0.043*
H7B	0.5521	0.6576	0.9100	0.043*
H7C	0.4996	0.6397	0.8484	0.043*
C4	0.7451 (2)	0.3294 (2)	0.9466 (2)	0.0274 (10)
C3	0.8015 (3)	0.5366 (3)	0.9830 (3)	0.0315 (11)
H3	0.8045	0.5031	1.0189	0.038*
C2	0.8412 (3)	0.5942 (3)	0.9774 (3)	0.0376 (12)
H2A	0.8775	0.6080	1.0077	0.045*
C5	0.8106 (3)	0.2887 (3)	0.9543 (3)	0.0455 (14)
H5A	0.8056	0.2439	0.9309	0.068*
H5B	0.8201	0.2810	1.0036	0.068*
H5C	0.8491	0.3144	0.9335	0.068*
F4	0.7663 (6)	0.7289 (6)	0.8223 (5)	0.081 (3)	0.5
F3	0.7551 (16)	0.7937 (11)	0.7022 (11)	0.081 (3)	0.25
F1	0.6850 (6)	0.6653 (10)	0.7526 (8)	0.135 (6)	0.5
N3	0.9500 (14)	0.4500 (14)	1.0500 (14)	0.105 (12)	0.5
C9	0.9132 (16)	0.4132 (16)	1.0868 (16)	0.095 (12)	0.5
C8	0.8774 (15)	0.3774 (15)	1.1226 (15)	0.138 (16)	0.5
H8A	0.8960	0.3765	1.1700	0.208*	0.1667
H8B	0.8767	0.3300	1.1042	0.208*	0.1667
H8C	0.8302	0.3958	1.1235	0.208*	0.1667
P1	0.7265 (6)	0.7265 (6)	0.7265 (6)	0.099 (6)	0.5
F5	0.7899 (15)	0.7113 (13)	0.7942 (13)	0.081 (3)	0.25
F2	0.7277 (7)	0.7606 (8)	0.6657 (6)	0.104 (4)	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.0192 (2)	0.0191 (2)	0.0218 (2)	−0.00133 (13)	−0.00203 (13)	0.00176 (13)
P1B	0.045 (2)	0.045 (2)	0.045 (2)	0.013 (2)	0.013 (2)	0.013 (2)
O1	0.0181 (10)	0.0181 (10)	0.0181 (10)	−0.0019 (12)	−0.0019 (12)	0.0019 (12)
O2	0.0231 (16)	0.0240 (16)	0.0283 (17)	0.0016 (13)	−0.0001 (13)	0.0045 (13)
O3	0.0232 (16)	0.0270 (17)	0.0313 (17)	−0.0017 (13)	−0.0048 (14)	0.0061 (14)
O5	0.0242 (16)	0.0201 (15)	0.0209 (15)	0.0000 (12)	−0.0042 (12)	0.0031 (12)
O4	0.0252 (17)	0.0225 (16)	0.0268 (17)	0.0020 (13)	−0.0040 (13)	0.0003 (13)
N1	0.0193 (19)	0.0231 (19)	0.028 (2)	−0.0042 (15)	0.0026 (16)	−0.0019 (16)
N2	0.032 (2)	0.019 (2)	0.050 (3)	−0.0082 (17)	0.0065 (19)	−0.0032 (18)
C6	0.020 (2)	0.029 (2)	0.019 (2)	0.0021 (18)	0.0025 (18)	0.0083 (18)
C1	0.027 (2)	0.024 (2)	0.039 (3)	−0.0027 (19)	0.001 (2)	0.003 (2)
C7	0.028 (2)	0.030 (2)	0.028 (2)	0.002 (2)	−0.002 (2)	0.006 (2)
C4	0.030 (3)	0.023 (2)	0.029 (2)	0.002 (2)	0.000 (2)	0.0011 (19)
C3	0.030 (3)	0.039 (3)	0.026 (2)	−0.007 (2)	0.000 (2)	−0.002 (2)
C2	0.036 (3)	0.044 (3)	0.033 (3)	−0.013 (2)	−0.002 (2)	−0.005 (2)
C5	0.028 (3)	0.043 (3)	0.066 (4)	0.008 (2)	−0.007 (3)	0.020 (3)
F4	0.105 (8)	0.078 (6)	0.061 (6)	0.003 (5)	−0.005 (5)	0.018 (5)
F3	0.105 (8)	0.078 (6)	0.061 (6)	0.003 (5)	−0.005 (5)	0.018 (5)
F1	0.066 (7)	0.201 (16)	0.139 (10)	−0.014 (8)	0.009 (6)	0.125 (11)
N3	0.105 (12)	0.105 (12)	0.105 (12)	0.063 (15)	−0.063 (15)	−0.063 (15)
C9	0.095 (12)	0.095 (12)	0.095 (12)	0.022 (14)	−0.022 (14)	−0.022 (14)
C8	0.138 (16)	0.138 (16)	0.138 (16)	0.01 (2)	−0.01 (2)	−0.01 (2)
P1	0.099 (6)	0.099 (6)	0.099 (6)	0.059 (7)	0.059 (7)	0.059 (7)
F5	0.105 (8)	0.078 (6)	0.061 (6)	0.003 (5)	−0.005 (5)	0.018 (5)
F2	0.093 (8)	0.162 (13)	0.056 (6)	−0.009 (8)	−0.023 (6)	0.044 (7)

Geometric parameters (Å, º)

Ru1—O1	1.9211 (4)	C7—H7C	0.9800
Ru1—O2	2.036 (3)	C4—C5	1.495 (7)
Ru1—O3^i	2.057 (3)	C3—H3	0.9500
Ru1—O5^ii	2.050 (3)	C3—C2	1.354 (7)
Ru1—O4	2.024 (3)	C2—H2A	0.9500
Ru1—N1	2.093 (4)	C5—H5A	0.9800
P1B—F5^iii	1.46 (2)	C5—H5B	0.9800
P1B—F5^iv	1.46 (2)	C5—H5C	0.9800
P1B—F5	1.46 (2)	F4—F3^iii	1.49 (3)
P1B—F2^iii	1.571 (11)	F4—F3^iv	1.44 (2)
P1B—F2	1.571 (11)	F4—P1	2.002 (18)
P1B—F2^iv	1.571 (11)	F3—F4^iii	1.44 (2)
O1—Ru1^i	1.9212 (4)	F3—F4^iv	1.49 (3)
O1—Ru1^ii	1.9212 (4)	F3—P1	1.48 (2)
O2—C4	1.273 (5)	F1—P1	1.513 (16)
O3—Ru1^ii	2.057 (3)	N3—C9	1.23 (5)
O3—C4	1.263 (6)	C9—C8	1.20 (5)
O5—Ru1^i	2.050 (3)	C8—H8A	0.9838
O5—C6	1.274 (5)	C8—H8B	0.9822
O4—C6	1.257 (5)	C8—H8C	0.9787
N1—C1	1.320 (6)	P1—F4^iii	2.002 (18)
N1—C3	1.373 (6)	P1—F4^iv	2.002 (18)
N2—H2	0.8800	P1—F3^iv	1.48 (2)
N2—C1	1.342 (6)	P1—F3^iii	1.48 (2)
N2—C2	1.365 (7)	P1—F1^iv	1.513 (16)
C6—C7	1.494 (6)	P1—F1^iii	1.513 (16)
C1—H1	0.9500	F5—F2^iii	1.66 (3)
C7—H7A	0.9800	F2—F5^iv	1.66 (3)
C7—H7B	0.9800
O1—Ru1—O2	93.35 (15)	N2—C2—H2A	126.8
O1—Ru1—O3^i	93.70 (13)	C3—C2—N2	106.4 (4)
O1—Ru1—O5^ii	96.39 (12)	C3—C2—H2A	126.8
O1—Ru1—O4	93.13 (15)	C4—C5—H5A	109.5
O1—Ru1—N1	178.42 (14)	C4—C5—H5B	109.5
O2—Ru1—O3^i	87.89 (12)	C4—C5—H5C	109.5
O2—Ru1—O5^ii	90.05 (12)	H5A—C5—H5B	109.5
O2—Ru1—N1	88.22 (14)	H5A—C5—H5C	109.5
O3^i—Ru1—N1	86.18 (14)	H5B—C5—H5C	109.5
O5^ii—Ru1—O3^i	169.81 (12)	F3^iv—F4—F3^iii	95.2 (18)
O5^ii—Ru1—N1	83.78 (13)	F3^iv—F4—P1	47.7 (9)
O4—Ru1—O2	173.52 (13)	F3^iii—F4—P1	47.6 (9)
O4—Ru1—O3^i	91.53 (12)	F4^iii—F3—F4^iv	98.3 (16)
O4—Ru1—O5^ii	89.39 (12)	F4^iii—F3—P1	86.2 (13)
O4—Ru1—N1	85.30 (14)	P1—F3—F4^iv	84.5 (12)
F5—P1B—F5^iv	98.1 (14)	C8—C9—N3	180 (4)
F5—P1B—F5^iii	98.1 (14)	C9—C8—H8A	109.7
F5^iii—P1B—F5^iv	98.1 (14)	C9—C8—H8B	109.7
F5^iii—P1B—F2	111.2 (13)	C9—C8—H8C	109.8
F5—P1B—F2^iv	111.2 (13)	H8A—C8—H8B	109.0
F5^iv—P1B—F2^iv	148.0 (13)	H8A—C8—H8C	109.3
F5^iv—P1B—F2^iii	111.2 (13)	H8B—C8—H8C	109.4
F5—P1B—F2	148.0 (13)	F4^iii—P1—F4	67.4 (8)
F5^iv—P1B—F2	66.1 (11)	F4^iv—P1—F4	67.4 (8)
F5^iii—P1B—F2^iv	66.1 (11)	F4^iii—P1—F4^iv	67.4 (8)
F5^iii—P1B—F2^iii	148.0 (13)	F3—P1—F4	97.4 (15)
F5—P1B—F2^iii	66.1 (11)	F3^iii—P1—F4	47.9 (11)
F2^iv—P1B—F2	92.9 (9)	F3—P1—F4^iv	47.9 (11)
F2^iii—P1B—F2^iv	92.9 (9)	F3^iii—P1—F4^iv	46.1 (10)
F2^iii—P1B—F2	92.9 (9)	F3^iii—P1—F4^iii	97.4 (15)
Ru1—O1—Ru1^i	119.965 (9)	F3^iv—P1—F4	46.1 (10)
Ru1—O1—Ru1^ii	119.964 (9)	F3^iv—P1—F4^iv	97.4 (15)
Ru1^i—O1—Ru1^ii	119.964 (9)	F3—P1—F4^iii	46.1 (10)
C4—O2—Ru1	125.8 (3)	F3^iv—P1—F4^iii	47.9 (11)
C4—O3—Ru1^ii	133.7 (3)	F3^iii—P1—F3	93.9 (17)
C6—O5—Ru1^i	131.4 (3)	F3^iv—P1—F3	93.9 (17)
C6—O4—Ru1	126.9 (3)	F3^iii—P1—F3^iv	93.9 (17)
C1—N1—Ru1	126.5 (3)	F3—P1—F1^iii	80.4 (12)
C1—N1—C3	106.5 (4)	F3^iv—P1—F1	80.4 (13)
C3—N1—Ru1	126.6 (3)	F3^iii—P1—F1	95.3 (10)
C1—N2—H2	126.1	F3^iii—P1—F1^iv	80.4 (12)
C1—N2—C2	107.8 (4)	F3—P1—F1	169.5 (12)
C2—N2—H2	126.1	F3^iv—P1—F1^iv	169.5 (12)
O5—C6—C7	117.6 (4)	F3^iv—P1—F1^iii	95.3 (10)
O4—C6—O5	126.0 (4)	F3—P1—F1^iv	95.3 (10)
O4—C6—C7	116.4 (4)	F3^iii—P1—F1^iii	169.5 (12)
N1—C1—N2	110.4 (4)	F1—P1—F4^iv	141.3 (7)
N1—C1—H1	124.8	F1^iii—P1—F4^iii	85.1 (7)
N2—C1—H1	124.8	F1^iii—P1—F4	141.3 (7)
C6—C7—H7A	109.5	F1^iii—P1—F4^iv	127.3 (9)
C6—C7—H7B	109.5	F1—P1—F4	85.1 (7)
C6—C7—H7C	109.5	F1^iv—P1—F4^iv	85.1 (7)
H7A—C7—H7B	109.5	F1^iv—P1—F4	127.3 (9)
H7A—C7—H7C	109.5	F1—P1—F4^iii	127.3 (9)
H7B—C7—H7C	109.5	F1^iv—P1—F4^iii	141.3 (7)
O2—C4—C5	116.8 (4)	F1—P1—F1^iv	91.3 (12)
O3—C4—O2	126.0 (4)	F1^iii—P1—F1^iv	91.3 (12)
O3—C4—C5	117.1 (4)	F1—P1—F1^iii	91.3 (12)
N1—C3—H3	125.6	P1B—F5—F2^iii	60.2 (11)
C2—C3—N1	108.9 (4)	P1B—F2—F5^iv	53.7 (9)
C2—C3—H3	125.6

Symmetry codes: (i) −y+1, z−1/2, −x+3/2; (ii) −z+3/2, −x+1, y+1/2; (iii) y, z, x; (iv) z, x, y.

Hexa-µ₂-acetato-carbonyl-µ₃-oxido-bis(4-phenylpyridine)triruthenium methanol monosolvate (ae817a)

Crystal data

[Ru3(C2H3O2)6O(C11H9N)2(CO)]·CH4O	F(000) = 2088
Mr = 1043.91	Dx = 1.746 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 7.8680 (9) Å	Cell parameters from 8467 reflections
b = 22.098 (3) Å	θ = 2.6–25.3°
c = 22.848 (3) Å	µ = 1.20 mm^−1
β = 90.312 (2)°	T = 173 K
V = 3972.4 (8) Å^3	Plate, blue
Z = 4	0.32 × 0.15 × 0.01 mm

Data collection

Bruker APEXII CCD diffractometer	7285 independent reflections
Radiation source: sealed tube	5241 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.075
Detector resolution: 8.36 pixels mm^-1	θmax = 25.4°, θmin = 1.3°
ω scans	h = −9→9
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −26→26
Tmin = 0.641, Tmax = 0.745	l = −27→27
31959 measured reflections

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.044	H-atom parameters constrained
wR(F^2) = 0.112	w = 1/[σ^2(Fo^2) + (0.0529P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
7285 reflections	Δρmax = 1.05 e Å^−3
513 parameters	Δρmin = −0.48 e Å^−3
0 restraints

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. The structure was refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008) incorporated in Olex2 (Dolomanov et al., 2009). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ru1	0.64933 (6)	0.72903 (2)	0.23660 (2)	0.02788 (13)
Ru2	0.44995 (6)	0.62796 (2)	0.32691 (2)	0.02711 (13)
Ru3	0.64605 (5)	0.57734 (2)	0.21013 (2)	0.02533 (13)
O1	0.5777 (4)	0.64228 (14)	0.25848 (15)	0.0256 (8)
O2	0.7761 (6)	0.85158 (19)	0.2049 (2)	0.0567 (13)
O3	0.4094 (5)	0.76366 (16)	0.25058 (18)	0.0377 (10)
O4	0.2919 (5)	0.70177 (16)	0.31712 (17)	0.0356 (9)
O5	0.7231 (5)	0.74744 (16)	0.32245 (17)	0.0358 (9)
O6	0.6147 (5)	0.67449 (17)	0.38026 (16)	0.0361 (9)
O7	0.2729 (5)	0.57568 (16)	0.28353 (16)	0.0337 (9)
O8	0.4351 (5)	0.52422 (16)	0.22112 (17)	0.0351 (9)
O9	0.5832 (5)	0.55267 (16)	0.35239 (16)	0.0367 (10)
O10	0.7629 (5)	0.53436 (16)	0.27846 (16)	0.0341 (9)
O11	0.5762 (5)	0.71387 (16)	0.14955 (17)	0.0377 (9)
O12	0.5350 (5)	0.61358 (16)	0.13671 (15)	0.0346 (9)
O13	0.8987 (5)	0.70308 (17)	0.22313 (19)	0.0437 (11)
O14	0.8762 (5)	0.61121 (17)	0.18462 (18)	0.0425 (10)
N1	0.2899 (6)	0.61469 (19)	0.40068 (19)	0.0329 (11)
N2	0.7290 (5)	0.50544 (18)	0.15647 (18)	0.0271 (10)
C1	0.7227 (8)	0.8053 (3)	0.2169 (3)	0.0367 (14)
C2	0.1196 (7)	0.6088 (3)	0.3921 (3)	0.0373 (14)
H2	0.0779	0.6073	0.3530	0.045*
C3	0.0048 (7)	0.6049 (2)	0.4370 (3)	0.0371 (14)
H3	−0.1129	0.6001	0.4287	0.045*
C4	0.0614 (7)	0.6080 (2)	0.4943 (3)	0.0326 (13)
C5	0.2342 (8)	0.6144 (2)	0.5034 (3)	0.0394 (15)
H5	0.2784	0.6176	0.5420	0.047*
C6	0.3436 (8)	0.6163 (2)	0.4555 (2)	0.0361 (14)
H6	0.4624	0.6188	0.4628	0.043*
C7	−0.0650 (8)	0.6049 (3)	0.5437 (3)	0.0384 (14)
C8	−0.1941 (8)	0.5626 (3)	0.5424 (3)	0.0465 (16)
H8	−0.2036	0.5356	0.5102	0.056*
C9	−0.3110 (9)	0.5590 (3)	0.5883 (3)	0.061 (2)
H9	−0.3987	0.5295	0.5876	0.073*
C10	−0.2974 (9)	0.5990 (3)	0.6345 (3)	0.062 (2)
H10	−0.3767	0.5973	0.6657	0.075*
C11	−0.1678 (9)	0.6416 (3)	0.6355 (3)	0.0531 (18)
H11	−0.1595	0.6693	0.6672	0.064*
C12	−0.0497 (8)	0.6441 (3)	0.5903 (3)	0.0426 (15)
H12	0.0405	0.6727	0.5916	0.051*
C13	0.7912 (7)	0.5162 (3)	0.1029 (3)	0.0400 (15)
H13	0.7838	0.5561	0.0876	0.048*
C14	0.8650 (8)	0.4721 (3)	0.0693 (3)	0.0434 (15)
H14	0.9053	0.4818	0.0313	0.052*
C15	0.8813 (7)	0.4134 (3)	0.0902 (3)	0.0368 (14)
C16	0.8120 (7)	0.4025 (3)	0.1448 (3)	0.0390 (15)
H16	0.8177	0.3630	0.1610	0.047*
C17	0.7355 (7)	0.4477 (3)	0.1759 (3)	0.0388 (14)
H17	0.6851	0.4382	0.2124	0.047*
C18	0.9741 (7)	0.3673 (2)	0.0563 (3)	0.0375 (14)
C19	0.9793 (8)	0.3682 (3)	−0.0042 (3)	0.0437 (15)
H19	0.9220	0.3993	−0.0252	0.052*
C20	1.0674 (8)	0.3242 (3)	−0.0344 (3)	0.0495 (17)
H20	1.0702	0.3257	−0.0759	0.059*
C21	1.1502 (8)	0.2788 (3)	−0.0061 (3)	0.0515 (18)
H21	1.2077	0.2483	−0.0276	0.062*
C22	1.1497 (8)	0.2775 (3)	0.0543 (3)	0.0468 (16)
H22	1.2096	0.2467	0.0747	0.056*
C23	1.0612 (7)	0.3216 (3)	0.0853 (3)	0.0405 (15)
H23	1.0605	0.3203	0.1269	0.049*
C24	0.2966 (7)	0.7492 (2)	0.2861 (2)	0.0308 (13)
C25	0.1470 (7)	0.7922 (3)	0.2923 (3)	0.0421 (15)
H25A	0.1659	0.8187	0.3261	0.063*
H25B	0.0425	0.7689	0.2980	0.063*
H25C	0.1363	0.8168	0.2567	0.063*
C26	0.7070 (7)	0.7204 (3)	0.3699 (3)	0.0337 (13)
C27	0.8092 (8)	0.7442 (3)	0.4210 (3)	0.0416 (15)
H27A	0.9258	0.7288	0.4187	0.062*
H27B	0.7574	0.7307	0.4576	0.062*
H27C	0.8108	0.7885	0.4198	0.062*
C28	0.2987 (7)	0.5342 (2)	0.2472 (2)	0.0302 (13)
C29	0.1497 (7)	0.4932 (3)	0.2320 (3)	0.0413 (15)
H29A	0.0487	0.5066	0.2533	0.062*
H29B	0.1772	0.4515	0.2431	0.062*
H29C	0.1273	0.4951	0.1898	0.062*
C30	0.7089 (7)	0.5267 (2)	0.3299 (2)	0.0296 (12)
C31	0.8025 (7)	0.4817 (2)	0.3663 (2)	0.0380 (14)
H31A	0.7798	0.4894	0.4078	0.057*
H31B	0.9247	0.4854	0.3590	0.057*
H31C	0.7646	0.4408	0.3560	0.057*
C32	0.5280 (7)	0.6689 (3)	0.1211 (2)	0.0314 (13)
C33	0.4518 (8)	0.6805 (3)	0.0617 (2)	0.0418 (15)
H33A	0.4357	0.7241	0.0562	0.063*
H33B	0.3417	0.6599	0.0586	0.063*
H33C	0.5282	0.6650	0.0315	0.063*
C34	0.9574 (7)	0.6582 (3)	0.1972 (3)	0.0327 (13)
C35	1.1377 (7)	0.6611 (3)	0.1769 (3)	0.0387 (14)
H35A	1.1599	0.7011	0.1600	0.058*
H35B	1.1567	0.6299	0.1472	0.058*
H35C	1.2144	0.6543	0.2102	0.058*
O1S	0.3088 (7)	0.5284 (2)	0.0740 (3)	0.0809 (17)
H1S	0.3706	0.5465	0.0984	0.121*
C1S	0.3580 (10)	0.4677 (3)	0.0707 (4)	0.078 (2)
H1SA	0.4650	0.4646	0.0492	0.117*
H1SB	0.2697	0.4444	0.0504	0.117*
H1SC	0.3739	0.4516	0.1103	0.117*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ru1	0.0296 (3)	0.0239 (2)	0.0301 (3)	−0.00176 (18)	0.00353 (19)	0.00253 (19)
Ru2	0.0303 (3)	0.0241 (2)	0.0270 (3)	−0.00130 (19)	0.00530 (19)	0.00161 (18)
Ru3	0.0259 (2)	0.0239 (2)	0.0262 (3)	−0.00150 (18)	0.00342 (19)	0.00091 (18)
O1	0.0240 (19)	0.0233 (18)	0.030 (2)	0.0004 (15)	0.0022 (16)	−0.0017 (16)
O2	0.071 (3)	0.034 (2)	0.066 (3)	−0.015 (2)	−0.003 (3)	0.013 (2)
O3	0.028 (2)	0.035 (2)	0.050 (3)	0.0042 (17)	0.0119 (19)	0.0079 (19)
O4	0.037 (2)	0.033 (2)	0.037 (2)	0.0082 (17)	0.0060 (18)	0.0019 (18)
O5	0.040 (2)	0.034 (2)	0.034 (2)	−0.0106 (18)	0.0001 (19)	0.0028 (18)
O6	0.040 (2)	0.034 (2)	0.034 (2)	−0.0087 (19)	−0.0028 (18)	0.0026 (18)
O7	0.029 (2)	0.035 (2)	0.038 (2)	−0.0047 (17)	0.0087 (18)	−0.0056 (18)
O8	0.028 (2)	0.033 (2)	0.045 (2)	−0.0088 (17)	0.0106 (18)	−0.0101 (18)
O9	0.044 (2)	0.030 (2)	0.036 (2)	0.0050 (18)	0.0134 (19)	0.0112 (18)
O10	0.040 (2)	0.036 (2)	0.026 (2)	0.0056 (18)	0.0003 (18)	0.0062 (17)
O11	0.050 (3)	0.029 (2)	0.035 (2)	−0.0063 (18)	0.0026 (19)	0.0029 (18)
O12	0.047 (2)	0.033 (2)	0.024 (2)	0.0040 (18)	−0.0050 (18)	0.0000 (17)
O13	0.029 (2)	0.031 (2)	0.071 (3)	−0.0048 (18)	0.013 (2)	−0.008 (2)
O14	0.033 (2)	0.036 (2)	0.058 (3)	−0.0098 (19)	0.015 (2)	−0.007 (2)
N1	0.049 (3)	0.023 (2)	0.027 (3)	0.003 (2)	0.012 (2)	0.005 (2)
N2	0.030 (3)	0.027 (2)	0.025 (3)	−0.0004 (19)	0.002 (2)	−0.0005 (19)
C1	0.044 (4)	0.027 (3)	0.038 (4)	−0.001 (3)	−0.002 (3)	−0.001 (3)
C2	0.031 (3)	0.041 (3)	0.040 (4)	−0.001 (3)	0.010 (3)	−0.001 (3)
C3	0.032 (3)	0.036 (3)	0.044 (4)	−0.003 (3)	0.007 (3)	−0.001 (3)
C4	0.033 (3)	0.024 (3)	0.041 (4)	0.004 (2)	0.003 (3)	−0.003 (3)
C5	0.049 (4)	0.036 (3)	0.033 (4)	−0.003 (3)	−0.002 (3)	0.004 (3)
C6	0.047 (4)	0.027 (3)	0.035 (4)	−0.001 (3)	0.006 (3)	0.004 (3)
C7	0.046 (4)	0.036 (3)	0.033 (3)	0.006 (3)	0.006 (3)	0.010 (3)
C8	0.052 (4)	0.044 (4)	0.044 (4)	−0.005 (3)	0.012 (3)	−0.004 (3)
C9	0.050 (4)	0.065 (5)	0.068 (5)	−0.020 (4)	0.025 (4)	−0.003 (4)
C10	0.058 (5)	0.081 (5)	0.047 (4)	−0.015 (4)	0.020 (4)	−0.006 (4)
C11	0.055 (4)	0.060 (4)	0.044 (4)	0.003 (4)	0.010 (3)	−0.013 (3)
C12	0.047 (4)	0.038 (3)	0.042 (4)	−0.001 (3)	0.007 (3)	0.000 (3)
C13	0.045 (4)	0.038 (3)	0.038 (4)	0.007 (3)	0.005 (3)	0.004 (3)
C14	0.052 (4)	0.039 (3)	0.039 (4)	0.004 (3)	0.014 (3)	0.006 (3)
C15	0.032 (3)	0.040 (3)	0.039 (4)	−0.004 (3)	0.004 (3)	−0.001 (3)
C16	0.050 (4)	0.025 (3)	0.042 (4)	−0.005 (3)	0.009 (3)	0.001 (3)
C17	0.045 (4)	0.038 (3)	0.034 (3)	0.001 (3)	0.003 (3)	0.002 (3)
C18	0.038 (4)	0.032 (3)	0.042 (4)	−0.002 (3)	0.004 (3)	−0.005 (3)
C19	0.050 (4)	0.046 (4)	0.035 (4)	0.001 (3)	0.001 (3)	0.001 (3)
C20	0.061 (5)	0.053 (4)	0.035 (4)	0.008 (3)	0.007 (3)	−0.002 (3)
C21	0.053 (4)	0.040 (4)	0.061 (5)	0.008 (3)	0.010 (4)	−0.003 (3)
C22	0.051 (4)	0.042 (4)	0.047 (4)	0.012 (3)	0.010 (3)	−0.003 (3)
C23	0.047 (4)	0.037 (3)	0.038 (4)	−0.004 (3)	0.007 (3)	0.007 (3)
C24	0.029 (3)	0.032 (3)	0.032 (3)	−0.001 (2)	−0.001 (3)	0.002 (3)
C25	0.034 (3)	0.036 (3)	0.056 (4)	0.002 (3)	−0.005 (3)	−0.003 (3)
C26	0.033 (3)	0.035 (3)	0.033 (3)	0.002 (3)	0.000 (3)	−0.002 (3)
C27	0.047 (4)	0.041 (3)	0.037 (4)	−0.007 (3)	−0.005 (3)	−0.006 (3)
C28	0.031 (3)	0.030 (3)	0.030 (3)	0.001 (2)	−0.003 (3)	0.005 (3)
C29	0.036 (3)	0.037 (3)	0.052 (4)	−0.006 (3)	0.003 (3)	−0.009 (3)
C30	0.032 (3)	0.027 (3)	0.030 (3)	−0.007 (2)	0.000 (3)	−0.001 (2)
C31	0.046 (4)	0.030 (3)	0.038 (4)	0.005 (3)	0.000 (3)	0.006 (3)
C32	0.021 (3)	0.043 (4)	0.030 (3)	0.004 (3)	0.002 (2)	0.004 (3)
C33	0.053 (4)	0.038 (3)	0.034 (3)	−0.005 (3)	−0.008 (3)	0.004 (3)
C34	0.028 (3)	0.033 (3)	0.037 (3)	−0.001 (3)	0.004 (3)	0.007 (3)
C35	0.028 (3)	0.042 (3)	0.046 (4)	−0.003 (3)	0.005 (3)	0.002 (3)
O1S	0.094 (4)	0.058 (3)	0.090 (4)	0.002 (3)	−0.042 (3)	−0.011 (3)
C1S	0.061 (5)	0.068 (5)	0.104 (7)	−0.017 (4)	−0.016 (5)	−0.009 (5)

Geometric parameters (Å, º)

Ru1—O1	2.060 (3)	C11—H11	0.9500
Ru1—O3	2.063 (4)	C11—C12	1.394 (8)
Ru1—O5	2.082 (4)	C12—H12	0.9500
Ru1—O11	2.094 (4)	C13—H13	0.9500
Ru1—O13	2.069 (4)	C13—C14	1.373 (8)
Ru1—C1	1.839 (6)	C14—H14	0.9500
Ru2—O1	1.890 (3)	C14—C15	1.388 (8)
Ru2—O4	2.062 (4)	C15—C16	1.385 (8)
Ru2—O6	2.051 (4)	C15—C18	1.477 (8)
Ru2—O7	2.060 (4)	C16—H16	0.9500
Ru2—O9	2.049 (4)	C16—C17	1.367 (8)
Ru2—N1	2.130 (4)	C17—H17	0.9500
Ru3—O1	1.891 (3)	C18—C19	1.384 (8)
Ru3—O8	2.050 (3)	C18—C23	1.388 (8)
Ru3—O10	2.042 (4)	C19—H19	0.9500
Ru3—O12	2.050 (4)	C19—C20	1.381 (8)
Ru3—O14	2.047 (4)	C20—H20	0.9500
Ru3—N2	2.112 (4)	C20—C21	1.358 (9)
O2—C1	1.139 (6)	C21—H21	0.9500
O3—C24	1.247 (6)	C21—C22	1.381 (9)
O4—C24	1.265 (6)	C22—H22	0.9500
O5—C26	1.245 (6)	C22—C23	1.392 (8)
O6—C26	1.270 (6)	C23—H23	0.9500
O7—C28	1.254 (6)	C24—C25	1.521 (8)
O8—C28	1.249 (6)	C25—H25A	0.9800
O9—C30	1.256 (6)	C25—H25B	0.9800
O10—C30	1.263 (6)	C25—H25C	0.9800
O11—C32	1.246 (6)	C26—C27	1.508 (8)
O12—C32	1.274 (6)	C27—H27A	0.9800
O13—C34	1.246 (6)	C27—H27B	0.9800
O14—C34	1.251 (6)	C27—H27C	0.9800
N1—C2	1.359 (7)	C28—C29	1.520 (7)
N1—C6	1.321 (7)	C29—H29A	0.9800
N2—C13	1.342 (7)	C29—H29B	0.9800
N2—C17	1.351 (7)	C29—H29C	0.9800
C2—H2	0.9500	C30—C31	1.488 (7)
C2—C3	1.373 (8)	C31—H31A	0.9800
C3—H3	0.9500	C31—H31B	0.9800
C3—C4	1.383 (8)	C31—H31C	0.9800
C4—C5	1.381 (8)	C32—C33	1.503 (8)
C4—C7	1.510 (8)	C33—H33A	0.9800
C5—H5	0.9500	C33—H33B	0.9800
C5—C6	1.396 (8)	C33—H33C	0.9800
C6—H6	0.9500	C34—C35	1.497 (8)
C7—C8	1.381 (8)	C35—H35A	0.9800
C7—C12	1.376 (8)	C35—H35B	0.9800
C8—H8	0.9500	C35—H35C	0.9800
C8—C9	1.400 (8)	O1S—H1S	0.8400
C9—H9	0.9500	O1S—C1S	1.398 (8)
C9—C10	1.380 (9)	C1S—H1SA	0.9800
C10—H10	0.9500	C1S—H1SB	0.9800
C10—C11	1.388 (9)	C1S—H1SC	0.9800
O1—Ru1—O3	93.21 (14)	C7—C12—C11	119.4 (6)
O1—Ru1—O5	91.63 (14)	C7—C12—H12	120.3
O1—Ru1—O11	90.43 (14)	C11—C12—H12	120.3
O1—Ru1—O13	92.24 (14)	N2—C13—H13	118.6
O3—Ru1—O5	91.85 (16)	N2—C13—C14	122.8 (5)
O3—Ru1—O11	87.67 (16)	C14—C13—H13	118.6
O3—Ru1—O13	174.28 (14)	C13—C14—H14	119.7
O5—Ru1—O11	177.91 (14)	C13—C14—C15	120.5 (6)
O13—Ru1—O5	86.25 (16)	C15—C14—H14	119.7
O13—Ru1—O11	94.04 (16)	C14—C15—C18	120.6 (5)
C1—Ru1—O1	177.5 (2)	C16—C15—C14	115.9 (5)
C1—Ru1—O3	89.2 (2)	C16—C15—C18	123.5 (5)
C1—Ru1—O5	88.0 (2)	C15—C16—H16	119.4
C1—Ru1—O11	90.0 (2)	C17—C16—C15	121.1 (5)
C1—Ru1—O13	85.3 (2)	C17—C16—H16	119.4
O1—Ru2—O4	95.80 (14)	N2—C17—C16	122.4 (5)
O1—Ru2—O6	94.03 (15)	N2—C17—H17	118.8
O1—Ru2—O7	93.29 (14)	C16—C17—H17	118.8
O1—Ru2—O9	95.58 (14)	C19—C18—C15	122.2 (5)
O1—Ru2—N1	175.68 (16)	C19—C18—C23	118.1 (5)
O4—Ru2—N1	80.56 (16)	C23—C18—C15	119.7 (5)
O6—Ru2—O4	92.68 (15)	C18—C19—H19	119.8
O6—Ru2—O7	172.23 (14)	C20—C19—C18	120.4 (6)
O6—Ru2—N1	88.47 (17)	C20—C19—H19	119.8
O7—Ru2—O4	89.18 (15)	C19—C20—H20	119.2
O7—Ru2—N1	84.39 (16)	C21—C20—C19	121.5 (6)
O9—Ru2—O4	168.55 (15)	C21—C20—H20	119.2
O9—Ru2—O6	85.25 (15)	C20—C21—H21	120.4
O9—Ru2—O7	91.44 (15)	C20—C21—C22	119.2 (6)
O9—Ru2—N1	88.12 (16)	C22—C21—H21	120.4
O1—Ru3—O8	97.47 (14)	C21—C22—H22	120.1
O1—Ru3—O10	91.98 (14)	C21—C22—C23	119.9 (6)
O1—Ru3—O12	93.45 (14)	C23—C22—H22	120.1
O1—Ru3—O14	98.25 (15)	C18—C23—C22	120.9 (6)
O1—Ru3—N2	178.52 (15)	C18—C23—H23	119.6
O8—Ru3—O12	88.97 (15)	C22—C23—H23	119.6
O8—Ru3—N2	83.88 (15)	O3—C24—O4	126.9 (5)
O10—Ru3—O8	90.09 (15)	O3—C24—C25	117.0 (5)
O10—Ru3—O12	174.56 (14)	O4—C24—C25	116.2 (5)
O10—Ru3—O14	89.56 (16)	C24—C25—H25A	109.5
O10—Ru3—N2	87.40 (15)	C24—C25—H25B	109.5
O12—Ru3—N2	87.17 (15)	C24—C25—H25C	109.5
O14—Ru3—O8	164.28 (15)	H25A—C25—H25B	109.5
O14—Ru3—O12	89.89 (16)	H25A—C25—H25C	109.5
O14—Ru3—N2	80.40 (15)	H25B—C25—H25C	109.5
Ru2—O1—Ru1	120.25 (16)	O5—C26—O6	127.4 (5)
Ru2—O1—Ru3	120.68 (16)	O5—C26—C27	116.8 (5)
Ru3—O1—Ru1	119.05 (17)	O6—C26—C27	115.9 (5)
C24—O3—Ru1	131.3 (4)	C26—C27—H27A	109.5
C24—O4—Ru2	134.1 (4)	C26—C27—H27B	109.5
C26—O5—Ru1	134.2 (4)	C26—C27—H27C	109.5
C26—O6—Ru2	130.5 (4)	H27A—C27—H27B	109.5
C28—O7—Ru2	128.1 (3)	H27A—C27—H27C	109.5
C28—O8—Ru3	130.9 (3)	H27B—C27—H27C	109.5
C30—O9—Ru2	131.1 (3)	O7—C28—C29	117.3 (5)
C30—O10—Ru3	128.4 (4)	O8—C28—O7	126.0 (5)
C32—O11—Ru1	134.8 (4)	O8—C28—C29	116.7 (5)
C32—O12—Ru3	128.4 (4)	C28—C29—H29A	109.5
C34—O13—Ru1	130.2 (4)	C28—C29—H29B	109.5
C34—O14—Ru3	133.5 (4)	C28—C29—H29C	109.5
C2—N1—Ru2	119.1 (4)	H29A—C29—H29B	109.5
C6—N1—Ru2	124.0 (4)	H29A—C29—H29C	109.5
C6—N1—C2	116.7 (5)	H29B—C29—H29C	109.5
C13—N2—Ru3	120.7 (4)	O9—C30—O10	126.1 (5)
C13—N2—C17	117.0 (5)	O9—C30—C31	117.7 (5)
C17—N2—Ru3	122.0 (4)	O10—C30—C31	116.2 (5)
O2—C1—Ru1	176.6 (5)	C30—C31—H31A	109.5
N1—C2—H2	118.3	C30—C31—H31B	109.5
N1—C2—C3	123.4 (6)	C30—C31—H31C	109.5
C3—C2—H2	118.3	H31A—C31—H31B	109.5
C2—C3—H3	120.2	H31A—C31—H31C	109.5
C2—C3—C4	119.6 (6)	H31B—C31—H31C	109.5
C4—C3—H3	120.2	O11—C32—O12	127.3 (5)
C3—C4—C7	119.7 (5)	O11—C32—C33	117.0 (5)
C5—C4—C3	117.3 (5)	O12—C32—C33	115.7 (5)
C5—C4—C7	123.0 (5)	C32—C33—H33A	109.5
C4—C5—H5	120.1	C32—C33—H33B	109.5
C4—C5—C6	119.8 (6)	C32—C33—H33C	109.5
C6—C5—H5	120.1	H33A—C33—H33B	109.5
N1—C6—C5	123.1 (6)	H33A—C33—H33C	109.5
N1—C6—H6	118.4	H33B—C33—H33C	109.5
C5—C6—H6	118.4	O13—C34—O14	125.5 (5)
C8—C7—C4	120.1 (5)	O13—C34—C35	117.9 (5)
C12—C7—C4	119.6 (5)	O14—C34—C35	116.6 (5)
C12—C7—C8	120.3 (6)	C34—C35—H35A	109.5
C7—C8—H8	119.8	C34—C35—H35B	109.5
C7—C8—C9	120.5 (6)	C34—C35—H35C	109.5
C9—C8—H8	119.8	H35A—C35—H35B	109.5
C8—C9—H9	120.4	H35A—C35—H35C	109.5
C10—C9—C8	119.2 (6)	H35B—C35—H35C	109.5
C10—C9—H9	120.4	C1S—O1S—H1S	109.5
C9—C10—H10	120.0	O1S—C1S—H1SA	109.5
C9—C10—C11	120.0 (6)	O1S—C1S—H1SB	109.5
C11—C10—H10	120.0	O1S—C1S—H1SC	109.5
C10—C11—H11	119.7	H1SA—C1S—H1SB	109.5
C10—C11—C12	120.5 (6)	H1SA—C1S—H1SC	109.5
C12—C11—H11	119.7	H1SB—C1S—H1SC	109.5

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1S—H1S···O12	0.84	2.15	2.956 (6)	161