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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618013451/fn3271sup1.cif
Contains datablocks ae218b, ae218d, ae418a, ae817a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618013451/fn3271ae218bsup2.hkl
Contains datablock ae218b

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618013451/fn3271ae218dsup3.hkl
Contains datablock ae218d

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618013451/fn3271ae418asup4.hkl
Contains datablock ae418a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618013451/fn3271ae817asup5.hkl
Contains datablock ae817a

cdx

Chemdraw file https://doi.org/10.1107/S2053229618013451/fn3271ae218bsup6.cdx
Supplementary material

cdx

Chemdraw file https://doi.org/10.1107/S2053229618013451/fn3271ae218dsup7.cdx
Supplementary material

cdx

Chemdraw file https://doi.org/10.1107/S2053229618013451/fn3271ae418asup8.cdx
Supplementary material

cdx

Chemdraw file https://doi.org/10.1107/S2053229618013451/fn3271ae817asup9.cdx
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618013451/fn3271sup10.pdf
Cyclic voltammograms and mass spectra

CCDC references: 1857619; 1857722; 1857618; 1857613

Computing details top

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) top
Crystal data top
[Ru3(C2H3O2)6O(C3H4N2)(CO)]·CH4OF(000) = 1720
Mr = 869.69Dx = 1.789 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 9.6807 (6) ÅCell parameters from 9874 reflections
b = 18.5596 (12) Åθ = 2.2–27.5°
c = 18.5805 (12) ŵ = 1.45 mm1
β = 104.746 (1)°T = 173 K
V = 3228.4 (4) Å3Plate, blue
Z = 40.24 × 0.22 × 0.05 mm
Data collection top
Bruker APEXII CCD
diffractometer
7410 independent reflections
Radiation source: sealed tube6119 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
Detector resolution: 8.36 pixels mm-1θmax = 27.5°, θmin = 1.6°
ω scansh = 1212
Absorption correction: multi-scan
(SADABS; Bruker, 2015)
k = 2424
Tmin = 0.024, Tmax = 0.047l = 2424
59780 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.123 w = 1/[σ2(Fo2) + (0.0731P)2 + 3.9385P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
7410 reflectionsΔρmax = 2.15 e Å3
407 parametersΔρmin = 0.56 e Å3
0 restraints
Special details top

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 (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.47767 (4)0.62811 (2)0.66768 (2)0.02732 (10)
Ru20.40818 (3)0.58165 (2)0.82543 (2)0.02553 (10)
Ru30.72472 (3)0.52985 (2)0.79256 (2)0.02673 (10)
O10.5332 (3)0.58171 (14)0.76191 (15)0.0261 (6)
O20.2933 (3)0.56822 (17)0.63426 (16)0.0354 (7)
O30.2238 (3)0.57232 (17)0.74073 (17)0.0343 (6)
O40.3600 (3)0.70884 (15)0.70121 (16)0.0327 (6)
O50.3897 (3)0.69139 (15)0.82375 (15)0.0312 (6)
O60.5647 (3)0.59419 (17)0.92281 (16)0.0337 (6)
O70.7761 (3)0.58444 (16)0.89450 (16)0.0336 (6)
O80.4082 (3)0.47271 (15)0.83557 (18)0.0349 (7)
O90.6338 (3)0.44319 (15)0.83507 (16)0.0317 (6)
O100.8271 (3)0.61362 (17)0.75165 (18)0.0359 (7)
O110.6565 (3)0.69120 (16)0.69124 (17)0.0356 (7)
O120.6819 (3)0.47445 (15)0.69239 (16)0.0344 (7)
O130.5794 (3)0.55993 (16)0.61050 (16)0.0355 (7)
O140.9880 (4)0.4380 (2)0.8278 (2)0.0527 (9)
N10.4155 (4)0.68289 (19)0.56596 (19)0.0354 (8)
N20.4148 (6)0.7414 (2)0.4649 (2)0.0568 (13)
H20.44600.76110.42890.068*
N30.2692 (4)0.58160 (18)0.89548 (19)0.0293 (7)
N40.0713 (4)0.5896 (2)0.9314 (2)0.0339 (8)
H40.01930.59680.92960.041*
C10.4944 (6)0.7033 (3)0.5223 (2)0.0443 (12)
H10.59320.69280.52980.053*
C20.2809 (8)0.7443 (3)0.4714 (3)0.0562 (15)
H2A0.20160.76690.43840.067*
C30.2816 (6)0.7086 (3)0.5344 (3)0.0488 (13)
H30.20090.70220.55410.059*
C40.1315 (4)0.5954 (2)0.8741 (2)0.0318 (9)
H4A0.08140.60780.82470.038*
C50.1760 (5)0.5704 (3)0.9933 (3)0.0368 (10)
H50.16550.56211.04200.044*
C60.2973 (5)0.5658 (3)0.9701 (2)0.0365 (9)
H60.38850.55341.00090.044*
C70.2031 (5)0.5606 (3)0.6725 (3)0.0375 (10)
C80.0559 (6)0.5354 (4)0.6320 (3)0.0573 (15)
H8A0.05830.48360.62210.086*
H8B0.02430.56140.58480.086*
H8C0.01070.54470.66280.086*
C90.3494 (4)0.7287 (2)0.7633 (2)0.0310 (8)
C100.2831 (6)0.8011 (2)0.7690 (3)0.0401 (10)
H10A0.20770.79590.79520.060*
H10B0.24200.82010.71890.060*
H10C0.35640.83430.79650.060*
C110.6983 (5)0.5996 (2)0.9375 (2)0.0317 (9)
C120.7727 (5)0.6259 (3)1.0145 (3)0.0488 (13)
H12A0.87630.62121.02220.073*
H12B0.74160.59711.05170.073*
H12C0.74850.67661.01950.073*
C130.5108 (5)0.4288 (2)0.8420 (2)0.0336 (9)
C140.4822 (6)0.3524 (2)0.8607 (3)0.0421 (11)
H14A0.53660.31940.83710.063*
H14B0.38000.34200.84250.063*
H14C0.51150.34580.91480.063*
C150.7835 (5)0.6713 (2)0.7189 (3)0.0381 (10)
C160.8979 (7)0.7244 (4)0.7108 (4)0.072 (2)
H16A0.94590.74390.75980.108*
H16B0.85370.76380.67780.108*
H16C0.96780.69970.68960.108*
C170.6406 (5)0.5005 (2)0.6282 (2)0.0323 (9)
C180.6709 (6)0.4565 (3)0.5655 (3)0.0434 (11)
H18A0.72540.48560.53840.065*
H18B0.58050.44150.53150.065*
H18C0.72650.41370.58600.065*
C190.8921 (5)0.4766 (2)0.8162 (2)0.0342 (9)
O150.8235 (14)0.8141 (6)1.0013 (7)0.097 (4)0.5
H150.77020.84760.98010.145*0.5
C210.9033 (18)0.7871 (10)0.9528 (16)0.141 (10)0.5
H21A0.84020.78120.90280.211*0.5
H21B0.94490.74040.97120.211*0.5
H21C0.97980.82100.95100.211*0.5
O160.6812 (9)0.9193 (4)0.9102 (4)0.0494 (18)0.5
H160.74570.95050.91480.074*0.5
C220.6546 (13)0.8890 (6)0.8402 (6)0.053 (3)0.5
H22A0.56120.90520.81030.080*0.5
H22B0.65480.83640.84440.080*0.5
H22C0.72900.90400.81600.080*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.03264 (19)0.02588 (17)0.02346 (17)0.00168 (12)0.00718 (13)0.00102 (11)
Ru20.02497 (17)0.02691 (17)0.02479 (17)0.00049 (11)0.00646 (13)0.00183 (11)
Ru30.02659 (18)0.02874 (18)0.02511 (17)0.00108 (12)0.00703 (13)0.00105 (12)
O10.0274 (14)0.0275 (13)0.0236 (13)0.0001 (11)0.0071 (11)0.0001 (10)
O20.0383 (17)0.0388 (16)0.0285 (15)0.0011 (13)0.0072 (13)0.0043 (12)
O30.0303 (15)0.0406 (17)0.0299 (15)0.0001 (12)0.0037 (12)0.0000 (13)
O40.0403 (17)0.0311 (15)0.0272 (14)0.0041 (12)0.0094 (12)0.0004 (12)
O50.0405 (17)0.0273 (14)0.0269 (14)0.0017 (12)0.0103 (12)0.0012 (11)
O60.0278 (15)0.0460 (17)0.0265 (14)0.0007 (13)0.0055 (12)0.0015 (13)
O70.0296 (15)0.0424 (17)0.0291 (15)0.0003 (12)0.0080 (12)0.0061 (12)
O80.0319 (16)0.0277 (15)0.0477 (18)0.0014 (11)0.0147 (14)0.0056 (13)
O90.0337 (16)0.0272 (14)0.0353 (16)0.0025 (12)0.0106 (12)0.0058 (12)
O100.0318 (16)0.0381 (16)0.0396 (17)0.0018 (13)0.0124 (13)0.0068 (13)
O110.0365 (17)0.0314 (15)0.0392 (17)0.0002 (13)0.0099 (13)0.0046 (13)
O120.0438 (18)0.0314 (15)0.0287 (15)0.0075 (13)0.0107 (13)0.0003 (12)
O130.0467 (18)0.0337 (15)0.0275 (15)0.0089 (14)0.0118 (13)0.0005 (12)
O140.0367 (19)0.052 (2)0.066 (2)0.0146 (16)0.0059 (17)0.0010 (18)
N10.054 (2)0.0270 (17)0.0252 (17)0.0045 (16)0.0101 (16)0.0004 (14)
N20.099 (4)0.041 (2)0.028 (2)0.011 (2)0.012 (2)0.0075 (17)
N30.0280 (17)0.0326 (18)0.0275 (17)0.0006 (13)0.0075 (14)0.0022 (14)
N40.0236 (17)0.045 (2)0.0331 (19)0.0027 (15)0.0081 (14)0.0026 (16)
C10.068 (3)0.037 (2)0.027 (2)0.009 (2)0.009 (2)0.0003 (18)
C20.082 (4)0.044 (3)0.036 (3)0.017 (3)0.002 (3)0.005 (2)
C30.061 (3)0.051 (3)0.033 (2)0.020 (2)0.007 (2)0.005 (2)
C40.028 (2)0.034 (2)0.032 (2)0.0011 (16)0.0064 (17)0.0010 (17)
C50.034 (2)0.045 (3)0.033 (2)0.0017 (19)0.0122 (18)0.0064 (19)
C60.033 (2)0.046 (2)0.032 (2)0.0045 (19)0.0119 (18)0.0061 (19)
C70.036 (2)0.038 (2)0.035 (2)0.0006 (19)0.0037 (19)0.0024 (18)
C80.042 (3)0.083 (4)0.043 (3)0.009 (3)0.002 (2)0.007 (3)
C90.031 (2)0.030 (2)0.033 (2)0.0007 (16)0.0090 (17)0.0001 (16)
C100.055 (3)0.033 (2)0.038 (2)0.007 (2)0.022 (2)0.0027 (18)
C110.029 (2)0.037 (2)0.028 (2)0.0009 (17)0.0047 (16)0.0005 (17)
C120.031 (2)0.077 (4)0.036 (3)0.001 (2)0.005 (2)0.020 (2)
C130.043 (2)0.031 (2)0.029 (2)0.0007 (18)0.0135 (18)0.0015 (16)
C140.051 (3)0.028 (2)0.053 (3)0.0017 (19)0.024 (2)0.005 (2)
C150.042 (3)0.036 (2)0.037 (2)0.0046 (19)0.0117 (19)0.0029 (19)
C160.048 (3)0.062 (4)0.106 (5)0.010 (3)0.017 (3)0.034 (4)
C170.034 (2)0.033 (2)0.029 (2)0.0045 (17)0.0066 (17)0.0034 (17)
C180.056 (3)0.040 (2)0.033 (2)0.011 (2)0.009 (2)0.0066 (19)
C190.034 (2)0.036 (2)0.033 (2)0.0018 (18)0.0096 (18)0.0000 (17)
O150.102 (9)0.082 (7)0.106 (9)0.021 (6)0.027 (7)0.044 (6)
C210.065 (10)0.100 (13)0.28 (3)0.028 (9)0.088 (16)0.081 (17)
O160.067 (5)0.035 (4)0.046 (4)0.001 (3)0.015 (4)0.010 (3)
C220.057 (7)0.057 (6)0.045 (6)0.015 (5)0.014 (5)0.016 (5)
Geometric parameters (Å, º) top
Ru1—O11.902 (3)C2—H2A0.9500
Ru1—O22.060 (3)C2—C31.344 (7)
Ru1—O42.072 (3)C3—H30.9500
Ru1—O112.043 (3)C4—H4A0.9500
Ru1—O132.057 (3)C5—H50.9500
Ru1—N12.095 (4)C5—C61.352 (6)
Ru2—O11.893 (3)C6—H60.9500
Ru2—O32.064 (3)C7—C81.506 (7)
Ru2—O52.044 (3)C8—H8A0.9800
Ru2—O62.056 (3)C8—H8B0.9800
Ru2—O82.031 (3)C8—H8C0.9800
Ru2—N32.097 (3)C9—C101.504 (6)
Ru3—O12.038 (3)C10—H10A0.9800
Ru3—O72.093 (3)C10—H10B0.9800
Ru3—O92.083 (3)C10—H10C0.9800
Ru3—O102.088 (3)C11—C121.510 (6)
Ru3—O122.074 (3)C12—H12A0.9800
Ru3—C191.853 (5)C12—H12B0.9800
O2—C71.267 (6)C12—H12C0.9800
O3—C71.251 (5)C13—C141.503 (6)
O4—C91.241 (5)C14—H14A0.9800
O5—C91.292 (5)C14—H14B0.9800
O6—C111.256 (5)C14—H14C0.9800
O7—C111.261 (5)C15—C161.517 (7)
O8—C131.267 (5)C16—H16A0.9800
O9—C131.259 (5)C16—H16B0.9800
O10—C151.251 (5)C16—H16C0.9800
O11—C151.261 (6)C17—C181.512 (6)
O12—C171.254 (5)C18—H18A0.9800
O13—C171.255 (5)C18—H18B0.9800
O14—C191.148 (6)C18—H18C0.9800
N1—C11.305 (6)O15—H150.8400
N1—C31.365 (7)O15—C211.42 (2)
N2—H20.8800C21—H21A0.9800
N2—C11.346 (7)C21—H21B0.9800
N2—C21.333 (8)C21—H21C0.9800
N3—C41.316 (5)O16—H160.8400
N3—C61.375 (5)O16—C221.380 (12)
N4—H40.8800C22—H22A0.9800
N4—C41.342 (6)C22—H22B0.9800
N4—C51.372 (6)C22—H22C0.9800
C1—H10.9500
O1—Ru1—O293.06 (12)C2—C3—H3125.1
O1—Ru1—O495.67 (11)N3—C4—N4110.8 (4)
O1—Ru1—O1192.12 (12)N3—C4—H4A124.6
O1—Ru1—O1397.86 (11)N4—C4—H4A124.6
O1—Ru1—N1177.80 (12)N4—C5—H5127.3
O2—Ru1—O488.87 (12)C6—C5—N4105.4 (4)
O2—Ru1—N187.81 (14)C6—C5—H5127.3
O4—Ru1—N182.33 (13)N3—C6—H6125.0
O11—Ru1—O2174.79 (12)C5—C6—N3110.0 (4)
O11—Ru1—O491.26 (12)C5—C6—H6125.0
O11—Ru1—O1388.40 (13)O2—C7—C8117.0 (4)
O11—Ru1—N187.04 (14)O3—C7—O2126.4 (4)
O13—Ru1—O290.26 (13)O3—C7—C8116.6 (4)
O13—Ru1—O4166.47 (12)C7—C8—H8A109.5
O13—Ru1—N184.15 (13)C7—C8—H8B109.5
O1—Ru2—O395.19 (12)C7—C8—H8C109.5
O1—Ru2—O593.27 (11)H8A—C8—H8B109.5
O1—Ru2—O695.97 (12)H8A—C8—H8C109.5
O1—Ru2—O894.23 (12)H8B—C8—H8C109.5
O1—Ru2—N3179.81 (13)O4—C9—O5124.8 (4)
O3—Ru2—N384.63 (13)O4—C9—C10117.9 (4)
O5—Ru2—O390.95 (12)O5—C9—C10117.2 (4)
O5—Ru2—O686.71 (12)C9—C10—H10A109.5
O5—Ru2—N386.71 (12)C9—C10—H10B109.5
O6—Ru2—O3168.72 (12)C9—C10—H10C109.5
O6—Ru2—N384.22 (13)H10A—C10—H10B109.5
O8—Ru2—O388.10 (13)H10A—C10—H10C109.5
O8—Ru2—O5172.50 (12)H10B—C10—H10C109.5
O8—Ru2—O692.78 (13)O6—C11—O7126.4 (4)
O8—Ru2—N385.80 (13)O6—C11—C12116.6 (4)
O1—Ru3—O790.81 (11)O7—C11—C12117.0 (4)
O1—Ru3—O991.64 (11)C11—C12—H12A109.5
O1—Ru3—O1091.65 (11)C11—C12—H12B109.5
O1—Ru3—O1291.35 (11)C11—C12—H12C109.5
O9—Ru3—O793.26 (12)H12A—C12—H12B109.5
O9—Ru3—O10176.71 (12)H12A—C12—H12C109.5
O10—Ru3—O786.76 (12)H12B—C12—H12C109.5
O12—Ru3—O7177.79 (12)O8—C13—C14116.3 (4)
O12—Ru3—O987.15 (12)O9—C13—O8126.4 (4)
O12—Ru3—O1092.71 (12)O9—C13—C14117.3 (4)
C19—Ru3—O1175.54 (16)C13—C14—H14A109.5
C19—Ru3—O792.95 (16)C13—C14—H14B109.5
C19—Ru3—O985.75 (16)C13—C14—H14C109.5
C19—Ru3—O1090.96 (16)H14A—C14—H14B109.5
C19—Ru3—O1284.91 (16)H14A—C14—H14C109.5
Ru1—O1—Ru3119.67 (14)H14B—C14—H14C109.5
Ru2—O1—Ru1119.92 (14)O10—C15—O11128.4 (4)
Ru2—O1—Ru3120.39 (14)O10—C15—C16116.1 (4)
C7—O2—Ru1124.0 (3)O11—C15—C16115.5 (4)
C7—O3—Ru2132.2 (3)C15—C16—H16A109.5
C9—O4—Ru1132.6 (3)C15—C16—H16B109.5
C9—O5—Ru2123.6 (3)C15—C16—H16C109.5
C11—O6—Ru2133.4 (3)H16A—C16—H16B109.5
C11—O7—Ru3129.7 (3)H16A—C16—H16C109.5
C13—O8—Ru2129.1 (3)H16B—C16—H16C109.5
C13—O9—Ru3134.8 (3)O12—C17—O13127.1 (4)
C15—O10—Ru3133.0 (3)O12—C17—C18116.5 (4)
C15—O11—Ru1127.2 (3)O13—C17—C18116.4 (4)
C17—O12—Ru3127.2 (3)C17—C18—H18A109.5
C17—O13—Ru1131.4 (3)C17—C18—H18B109.5
C1—N1—Ru1128.5 (4)C17—C18—H18C109.5
C1—N1—C3105.9 (4)H18A—C18—H18B109.5
C3—N1—Ru1125.5 (3)H18A—C18—H18C109.5
C1—N2—H2125.6H18B—C18—H18C109.5
C2—N2—H2125.6O14—C19—Ru3173.5 (4)
C2—N2—C1108.9 (5)C21—O15—H15109.5
C4—N3—Ru2125.0 (3)O15—C21—H21A109.5
C4—N3—C6105.8 (4)O15—C21—H21B109.5
C6—N3—Ru2129.2 (3)O15—C21—H21C109.5
C4—N4—H4126.0H21A—C21—H21B109.5
C4—N4—C5108.0 (4)H21A—C21—H21C109.5
C5—N4—H4126.0H21B—C21—H21C109.5
N1—C1—N2109.7 (5)C22—O16—H16109.5
N1—C1—H1125.2O16—C22—H22A109.5
N2—C1—H1125.2O16—C22—H22B109.5
N2—C2—H2A127.2O16—C22—H22C109.5
N2—C2—C3105.7 (5)H22A—C22—H22B109.5
C3—C2—H2A127.2H22A—C22—H22C109.5
N1—C3—H3125.1H22B—C22—H22C109.5
C2—C3—N1109.8 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O5i0.882.092.858 (5)146
N4—H4···O7ii0.881.932.766 (5)157
O15—H15···O160.841.912.719 (12)163
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x1, y, z.
Hexa-µ2-acetato-µ3-oxido-tris(4-phenylpyridine)triruthenium pentahydrate (ae218d) top
Crystal data top
[Ru3(C2H3O2)6O(C11H9N)3]·5H2OZ = 2
Mr = 1229.13F(000) = 1244
Triclinic, P1Dx = 1.572 Mg m3
a = 11.700 (4) ÅMo Kα radiation, λ = 0.71073 Å
b = 15.033 (5) ÅCell parameters from 5429 reflections
c = 16.180 (5) Åθ = 2.5–22.4°
α = 78.256 (4)°µ = 0.93 mm1
β = 71.422 (3)°T = 173 K
γ = 76.364 (3)°Plate, brown
V = 2596.0 (14) Å30.28 × 0.02 × 0.002 mm
Data collection top
Bruker APEXII CCD
diffractometer
10222 independent reflections
Radiation source: sealed tube5227 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.155
Detector resolution: 8.36 pixels mm-1θmax = 26.2°, θmin = 1.3°
ω scansh = 1414
Absorption correction: multi-scan
(SADABS; Bruker, 2015)
k = 1818
Tmin = 0.534, Tmax = 0.745l = 1920
43041 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.083H-atom parameters constrained
wR(F2) = 0.254 w = 1/[σ2(Fo2) + (0.1342P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
10222 reflectionsΔρmax = 2.45 e Å3
628 parametersΔρmin = 1.13 e Å3
0 restraints
Special details top

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 (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.51924 (8)0.71860 (6)0.59071 (6)0.0388 (3)
Ru20.36729 (7)0.63005 (6)0.78939 (6)0.0381 (3)
Ru30.27149 (8)0.84710 (6)0.70788 (6)0.0397 (3)
O10.3867 (6)0.7319 (4)0.6981 (4)0.0359 (16)
O20.6533 (6)0.6838 (5)0.6568 (5)0.0436 (18)
O30.5549 (6)0.5904 (5)0.7749 (5)0.0404 (17)
O40.5311 (6)0.5779 (5)0.5929 (4)0.0403 (17)
O50.3690 (7)0.5414 (5)0.7056 (5)0.0464 (18)
O60.3618 (6)0.7050 (5)0.8864 (5)0.0445 (18)
O70.2563 (7)0.8444 (5)0.8404 (5)0.0475 (18)
O80.1770 (7)0.6529 (5)0.8212 (5)0.0469 (19)
O90.1206 (6)0.7862 (5)0.7384 (5)0.0479 (19)
O100.4088 (7)0.9242 (5)0.6797 (5)0.0459 (18)
O110.5471 (6)0.8545 (5)0.5679 (5)0.0428 (17)
O120.2610 (7)0.8671 (5)0.5783 (5)0.0480 (19)
O130.3970 (6)0.7468 (5)0.5165 (4)0.0446 (18)
N10.6602 (8)0.7064 (6)0.4701 (5)0.039 (2)
N20.3478 (8)0.5096 (6)0.8843 (6)0.044 (2)
N30.1417 (8)0.9715 (6)0.7188 (6)0.047 (2)
C10.7576 (10)0.6368 (8)0.4554 (7)0.046 (3)
H10.76920.59190.50400.055*
C20.8406 (10)0.6269 (8)0.3752 (8)0.052 (3)
H20.90750.57630.36950.063*
C30.8279 (8)0.6912 (7)0.3004 (7)0.039 (3)
C40.7273 (10)0.7623 (8)0.3145 (7)0.047 (3)
H40.71150.80590.26620.057*
C50.6482 (10)0.7705 (8)0.3999 (8)0.052 (3)
H50.58410.82290.40850.063*
C60.9108 (10)0.6812 (9)0.2103 (8)0.051 (3)
C70.9755 (11)0.5935 (9)0.1879 (8)0.054 (3)
H70.96610.54040.23100.064*
C81.0519 (11)0.5839 (10)0.1046 (8)0.059 (3)
H81.09340.52410.09060.071*
C91.0693 (12)0.6592 (12)0.0415 (9)0.071 (4)
H91.12420.65170.01530.085*
C101.0072 (12)0.7460 (10)0.0602 (8)0.064 (4)
H101.01840.79820.01610.077*
C110.9272 (11)0.7575 (9)0.1447 (8)0.060 (3)
H110.88400.81740.15730.072*
C120.4264 (10)0.4731 (8)0.9323 (7)0.048 (3)
H120.48570.50780.93020.057*
C130.4269 (10)0.3880 (8)0.9850 (8)0.049 (3)
H130.48360.36751.01890.059*
C140.3453 (10)0.3322 (8)0.9888 (7)0.046 (3)
C150.2611 (10)0.3705 (8)0.9394 (8)0.050 (3)
H150.20090.33680.94120.060*
C160.2646 (10)0.4556 (8)0.8889 (7)0.049 (3)
H160.20730.47850.85570.059*
C170.3482 (10)0.2380 (7)1.0414 (8)0.047 (3)
C180.3201 (14)0.1675 (9)1.0110 (11)0.077 (4)
H180.29660.18020.95810.093*
C190.326 (2)0.0794 (11)1.0576 (15)0.140 (9)
H190.31030.03061.03620.168*
C200.358 (2)0.0632 (13)1.1384 (17)0.156 (11)
H200.35930.00351.17210.188*
C210.3846 (15)0.1304 (10)1.1676 (11)0.096 (6)
H210.40680.11841.22090.115*
C220.3799 (12)0.2172 (10)1.1195 (9)0.066 (4)
H220.39900.26471.14070.080*
C230.1461 (10)1.0449 (7)0.6510 (8)0.050 (3)
H230.21581.04350.60070.060*
C240.0504 (10)1.1209 (8)0.6551 (8)0.051 (3)
H240.05401.16870.60630.061*
C250.0512 (10)1.1280 (8)0.7300 (8)0.048 (3)
C260.0488 (11)1.0559 (9)0.7972 (9)0.059 (3)
H260.11471.05890.84980.070*
C270.0428 (10)0.9804 (8)0.7926 (8)0.049 (3)
H270.03830.93270.84150.059*
C280.1536 (11)1.2082 (8)0.7346 (8)0.054 (3)
C290.1417 (13)1.2919 (9)0.6853 (10)0.067 (4)
H290.06371.29820.64510.080*
C300.2349 (15)1.3686 (11)0.6892 (13)0.095 (5)
H300.22111.42620.65440.114*
C310.3525 (17)1.3575 (12)0.7476 (12)0.091 (5)
H310.41901.40850.75170.109*
C320.3713 (13)1.2727 (13)0.7990 (10)0.090 (5)
H320.44961.26620.83860.108*
C330.2733 (13)1.1969 (10)0.7917 (9)0.071 (4)
H330.28631.13820.82450.085*
C340.6488 (10)0.6221 (8)0.7255 (8)0.044 (3)
C350.7681 (11)0.5877 (9)0.7504 (9)0.066 (4)
H35A0.83150.56010.70160.099*
H35B0.75540.54110.80290.099*
H35C0.79440.63960.76270.099*
C360.4566 (11)0.5238 (7)0.6371 (7)0.044 (3)
C370.4713 (11)0.4344 (7)0.6075 (7)0.051 (3)
H37A0.43930.44400.55670.076*
H37B0.42610.39330.65550.076*
H37C0.55850.40620.59070.076*
C380.3054 (9)0.7872 (8)0.8945 (7)0.044 (3)
C390.2988 (12)0.8201 (8)0.9784 (8)0.058 (3)
H39A0.29110.76851.02670.087*
H39B0.22740.86970.99250.087*
H39C0.37370.84340.97050.087*
C400.1004 (10)0.7131 (9)0.7899 (8)0.048 (3)
C410.0304 (11)0.6948 (10)0.8191 (11)0.080 (4)
H41A0.08720.74820.84410.119*
H41B0.03650.63990.86360.119*
H41C0.05140.68460.76820.119*
C420.5070 (10)0.9162 (7)0.6177 (7)0.040 (2)
C430.5857 (11)0.9889 (8)0.6024 (8)0.052 (3)
H43A0.58341.02950.54710.079*
H43B0.67050.95830.59920.079*
H43C0.55391.02560.65120.079*
C440.3064 (10)0.8120 (8)0.5209 (8)0.048 (3)
C450.2407 (11)0.8278 (8)0.4492 (8)0.057 (3)
H45A0.15920.81130.47540.085*
H45B0.28870.78910.40330.085*
H45C0.23210.89300.42320.085*
O170.0382 (6)0.9449 (5)0.5641 (4)0.167 (16)0.5
O160.0212 (6)0.5798 (5)0.5311 (4)0.140 (5)
H16A0.00470.54460.58030.210*
H16B0.07440.54630.49290.210*
O140.8753 (6)0.7597 (5)0.5557 (4)0.113 (4)
H14A0.83620.80190.58950.170*
H14B0.94790.74480.56350.170*
O150.2106 (6)0.6072 (5)0.5875 (4)0.149 (14)0.5
H15A0.17950.61500.54380.224*0.5
H15B0.26650.64160.56920.224*0.5
O180.3175 (6)1.0352 (5)0.8261 (4)0.208 (8)
H18A0.31640.99170.87080.311*
H18B0.25751.07900.84630.311*
O17A0.0478 (6)0.8844 (5)0.6228 (4)0.127 (11)0.5
H17C0.01250.82690.61960.190*0.5
H17D0.08480.88610.67860.190*0.5
O15A0.1481 (6)0.6046 (5)0.6360 (4)0.24 (3)0.5
H17A0.01310.98880.57730.366*0.5
H17B0.02420.89950.55840.366*0.5
H15C0.12910.55390.66930.366*0.5
H15D0.14100.64590.66880.366*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0379 (5)0.0391 (5)0.0462 (5)0.0119 (4)0.0126 (4)0.0141 (4)
Ru20.0362 (5)0.0385 (5)0.0465 (5)0.0113 (4)0.0144 (4)0.0122 (4)
Ru30.0366 (5)0.0392 (5)0.0486 (6)0.0084 (4)0.0144 (4)0.0131 (4)
O10.037 (4)0.042 (4)0.037 (4)0.013 (3)0.012 (3)0.015 (3)
O20.038 (4)0.047 (4)0.054 (5)0.015 (3)0.015 (4)0.014 (4)
O30.041 (4)0.041 (4)0.047 (4)0.013 (3)0.016 (3)0.011 (3)
O40.043 (4)0.039 (4)0.048 (4)0.012 (3)0.018 (3)0.014 (3)
O50.051 (5)0.049 (5)0.046 (5)0.017 (4)0.011 (4)0.016 (4)
O60.045 (4)0.049 (5)0.047 (4)0.012 (4)0.017 (4)0.014 (4)
O70.048 (4)0.041 (4)0.056 (5)0.005 (4)0.018 (4)0.010 (4)
O80.041 (4)0.049 (5)0.058 (5)0.017 (4)0.014 (4)0.013 (4)
O90.044 (4)0.042 (4)0.068 (5)0.015 (4)0.023 (4)0.010 (4)
O100.045 (4)0.040 (4)0.060 (5)0.015 (3)0.012 (4)0.017 (4)
O110.040 (4)0.044 (4)0.049 (4)0.013 (3)0.010 (3)0.012 (4)
O120.047 (4)0.042 (4)0.064 (5)0.002 (4)0.024 (4)0.018 (4)
O130.043 (4)0.056 (5)0.045 (4)0.014 (4)0.014 (3)0.020 (4)
N10.051 (6)0.035 (5)0.039 (5)0.016 (4)0.012 (4)0.014 (4)
N20.036 (5)0.054 (6)0.046 (5)0.009 (4)0.013 (4)0.011 (4)
N30.043 (5)0.042 (5)0.062 (6)0.006 (4)0.016 (5)0.016 (5)
C10.037 (6)0.060 (8)0.045 (7)0.006 (6)0.015 (5)0.015 (6)
C20.039 (6)0.059 (8)0.067 (8)0.015 (6)0.020 (6)0.012 (6)
C30.021 (5)0.047 (6)0.057 (7)0.014 (5)0.013 (5)0.010 (5)
C40.046 (7)0.060 (7)0.045 (7)0.031 (6)0.010 (5)0.007 (6)
C50.048 (7)0.055 (8)0.056 (8)0.006 (6)0.005 (6)0.030 (6)
C60.035 (6)0.075 (9)0.056 (8)0.023 (6)0.016 (5)0.019 (7)
C70.056 (7)0.060 (8)0.055 (8)0.022 (6)0.020 (6)0.012 (6)
C80.051 (7)0.076 (9)0.050 (8)0.018 (7)0.006 (6)0.016 (7)
C90.051 (8)0.109 (12)0.063 (9)0.029 (8)0.012 (7)0.026 (9)
C100.064 (8)0.082 (10)0.048 (8)0.030 (8)0.006 (7)0.007 (7)
C110.058 (8)0.071 (9)0.063 (9)0.032 (7)0.014 (7)0.019 (7)
C120.049 (7)0.054 (7)0.049 (7)0.025 (6)0.014 (6)0.007 (6)
C130.055 (7)0.046 (7)0.058 (7)0.017 (6)0.027 (6)0.010 (6)
C140.040 (6)0.060 (7)0.046 (7)0.018 (5)0.011 (5)0.015 (6)
C150.045 (7)0.053 (7)0.059 (8)0.020 (6)0.019 (6)0.006 (6)
C160.049 (7)0.055 (7)0.053 (7)0.023 (6)0.021 (6)0.002 (6)
C170.046 (7)0.043 (7)0.058 (8)0.025 (5)0.016 (6)0.001 (6)
C180.096 (11)0.053 (8)0.110 (12)0.030 (8)0.061 (10)0.001 (8)
C190.22 (2)0.059 (11)0.20 (2)0.075 (13)0.13 (2)0.033 (12)
C200.24 (3)0.082 (14)0.21 (2)0.079 (16)0.16 (2)0.061 (15)
C210.126 (14)0.070 (10)0.119 (14)0.058 (10)0.080 (12)0.044 (10)
C220.067 (9)0.080 (10)0.063 (9)0.038 (7)0.024 (7)0.003 (7)
C230.048 (7)0.038 (6)0.080 (9)0.000 (5)0.040 (6)0.020 (6)
C240.051 (7)0.049 (7)0.057 (8)0.015 (6)0.020 (6)0.005 (6)
C250.045 (7)0.042 (7)0.068 (8)0.004 (5)0.026 (6)0.023 (6)
C260.050 (7)0.066 (9)0.072 (9)0.009 (7)0.024 (6)0.028 (7)
C270.047 (7)0.042 (7)0.063 (8)0.001 (6)0.030 (6)0.000 (6)
C280.061 (8)0.044 (7)0.065 (8)0.014 (6)0.035 (7)0.025 (6)
C290.076 (9)0.048 (8)0.093 (10)0.003 (7)0.048 (8)0.021 (7)
C300.077 (11)0.064 (10)0.151 (16)0.022 (9)0.048 (12)0.047 (10)
C310.106 (14)0.090 (12)0.090 (12)0.033 (10)0.067 (11)0.039 (10)
C320.057 (9)0.143 (16)0.057 (9)0.032 (10)0.024 (7)0.032 (10)
C330.076 (10)0.072 (9)0.065 (9)0.015 (8)0.029 (8)0.031 (7)
C340.037 (6)0.051 (7)0.052 (7)0.008 (5)0.014 (5)0.021 (6)
C350.055 (8)0.074 (9)0.083 (10)0.014 (7)0.040 (7)0.004 (7)
C360.060 (7)0.031 (6)0.049 (7)0.014 (5)0.019 (6)0.015 (5)
C370.062 (7)0.044 (7)0.049 (7)0.009 (6)0.017 (6)0.013 (5)
C380.034 (6)0.046 (7)0.055 (7)0.014 (5)0.009 (5)0.011 (6)
C390.068 (8)0.058 (8)0.059 (8)0.016 (6)0.019 (6)0.027 (6)
C400.038 (6)0.049 (7)0.062 (8)0.002 (6)0.017 (6)0.020 (6)
C410.044 (7)0.073 (9)0.125 (13)0.029 (7)0.022 (8)0.005 (9)
C420.038 (6)0.039 (6)0.049 (7)0.010 (5)0.018 (5)0.009 (5)
C430.057 (7)0.048 (7)0.068 (8)0.019 (6)0.028 (6)0.017 (6)
C440.043 (7)0.041 (7)0.065 (8)0.011 (6)0.015 (6)0.015 (6)
C450.063 (8)0.063 (8)0.059 (8)0.011 (6)0.033 (6)0.017 (6)
O170.073 (18)0.18 (3)0.28 (4)0.016 (18)0.05 (2)0.15 (3)
O160.139 (11)0.148 (12)0.157 (13)0.033 (9)0.084 (10)0.002 (10)
O140.072 (7)0.152 (11)0.110 (9)0.044 (7)0.018 (6)0.009 (8)
O150.21 (3)0.09 (2)0.22 (3)0.06 (2)0.17 (3)0.012 (19)
O180.29 (2)0.112 (12)0.24 (2)0.010 (14)0.116 (18)0.040 (12)
O17A0.101 (19)0.14 (3)0.17 (3)0.021 (17)0.064 (19)0.06 (2)
O15A0.39 (7)0.10 (3)0.22 (4)0.05 (3)0.02 (4)0.08 (3)
Geometric parameters (Å, º) top
Ru1—O11.934 (6)C18—H180.9500
Ru1—O22.082 (7)C18—C191.38 (2)
Ru1—O42.080 (7)C19—H190.9500
Ru1—O112.084 (7)C19—C201.43 (3)
Ru1—O132.066 (7)C20—H200.9500
Ru1—N12.124 (8)C20—C211.34 (2)
Ru2—O11.899 (6)C21—H210.9500
Ru2—O32.083 (7)C21—C221.375 (17)
Ru2—O52.078 (7)C22—H220.9500
Ru2—O62.087 (7)C23—H230.9500
Ru2—O82.079 (7)C23—C241.394 (15)
Ru2—N22.128 (9)C24—H240.9500
Ru3—O11.928 (6)C24—C251.403 (16)
Ru3—O72.088 (8)C25—C261.371 (16)
Ru3—O92.055 (7)C25—C281.481 (15)
Ru3—O102.080 (7)C26—H260.9500
Ru3—O122.096 (8)C26—C271.361 (16)
Ru3—N32.111 (9)C27—H270.9500
O2—C341.289 (13)C28—C291.357 (17)
O3—C341.267 (12)C28—C331.439 (18)
O4—C361.279 (12)C29—H290.9500
O5—C361.272 (13)C29—C301.385 (18)
O6—C381.268 (12)C30—H300.9500
O7—C381.271 (12)C30—C311.42 (2)
O8—C401.265 (13)C31—H310.9500
O9—C401.258 (13)C31—C321.40 (2)
O10—C421.261 (12)C32—H320.9500
O11—C421.262 (12)C32—C331.407 (18)
O12—C441.273 (13)C33—H330.9500
O13—C441.257 (13)C34—C351.521 (15)
N1—C11.348 (13)C35—H35A0.9800
N1—C51.353 (14)C35—H35B0.9800
N2—C121.340 (13)C35—H35C0.9800
N2—C161.384 (13)C36—C371.472 (14)
N3—C231.387 (14)C37—H37A0.9800
N3—C271.377 (14)C37—H37B0.9800
C1—H10.9500C37—H37C0.9800
C1—C21.363 (15)C38—C391.511 (15)
C2—H20.9500C39—H39A0.9800
C2—C31.411 (15)C39—H39B0.9800
C3—C41.384 (15)C39—H39C0.9800
C3—C61.487 (15)C40—C411.525 (15)
C4—H40.9500C41—H41A0.9800
C4—C51.407 (15)C41—H41B0.9800
C5—H50.9500C41—H41C0.9800
C6—C71.411 (16)C42—C431.524 (14)
C6—C111.398 (16)C43—H43A0.9800
C7—H70.9500C43—H43B0.9800
C7—C81.373 (16)C43—H43C0.9800
C8—H80.9500C44—C451.539 (15)
C8—C91.367 (18)C45—H45A0.9800
C9—H90.9500C45—H45B0.9800
C9—C101.376 (19)C45—H45C0.9800
C10—H100.9500O17—H17A0.8699
C10—C111.407 (17)O17—H17B0.8700
C11—H110.9500O16—H16A0.8695
C12—H120.9500O16—H16B0.8700
C12—C131.385 (15)O14—H14A0.8699
C13—H130.9500O14—H14B0.8693
C13—C141.391 (14)O15—H15A0.8700
C14—C151.410 (15)O15—H15B0.8700
C14—C171.496 (15)O18—H18A0.8698
C15—H150.9500O18—H18B0.8698
C15—C161.373 (15)O17A—H17C0.8701
C16—H160.9500O17A—H17D0.8700
C17—C181.396 (16)O15A—H15C0.8700
C17—C221.385 (16)O15A—H15D0.8698
O1—Ru1—O293.1 (3)C15—C16—N2122.9 (10)
O1—Ru1—O496.9 (3)C15—C16—H16118.6
O1—Ru1—O1195.7 (3)C18—C17—C14119.8 (11)
O1—Ru1—O1391.5 (3)C22—C17—C14122.0 (10)
O1—Ru1—N1177.9 (3)C22—C17—C18118.2 (11)
O2—Ru1—O1187.7 (3)C17—C18—H18119.9
O2—Ru1—N189.0 (3)C19—C18—C17120.3 (14)
O4—Ru1—O287.9 (3)C19—C18—H18119.9
O4—Ru1—O11166.8 (3)C18—C19—H19120.7
O4—Ru1—N183.6 (3)C18—C19—C20118.6 (16)
O11—Ru1—N183.9 (3)C20—C19—H19120.7
O13—Ru1—O2175.0 (3)C19—C20—H20119.4
O13—Ru1—O489.4 (3)C21—C20—C19121.2 (16)
O13—Ru1—O1194.0 (3)C21—C20—H20119.4
O13—Ru1—N186.5 (3)C20—C21—H21120.4
O1—Ru2—O393.6 (3)C20—C21—C22119.2 (16)
O1—Ru2—O593.3 (3)C22—C21—H21120.4
O1—Ru2—O694.0 (3)C17—C22—H22118.8
O1—Ru2—O895.6 (3)C21—C22—C17122.5 (13)
O1—Ru2—N2175.7 (3)C21—C22—H22118.8
O3—Ru2—O686.5 (3)N3—C23—H23119.3
O3—Ru2—N286.1 (3)N3—C23—C24121.3 (11)
O5—Ru2—O393.4 (3)C24—C23—H23119.3
O5—Ru2—O6172.7 (3)C23—C24—H24119.5
O5—Ru2—O886.9 (3)C23—C24—C25121.1 (11)
O5—Ru2—N282.5 (3)C25—C24—H24119.5
O6—Ru2—N290.2 (3)C24—C25—C28121.4 (11)
O8—Ru2—O3170.7 (3)C26—C25—C24115.5 (11)
O8—Ru2—O692.1 (3)C26—C25—C28123.1 (12)
O8—Ru2—N284.8 (3)C25—C26—H26118.2
O1—Ru3—O793.9 (3)C27—C26—C25123.7 (12)
O1—Ru3—O994.1 (3)C27—C26—H26118.2
O1—Ru3—O1093.0 (3)N3—C27—H27119.2
O1—Ru3—O1295.3 (3)C26—C27—N3121.5 (11)
O1—Ru3—N3178.5 (3)C26—C27—H27119.2
O7—Ru3—O12170.5 (3)C29—C28—C25123.4 (12)
O7—Ru3—N386.4 (3)C29—C28—C33117.7 (12)
O9—Ru3—O792.3 (3)C33—C28—C25118.9 (11)
O9—Ru3—O10172.8 (3)C28—C29—H29117.6
O9—Ru3—O1284.8 (3)C28—C29—C30124.8 (16)
O9—Ru3—N384.4 (3)C30—C29—H29117.6
O10—Ru3—O786.6 (3)C29—C30—H30121.4
O10—Ru3—O1295.1 (3)C29—C30—C31117.2 (17)
O10—Ru3—N388.4 (3)C31—C30—H30121.4
O12—Ru3—N384.3 (3)C30—C31—H31119.6
Ru2—O1—Ru1119.8 (3)C32—C31—C30120.8 (14)
Ru2—O1—Ru3121.1 (3)C32—C31—H31119.6
Ru3—O1—Ru1119.0 (3)C31—C32—H32120.2
C34—O2—Ru1123.3 (6)C31—C32—C33119.5 (15)
C34—O3—Ru2134.2 (7)C33—C32—H32120.2
C36—O4—Ru1130.9 (7)C28—C33—H33120.0
C36—O5—Ru2124.0 (6)C32—C33—C28119.9 (14)
C38—O6—Ru2125.6 (7)C32—C33—H33120.0
C38—O7—Ru3132.7 (7)O2—C34—C35115.7 (10)
C40—O8—Ru2132.3 (7)O3—C34—O2126.5 (10)
C40—O9—Ru3127.4 (7)O3—C34—C35117.8 (11)
C42—O10—Ru3125.7 (7)C34—C35—H35A109.5
C42—O11—Ru1130.2 (7)C34—C35—H35B109.5
C44—O12—Ru3128.8 (7)C34—C35—H35C109.5
C44—O13—Ru1126.6 (7)H35A—C35—H35B109.5
C1—N1—Ru1125.7 (7)H35A—C35—H35C109.5
C1—N1—C5116.3 (9)H35B—C35—H35C109.5
C5—N1—Ru1117.8 (7)O4—C36—C37118.6 (10)
C12—N2—Ru2122.9 (7)O5—C36—O4124.7 (9)
C12—N2—C16115.5 (9)O5—C36—C37116.7 (10)
C16—N2—Ru2120.7 (7)C36—C37—H37A109.5
C23—N3—Ru3122.6 (8)C36—C37—H37B109.5
C27—N3—Ru3120.5 (7)C36—C37—H37C109.5
C27—N3—C23116.8 (9)H37A—C37—H37B109.5
N1—C1—H1117.9H37A—C37—H37C109.5
N1—C1—C2124.2 (11)H37B—C37—H37C109.5
C2—C1—H1117.9O6—C38—O7127.9 (10)
C1—C2—H2119.7O6—C38—C39114.9 (10)
C1—C2—C3120.5 (11)O7—C38—C39117.2 (10)
C3—C2—H2119.7C38—C39—H39A109.5
C2—C3—C6123.2 (10)C38—C39—H39B109.5
C4—C3—C2115.8 (10)C38—C39—H39C109.5
C4—C3—C6120.9 (10)H39A—C39—H39B109.5
C3—C4—H4119.7H39A—C39—H39C109.5
C3—C4—C5120.6 (11)H39B—C39—H39C109.5
C5—C4—H4119.7O8—C40—C41115.9 (11)
N1—C5—C4122.4 (11)O9—C40—O8127.0 (10)
N1—C5—H5118.8O9—C40—C41117.1 (10)
C4—C5—H5118.8C40—C41—H41A109.5
C7—C6—C3120.7 (11)C40—C41—H41B109.5
C11—C6—C3121.7 (11)C40—C41—H41C109.5
C11—C6—C7117.6 (11)H41A—C41—H41B109.5
C6—C7—H7119.6H41A—C41—H41C109.5
C8—C7—C6120.9 (12)H41B—C41—H41C109.5
C8—C7—H7119.6O10—C42—O11127.0 (9)
C7—C8—H8119.5O10—C42—C43116.1 (10)
C9—C8—C7121.0 (13)O11—C42—C43116.9 (10)
C9—C8—H8119.5C42—C43—H43A109.5
C8—C9—H9119.9C42—C43—H43B109.5
C8—C9—C10120.1 (13)C42—C43—H43C109.5
C10—C9—H9119.9H43A—C43—H43B109.5
C9—C10—H10120.0H43A—C43—H43C109.5
C9—C10—C11120.0 (13)H43B—C43—H43C109.5
C11—C10—H10120.0O12—C44—C45115.2 (10)
C6—C11—C10120.4 (13)O13—C44—O12127.9 (11)
C6—C11—H11119.8O13—C44—C45116.9 (10)
C10—C11—H11119.8C44—C45—H45A109.5
N2—C12—H12117.9C44—C45—H45B109.5
N2—C12—C13124.3 (10)C44—C45—H45C109.5
C13—C12—H12117.9H45A—C45—H45B109.5
C12—C13—H13119.6H45A—C45—H45C109.5
C12—C13—C14120.8 (10)H45B—C45—H45C109.5
C14—C13—H13119.6H17A—O17—H17B104.5
C13—C14—C15115.4 (10)H16A—O16—H16B109.6
C13—C14—C17121.9 (10)H14A—O14—H14B104.5
C15—C14—C17122.7 (10)H15A—O15—H15B104.5
C14—C15—H15119.4H18A—O18—H18B104.5
C16—C15—C14121.1 (10)H17C—O17A—H17D104.5
C16—C15—H15119.4H15C—O15A—H15D109.5
N2—C16—H16118.6
Hexa-µ2-acetato-µ3-oxido-tris(1H-imidazole)triruthenium hexafluorophosphate acetonitrile hemisolvate (ae418a) top
Crystal data top
[Ru3(C2H3O2)6O(C3H4N2)3]PF6·0.5C2H3NMo Kα radiation, λ = 0.71073 Å
Mr = 1043.23Cell parameters from 9943 reflections
Cubic, Pa3θ = 2.4–25.3°
a = 19.2946 (13) ŵ = 1.39 mm1
V = 7183.0 (15) Å3T = 173 K
Z = 8.0Plate, black
F(000) = 41120.34 × 0.20 × 0.03 mm
Dx = 1.929 Mg m3
Data collection top
Bruker APEXII CCD
diffractometer
2203 independent reflections
Radiation source: sealed tube1841 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.093
Detector resolution: 8.36 pixels mm-1θmax = 25.4°, θmin = 1.8°
ω scansh = 2323
Absorption correction: multi-scan
(TWINABS; Bruker, 2012)
k = 2323
Tmin = 0.655, Tmax = 0.745l = 2323
110680 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.111 w = 1/[σ2(Fo2) + (0.0602P)2 + 16.5814P]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max = 0.001
2203 reflectionsΔρmax = 1.70 e Å3
180 parametersΔρmin = 0.44 e Å3
0 restraints
Special details top

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 (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.67622 (2)0.46270 (2)0.91302 (2)0.02005 (17)
P1B0.7438 (3)0.7438 (3)0.7438 (3)0.045 (2)0.5
O10.60126 (15)0.39874 (15)0.89874 (15)0.0181 (10)
O20.74925 (16)0.38654 (16)0.91384 (15)0.0251 (7)
O30.69122 (16)0.30476 (16)0.97439 (16)0.0272 (7)
O50.53899 (15)0.51922 (15)0.82687 (15)0.0217 (7)
O40.61256 (16)0.54609 (15)0.91362 (16)0.0248 (7)
N10.75597 (19)0.53466 (18)0.9283 (2)0.0236 (8)
N20.8190 (2)0.6284 (2)0.9196 (2)0.0340 (10)
H20.83550.66780.90360.041*
C60.5676 (2)0.5613 (2)0.8690 (2)0.0226 (9)
C10.7675 (2)0.5911 (2)0.8914 (3)0.0301 (11)
H10.74280.60350.85060.036*
C70.5477 (2)0.6360 (2)0.8643 (2)0.0284 (10)
H7A0.57830.65960.83140.043*
H7B0.55210.65760.91000.043*
H7C0.49960.63970.84840.043*
C40.7451 (2)0.3294 (2)0.9466 (2)0.0274 (10)
C30.8015 (3)0.5366 (3)0.9830 (3)0.0315 (11)
H30.80450.50311.01890.038*
C20.8412 (3)0.5942 (3)0.9774 (3)0.0376 (12)
H2A0.87750.60801.00770.045*
C50.8106 (3)0.2887 (3)0.9543 (3)0.0455 (14)
H5A0.80560.24390.93090.068*
H5B0.82010.28101.00360.068*
H5C0.84910.31440.93350.068*
F40.7663 (6)0.7289 (6)0.8223 (5)0.081 (3)0.5
F30.7551 (16)0.7937 (11)0.7022 (11)0.081 (3)0.25
F10.6850 (6)0.6653 (10)0.7526 (8)0.135 (6)0.5
N30.9500 (14)0.4500 (14)1.0500 (14)0.105 (12)0.5
C90.9132 (16)0.4132 (16)1.0868 (16)0.095 (12)0.5
C80.8774 (15)0.3774 (15)1.1226 (15)0.138 (16)0.5
H8A0.89600.37651.17000.208*0.1667
H8B0.87670.33001.10420.208*0.1667
H8C0.83020.39581.12350.208*0.1667
P10.7265 (6)0.7265 (6)0.7265 (6)0.099 (6)0.5
F50.7899 (15)0.7113 (13)0.7942 (13)0.081 (3)0.25
F20.7277 (7)0.7606 (8)0.6657 (6)0.104 (4)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0192 (2)0.0191 (2)0.0218 (2)0.00133 (13)0.00203 (13)0.00176 (13)
P1B0.045 (2)0.045 (2)0.045 (2)0.013 (2)0.013 (2)0.013 (2)
O10.0181 (10)0.0181 (10)0.0181 (10)0.0019 (12)0.0019 (12)0.0019 (12)
O20.0231 (16)0.0240 (16)0.0283 (17)0.0016 (13)0.0001 (13)0.0045 (13)
O30.0232 (16)0.0270 (17)0.0313 (17)0.0017 (13)0.0048 (14)0.0061 (14)
O50.0242 (16)0.0201 (15)0.0209 (15)0.0000 (12)0.0042 (12)0.0031 (12)
O40.0252 (17)0.0225 (16)0.0268 (17)0.0020 (13)0.0040 (13)0.0003 (13)
N10.0193 (19)0.0231 (19)0.028 (2)0.0042 (15)0.0026 (16)0.0019 (16)
N20.032 (2)0.019 (2)0.050 (3)0.0082 (17)0.0065 (19)0.0032 (18)
C60.020 (2)0.029 (2)0.019 (2)0.0021 (18)0.0025 (18)0.0083 (18)
C10.027 (2)0.024 (2)0.039 (3)0.0027 (19)0.001 (2)0.003 (2)
C70.028 (2)0.030 (2)0.028 (2)0.002 (2)0.002 (2)0.006 (2)
C40.030 (3)0.023 (2)0.029 (2)0.002 (2)0.000 (2)0.0011 (19)
C30.030 (3)0.039 (3)0.026 (2)0.007 (2)0.000 (2)0.002 (2)
C20.036 (3)0.044 (3)0.033 (3)0.013 (2)0.002 (2)0.005 (2)
C50.028 (3)0.043 (3)0.066 (4)0.008 (2)0.007 (3)0.020 (3)
F40.105 (8)0.078 (6)0.061 (6)0.003 (5)0.005 (5)0.018 (5)
F30.105 (8)0.078 (6)0.061 (6)0.003 (5)0.005 (5)0.018 (5)
F10.066 (7)0.201 (16)0.139 (10)0.014 (8)0.009 (6)0.125 (11)
N30.105 (12)0.105 (12)0.105 (12)0.063 (15)0.063 (15)0.063 (15)
C90.095 (12)0.095 (12)0.095 (12)0.022 (14)0.022 (14)0.022 (14)
C80.138 (16)0.138 (16)0.138 (16)0.01 (2)0.01 (2)0.01 (2)
P10.099 (6)0.099 (6)0.099 (6)0.059 (7)0.059 (7)0.059 (7)
F50.105 (8)0.078 (6)0.061 (6)0.003 (5)0.005 (5)0.018 (5)
F20.093 (8)0.162 (13)0.056 (6)0.009 (8)0.023 (6)0.044 (7)
Geometric parameters (Å, º) top
Ru1—O11.9211 (4)C7—H7C0.9800
Ru1—O22.036 (3)C4—C51.495 (7)
Ru1—O3i2.057 (3)C3—H30.9500
Ru1—O5ii2.050 (3)C3—C21.354 (7)
Ru1—O42.024 (3)C2—H2A0.9500
Ru1—N12.093 (4)C5—H5A0.9800
P1B—F5iii1.46 (2)C5—H5B0.9800
P1B—F5iv1.46 (2)C5—H5C0.9800
P1B—F51.46 (2)F4—F3iii1.49 (3)
P1B—F2iii1.571 (11)F4—F3iv1.44 (2)
P1B—F21.571 (11)F4—P12.002 (18)
P1B—F2iv1.571 (11)F3—F4iii1.44 (2)
O1—Ru1i1.9212 (4)F3—F4iv1.49 (3)
O1—Ru1ii1.9212 (4)F3—P11.48 (2)
O2—C41.273 (5)F1—P11.513 (16)
O3—Ru1ii2.057 (3)N3—C91.23 (5)
O3—C41.263 (6)C9—C81.20 (5)
O5—Ru1i2.050 (3)C8—H8A0.9838
O5—C61.274 (5)C8—H8B0.9822
O4—C61.257 (5)C8—H8C0.9787
N1—C11.320 (6)P1—F4iii2.002 (18)
N1—C31.373 (6)P1—F4iv2.002 (18)
N2—H20.8800P1—F3iv1.48 (2)
N2—C11.342 (6)P1—F3iii1.48 (2)
N2—C21.365 (7)P1—F1iv1.513 (16)
C6—C71.494 (6)P1—F1iii1.513 (16)
C1—H10.9500F5—F2iii1.66 (3)
C7—H7A0.9800F2—F5iv1.66 (3)
C7—H7B0.9800
O1—Ru1—O293.35 (15)N2—C2—H2A126.8
O1—Ru1—O3i93.70 (13)C3—C2—N2106.4 (4)
O1—Ru1—O5ii96.39 (12)C3—C2—H2A126.8
O1—Ru1—O493.13 (15)C4—C5—H5A109.5
O1—Ru1—N1178.42 (14)C4—C5—H5B109.5
O2—Ru1—O3i87.89 (12)C4—C5—H5C109.5
O2—Ru1—O5ii90.05 (12)H5A—C5—H5B109.5
O2—Ru1—N188.22 (14)H5A—C5—H5C109.5
O3i—Ru1—N186.18 (14)H5B—C5—H5C109.5
O5ii—Ru1—O3i169.81 (12)F3iv—F4—F3iii95.2 (18)
O5ii—Ru1—N183.78 (13)F3iv—F4—P147.7 (9)
O4—Ru1—O2173.52 (13)F3iii—F4—P147.6 (9)
O4—Ru1—O3i91.53 (12)F4iii—F3—F4iv98.3 (16)
O4—Ru1—O5ii89.39 (12)F4iii—F3—P186.2 (13)
O4—Ru1—N185.30 (14)P1—F3—F4iv84.5 (12)
F5—P1B—F5iv98.1 (14)C8—C9—N3180 (4)
F5—P1B—F5iii98.1 (14)C9—C8—H8A109.7
F5iii—P1B—F5iv98.1 (14)C9—C8—H8B109.7
F5iii—P1B—F2111.2 (13)C9—C8—H8C109.8
F5—P1B—F2iv111.2 (13)H8A—C8—H8B109.0
F5iv—P1B—F2iv148.0 (13)H8A—C8—H8C109.3
F5iv—P1B—F2iii111.2 (13)H8B—C8—H8C109.4
F5—P1B—F2148.0 (13)F4iii—P1—F467.4 (8)
F5iv—P1B—F266.1 (11)F4iv—P1—F467.4 (8)
F5iii—P1B—F2iv66.1 (11)F4iii—P1—F4iv67.4 (8)
F5iii—P1B—F2iii148.0 (13)F3—P1—F497.4 (15)
F5—P1B—F2iii66.1 (11)F3iii—P1—F447.9 (11)
F2iv—P1B—F292.9 (9)F3—P1—F4iv47.9 (11)
F2iii—P1B—F2iv92.9 (9)F3iii—P1—F4iv46.1 (10)
F2iii—P1B—F292.9 (9)F3iii—P1—F4iii97.4 (15)
Ru1—O1—Ru1i119.965 (9)F3iv—P1—F446.1 (10)
Ru1—O1—Ru1ii119.964 (9)F3iv—P1—F4iv97.4 (15)
Ru1i—O1—Ru1ii119.964 (9)F3—P1—F4iii46.1 (10)
C4—O2—Ru1125.8 (3)F3iv—P1—F4iii47.9 (11)
C4—O3—Ru1ii133.7 (3)F3iii—P1—F393.9 (17)
C6—O5—Ru1i131.4 (3)F3iv—P1—F393.9 (17)
C6—O4—Ru1126.9 (3)F3iii—P1—F3iv93.9 (17)
C1—N1—Ru1126.5 (3)F3—P1—F1iii80.4 (12)
C1—N1—C3106.5 (4)F3iv—P1—F180.4 (13)
C3—N1—Ru1126.6 (3)F3iii—P1—F195.3 (10)
C1—N2—H2126.1F3iii—P1—F1iv80.4 (12)
C1—N2—C2107.8 (4)F3—P1—F1169.5 (12)
C2—N2—H2126.1F3iv—P1—F1iv169.5 (12)
O5—C6—C7117.6 (4)F3iv—P1—F1iii95.3 (10)
O4—C6—O5126.0 (4)F3—P1—F1iv95.3 (10)
O4—C6—C7116.4 (4)F3iii—P1—F1iii169.5 (12)
N1—C1—N2110.4 (4)F1—P1—F4iv141.3 (7)
N1—C1—H1124.8F1iii—P1—F4iii85.1 (7)
N2—C1—H1124.8F1iii—P1—F4141.3 (7)
C6—C7—H7A109.5F1iii—P1—F4iv127.3 (9)
C6—C7—H7B109.5F1—P1—F485.1 (7)
C6—C7—H7C109.5F1iv—P1—F4iv85.1 (7)
H7A—C7—H7B109.5F1iv—P1—F4127.3 (9)
H7A—C7—H7C109.5F1—P1—F4iii127.3 (9)
H7B—C7—H7C109.5F1iv—P1—F4iii141.3 (7)
O2—C4—C5116.8 (4)F1—P1—F1iv91.3 (12)
O3—C4—O2126.0 (4)F1iii—P1—F1iv91.3 (12)
O3—C4—C5117.1 (4)F1—P1—F1iii91.3 (12)
N1—C3—H3125.6P1B—F5—F2iii60.2 (11)
C2—C3—N1108.9 (4)P1B—F2—F5iv53.7 (9)
C2—C3—H3125.6
Symmetry codes: (i) y+1, z1/2, 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) top
Crystal data top
[Ru3(C2H3O2)6O(C11H9N)2(CO)]·CH4OF(000) = 2088
Mr = 1043.91Dx = 1.746 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 7.8680 (9) ÅCell parameters from 8467 reflections
b = 22.098 (3) Åθ = 2.6–25.3°
c = 22.848 (3) ŵ = 1.20 mm1
β = 90.312 (2)°T = 173 K
V = 3972.4 (8) Å3Plate, blue
Z = 40.32 × 0.15 × 0.01 mm
Data collection top
Bruker APEXII CCD
diffractometer
7285 independent reflections
Radiation source: sealed tube5241 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.075
Detector resolution: 8.36 pixels mm-1θmax = 25.4°, θmin = 1.3°
ω scansh = 99
Absorption correction: multi-scan
(SADABS; Bruker, 2015)
k = 2626
Tmin = 0.641, Tmax = 0.745l = 2727
31959 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.044H-atom parameters constrained
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0529P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
7285 reflectionsΔρmax = 1.05 e Å3
513 parametersΔρmin = 0.48 e Å3
0 restraints
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ru10.64933 (6)0.72903 (2)0.23660 (2)0.02788 (13)
Ru20.44995 (6)0.62796 (2)0.32691 (2)0.02711 (13)
Ru30.64605 (5)0.57734 (2)0.21013 (2)0.02533 (13)
O10.5777 (4)0.64228 (14)0.25848 (15)0.0256 (8)
O20.7761 (6)0.85158 (19)0.2049 (2)0.0567 (13)
O30.4094 (5)0.76366 (16)0.25058 (18)0.0377 (10)
O40.2919 (5)0.70177 (16)0.31712 (17)0.0356 (9)
O50.7231 (5)0.74744 (16)0.32245 (17)0.0358 (9)
O60.6147 (5)0.67449 (17)0.38026 (16)0.0361 (9)
O70.2729 (5)0.57568 (16)0.28353 (16)0.0337 (9)
O80.4351 (5)0.52422 (16)0.22112 (17)0.0351 (9)
O90.5832 (5)0.55267 (16)0.35239 (16)0.0367 (10)
O100.7629 (5)0.53436 (16)0.27846 (16)0.0341 (9)
O110.5762 (5)0.71387 (16)0.14955 (17)0.0377 (9)
O120.5350 (5)0.61358 (16)0.13671 (15)0.0346 (9)
O130.8987 (5)0.70308 (17)0.22313 (19)0.0437 (11)
O140.8762 (5)0.61121 (17)0.18462 (18)0.0425 (10)
N10.2899 (6)0.61469 (19)0.40068 (19)0.0329 (11)
N20.7290 (5)0.50544 (18)0.15647 (18)0.0271 (10)
C10.7227 (8)0.8053 (3)0.2169 (3)0.0367 (14)
C20.1196 (7)0.6088 (3)0.3921 (3)0.0373 (14)
H20.07790.60730.35300.045*
C30.0048 (7)0.6049 (2)0.4370 (3)0.0371 (14)
H30.11290.60010.42870.045*
C40.0614 (7)0.6080 (2)0.4943 (3)0.0326 (13)
C50.2342 (8)0.6144 (2)0.5034 (3)0.0394 (15)
H50.27840.61760.54200.047*
C60.3436 (8)0.6163 (2)0.4555 (2)0.0361 (14)
H60.46240.61880.46280.043*
C70.0650 (8)0.6049 (3)0.5437 (3)0.0384 (14)
C80.1941 (8)0.5626 (3)0.5424 (3)0.0465 (16)
H80.20360.53560.51020.056*
C90.3110 (9)0.5590 (3)0.5883 (3)0.061 (2)
H90.39870.52950.58760.073*
C100.2974 (9)0.5990 (3)0.6345 (3)0.062 (2)
H100.37670.59730.66570.075*
C110.1678 (9)0.6416 (3)0.6355 (3)0.0531 (18)
H110.15950.66930.66720.064*
C120.0497 (8)0.6441 (3)0.5903 (3)0.0426 (15)
H120.04050.67270.59160.051*
C130.7912 (7)0.5162 (3)0.1029 (3)0.0400 (15)
H130.78380.55610.08760.048*
C140.8650 (8)0.4721 (3)0.0693 (3)0.0434 (15)
H140.90530.48180.03130.052*
C150.8813 (7)0.4134 (3)0.0902 (3)0.0368 (14)
C160.8120 (7)0.4025 (3)0.1448 (3)0.0390 (15)
H160.81770.36300.16100.047*
C170.7355 (7)0.4477 (3)0.1759 (3)0.0388 (14)
H170.68510.43820.21240.047*
C180.9741 (7)0.3673 (2)0.0563 (3)0.0375 (14)
C190.9793 (8)0.3682 (3)0.0042 (3)0.0437 (15)
H190.92200.39930.02520.052*
C201.0674 (8)0.3242 (3)0.0344 (3)0.0495 (17)
H201.07020.32570.07590.059*
C211.1502 (8)0.2788 (3)0.0061 (3)0.0515 (18)
H211.20770.24830.02760.062*
C221.1497 (8)0.2775 (3)0.0543 (3)0.0468 (16)
H221.20960.24670.07470.056*
C231.0612 (7)0.3216 (3)0.0853 (3)0.0405 (15)
H231.06050.32030.12690.049*
C240.2966 (7)0.7492 (2)0.2861 (2)0.0308 (13)
C250.1470 (7)0.7922 (3)0.2923 (3)0.0421 (15)
H25A0.16590.81870.32610.063*
H25B0.04250.76890.29800.063*
H25C0.13630.81680.25670.063*
C260.7070 (7)0.7204 (3)0.3699 (3)0.0337 (13)
C270.8092 (8)0.7442 (3)0.4210 (3)0.0416 (15)
H27A0.92580.72880.41870.062*
H27B0.75740.73070.45760.062*
H27C0.81080.78850.41980.062*
C280.2987 (7)0.5342 (2)0.2472 (2)0.0302 (13)
C290.1497 (7)0.4932 (3)0.2320 (3)0.0413 (15)
H29A0.04870.50660.25330.062*
H29B0.17720.45150.24310.062*
H29C0.12730.49510.18980.062*
C300.7089 (7)0.5267 (2)0.3299 (2)0.0296 (12)
C310.8025 (7)0.4817 (2)0.3663 (2)0.0380 (14)
H31A0.77980.48940.40780.057*
H31B0.92470.48540.35900.057*
H31C0.76460.44080.35600.057*
C320.5280 (7)0.6689 (3)0.1211 (2)0.0314 (13)
C330.4518 (8)0.6805 (3)0.0617 (2)0.0418 (15)
H33A0.43570.72410.05620.063*
H33B0.34170.65990.05860.063*
H33C0.52820.66500.03150.063*
C340.9574 (7)0.6582 (3)0.1972 (3)0.0327 (13)
C351.1377 (7)0.6611 (3)0.1769 (3)0.0387 (14)
H35A1.15990.70110.16000.058*
H35B1.15670.62990.14720.058*
H35C1.21440.65430.21020.058*
O1S0.3088 (7)0.5284 (2)0.0740 (3)0.0809 (17)
H1S0.37060.54650.09840.121*
C1S0.3580 (10)0.4677 (3)0.0707 (4)0.078 (2)
H1SA0.46500.46460.04920.117*
H1SB0.26970.44440.05040.117*
H1SC0.37390.45160.11030.117*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0296 (3)0.0239 (2)0.0301 (3)0.00176 (18)0.00353 (19)0.00253 (19)
Ru20.0303 (3)0.0241 (2)0.0270 (3)0.00130 (19)0.00530 (19)0.00161 (18)
Ru30.0259 (2)0.0239 (2)0.0262 (3)0.00150 (18)0.00342 (19)0.00091 (18)
O10.0240 (19)0.0233 (18)0.030 (2)0.0004 (15)0.0022 (16)0.0017 (16)
O20.071 (3)0.034 (2)0.066 (3)0.015 (2)0.003 (3)0.013 (2)
O30.028 (2)0.035 (2)0.050 (3)0.0042 (17)0.0119 (19)0.0079 (19)
O40.037 (2)0.033 (2)0.037 (2)0.0082 (17)0.0060 (18)0.0019 (18)
O50.040 (2)0.034 (2)0.034 (2)0.0106 (18)0.0001 (19)0.0028 (18)
O60.040 (2)0.034 (2)0.034 (2)0.0087 (19)0.0028 (18)0.0026 (18)
O70.029 (2)0.035 (2)0.038 (2)0.0047 (17)0.0087 (18)0.0056 (18)
O80.028 (2)0.033 (2)0.045 (2)0.0088 (17)0.0106 (18)0.0101 (18)
O90.044 (2)0.030 (2)0.036 (2)0.0050 (18)0.0134 (19)0.0112 (18)
O100.040 (2)0.036 (2)0.026 (2)0.0056 (18)0.0003 (18)0.0062 (17)
O110.050 (3)0.029 (2)0.035 (2)0.0063 (18)0.0026 (19)0.0029 (18)
O120.047 (2)0.033 (2)0.024 (2)0.0040 (18)0.0050 (18)0.0000 (17)
O130.029 (2)0.031 (2)0.071 (3)0.0048 (18)0.013 (2)0.008 (2)
O140.033 (2)0.036 (2)0.058 (3)0.0098 (19)0.015 (2)0.007 (2)
N10.049 (3)0.023 (2)0.027 (3)0.003 (2)0.012 (2)0.005 (2)
N20.030 (3)0.027 (2)0.025 (3)0.0004 (19)0.002 (2)0.0005 (19)
C10.044 (4)0.027 (3)0.038 (4)0.001 (3)0.002 (3)0.001 (3)
C20.031 (3)0.041 (3)0.040 (4)0.001 (3)0.010 (3)0.001 (3)
C30.032 (3)0.036 (3)0.044 (4)0.003 (3)0.007 (3)0.001 (3)
C40.033 (3)0.024 (3)0.041 (4)0.004 (2)0.003 (3)0.003 (3)
C50.049 (4)0.036 (3)0.033 (4)0.003 (3)0.002 (3)0.004 (3)
C60.047 (4)0.027 (3)0.035 (4)0.001 (3)0.006 (3)0.004 (3)
C70.046 (4)0.036 (3)0.033 (3)0.006 (3)0.006 (3)0.010 (3)
C80.052 (4)0.044 (4)0.044 (4)0.005 (3)0.012 (3)0.004 (3)
C90.050 (4)0.065 (5)0.068 (5)0.020 (4)0.025 (4)0.003 (4)
C100.058 (5)0.081 (5)0.047 (4)0.015 (4)0.020 (4)0.006 (4)
C110.055 (4)0.060 (4)0.044 (4)0.003 (4)0.010 (3)0.013 (3)
C120.047 (4)0.038 (3)0.042 (4)0.001 (3)0.007 (3)0.000 (3)
C130.045 (4)0.038 (3)0.038 (4)0.007 (3)0.005 (3)0.004 (3)
C140.052 (4)0.039 (3)0.039 (4)0.004 (3)0.014 (3)0.006 (3)
C150.032 (3)0.040 (3)0.039 (4)0.004 (3)0.004 (3)0.001 (3)
C160.050 (4)0.025 (3)0.042 (4)0.005 (3)0.009 (3)0.001 (3)
C170.045 (4)0.038 (3)0.034 (3)0.001 (3)0.003 (3)0.002 (3)
C180.038 (4)0.032 (3)0.042 (4)0.002 (3)0.004 (3)0.005 (3)
C190.050 (4)0.046 (4)0.035 (4)0.001 (3)0.001 (3)0.001 (3)
C200.061 (5)0.053 (4)0.035 (4)0.008 (3)0.007 (3)0.002 (3)
C210.053 (4)0.040 (4)0.061 (5)0.008 (3)0.010 (4)0.003 (3)
C220.051 (4)0.042 (4)0.047 (4)0.012 (3)0.010 (3)0.003 (3)
C230.047 (4)0.037 (3)0.038 (4)0.004 (3)0.007 (3)0.007 (3)
C240.029 (3)0.032 (3)0.032 (3)0.001 (2)0.001 (3)0.002 (3)
C250.034 (3)0.036 (3)0.056 (4)0.002 (3)0.005 (3)0.003 (3)
C260.033 (3)0.035 (3)0.033 (3)0.002 (3)0.000 (3)0.002 (3)
C270.047 (4)0.041 (3)0.037 (4)0.007 (3)0.005 (3)0.006 (3)
C280.031 (3)0.030 (3)0.030 (3)0.001 (2)0.003 (3)0.005 (3)
C290.036 (3)0.037 (3)0.052 (4)0.006 (3)0.003 (3)0.009 (3)
C300.032 (3)0.027 (3)0.030 (3)0.007 (2)0.000 (3)0.001 (2)
C310.046 (4)0.030 (3)0.038 (4)0.005 (3)0.000 (3)0.006 (3)
C320.021 (3)0.043 (4)0.030 (3)0.004 (3)0.002 (2)0.004 (3)
C330.053 (4)0.038 (3)0.034 (3)0.005 (3)0.008 (3)0.004 (3)
C340.028 (3)0.033 (3)0.037 (3)0.001 (3)0.004 (3)0.007 (3)
C350.028 (3)0.042 (3)0.046 (4)0.003 (3)0.005 (3)0.002 (3)
O1S0.094 (4)0.058 (3)0.090 (4)0.002 (3)0.042 (3)0.011 (3)
C1S0.061 (5)0.068 (5)0.104 (7)0.017 (4)0.016 (5)0.009 (5)
Geometric parameters (Å, º) top
Ru1—O12.060 (3)C11—H110.9500
Ru1—O32.063 (4)C11—C121.394 (8)
Ru1—O52.082 (4)C12—H120.9500
Ru1—O112.094 (4)C13—H130.9500
Ru1—O132.069 (4)C13—C141.373 (8)
Ru1—C11.839 (6)C14—H140.9500
Ru2—O11.890 (3)C14—C151.388 (8)
Ru2—O42.062 (4)C15—C161.385 (8)
Ru2—O62.051 (4)C15—C181.477 (8)
Ru2—O72.060 (4)C16—H160.9500
Ru2—O92.049 (4)C16—C171.367 (8)
Ru2—N12.130 (4)C17—H170.9500
Ru3—O11.891 (3)C18—C191.384 (8)
Ru3—O82.050 (3)C18—C231.388 (8)
Ru3—O102.042 (4)C19—H190.9500
Ru3—O122.050 (4)C19—C201.381 (8)
Ru3—O142.047 (4)C20—H200.9500
Ru3—N22.112 (4)C20—C211.358 (9)
O2—C11.139 (6)C21—H210.9500
O3—C241.247 (6)C21—C221.381 (9)
O4—C241.265 (6)C22—H220.9500
O5—C261.245 (6)C22—C231.392 (8)
O6—C261.270 (6)C23—H230.9500
O7—C281.254 (6)C24—C251.521 (8)
O8—C281.249 (6)C25—H25A0.9800
O9—C301.256 (6)C25—H25B0.9800
O10—C301.263 (6)C25—H25C0.9800
O11—C321.246 (6)C26—C271.508 (8)
O12—C321.274 (6)C27—H27A0.9800
O13—C341.246 (6)C27—H27B0.9800
O14—C341.251 (6)C27—H27C0.9800
N1—C21.359 (7)C28—C291.520 (7)
N1—C61.321 (7)C29—H29A0.9800
N2—C131.342 (7)C29—H29B0.9800
N2—C171.351 (7)C29—H29C0.9800
C2—H20.9500C30—C311.488 (7)
C2—C31.373 (8)C31—H31A0.9800
C3—H30.9500C31—H31B0.9800
C3—C41.383 (8)C31—H31C0.9800
C4—C51.381 (8)C32—C331.503 (8)
C4—C71.510 (8)C33—H33A0.9800
C5—H50.9500C33—H33B0.9800
C5—C61.396 (8)C33—H33C0.9800
C6—H60.9500C34—C351.497 (8)
C7—C81.381 (8)C35—H35A0.9800
C7—C121.376 (8)C35—H35B0.9800
C8—H80.9500C35—H35C0.9800
C8—C91.400 (8)O1S—H1S0.8400
C9—H90.9500O1S—C1S1.398 (8)
C9—C101.380 (9)C1S—H1SA0.9800
C10—H100.9500C1S—H1SB0.9800
C10—C111.388 (9)C1S—H1SC0.9800
O1—Ru1—O393.21 (14)C7—C12—C11119.4 (6)
O1—Ru1—O591.63 (14)C7—C12—H12120.3
O1—Ru1—O1190.43 (14)C11—C12—H12120.3
O1—Ru1—O1392.24 (14)N2—C13—H13118.6
O3—Ru1—O591.85 (16)N2—C13—C14122.8 (5)
O3—Ru1—O1187.67 (16)C14—C13—H13118.6
O3—Ru1—O13174.28 (14)C13—C14—H14119.7
O5—Ru1—O11177.91 (14)C13—C14—C15120.5 (6)
O13—Ru1—O586.25 (16)C15—C14—H14119.7
O13—Ru1—O1194.04 (16)C14—C15—C18120.6 (5)
C1—Ru1—O1177.5 (2)C16—C15—C14115.9 (5)
C1—Ru1—O389.2 (2)C16—C15—C18123.5 (5)
C1—Ru1—O588.0 (2)C15—C16—H16119.4
C1—Ru1—O1190.0 (2)C17—C16—C15121.1 (5)
C1—Ru1—O1385.3 (2)C17—C16—H16119.4
O1—Ru2—O495.80 (14)N2—C17—C16122.4 (5)
O1—Ru2—O694.03 (15)N2—C17—H17118.8
O1—Ru2—O793.29 (14)C16—C17—H17118.8
O1—Ru2—O995.58 (14)C19—C18—C15122.2 (5)
O1—Ru2—N1175.68 (16)C19—C18—C23118.1 (5)
O4—Ru2—N180.56 (16)C23—C18—C15119.7 (5)
O6—Ru2—O492.68 (15)C18—C19—H19119.8
O6—Ru2—O7172.23 (14)C20—C19—C18120.4 (6)
O6—Ru2—N188.47 (17)C20—C19—H19119.8
O7—Ru2—O489.18 (15)C19—C20—H20119.2
O7—Ru2—N184.39 (16)C21—C20—C19121.5 (6)
O9—Ru2—O4168.55 (15)C21—C20—H20119.2
O9—Ru2—O685.25 (15)C20—C21—H21120.4
O9—Ru2—O791.44 (15)C20—C21—C22119.2 (6)
O9—Ru2—N188.12 (16)C22—C21—H21120.4
O1—Ru3—O897.47 (14)C21—C22—H22120.1
O1—Ru3—O1091.98 (14)C21—C22—C23119.9 (6)
O1—Ru3—O1293.45 (14)C23—C22—H22120.1
O1—Ru3—O1498.25 (15)C18—C23—C22120.9 (6)
O1—Ru3—N2178.52 (15)C18—C23—H23119.6
O8—Ru3—O1288.97 (15)C22—C23—H23119.6
O8—Ru3—N283.88 (15)O3—C24—O4126.9 (5)
O10—Ru3—O890.09 (15)O3—C24—C25117.0 (5)
O10—Ru3—O12174.56 (14)O4—C24—C25116.2 (5)
O10—Ru3—O1489.56 (16)C24—C25—H25A109.5
O10—Ru3—N287.40 (15)C24—C25—H25B109.5
O12—Ru3—N287.17 (15)C24—C25—H25C109.5
O14—Ru3—O8164.28 (15)H25A—C25—H25B109.5
O14—Ru3—O1289.89 (16)H25A—C25—H25C109.5
O14—Ru3—N280.40 (15)H25B—C25—H25C109.5
Ru2—O1—Ru1120.25 (16)O5—C26—O6127.4 (5)
Ru2—O1—Ru3120.68 (16)O5—C26—C27116.8 (5)
Ru3—O1—Ru1119.05 (17)O6—C26—C27115.9 (5)
C24—O3—Ru1131.3 (4)C26—C27—H27A109.5
C24—O4—Ru2134.1 (4)C26—C27—H27B109.5
C26—O5—Ru1134.2 (4)C26—C27—H27C109.5
C26—O6—Ru2130.5 (4)H27A—C27—H27B109.5
C28—O7—Ru2128.1 (3)H27A—C27—H27C109.5
C28—O8—Ru3130.9 (3)H27B—C27—H27C109.5
C30—O9—Ru2131.1 (3)O7—C28—C29117.3 (5)
C30—O10—Ru3128.4 (4)O8—C28—O7126.0 (5)
C32—O11—Ru1134.8 (4)O8—C28—C29116.7 (5)
C32—O12—Ru3128.4 (4)C28—C29—H29A109.5
C34—O13—Ru1130.2 (4)C28—C29—H29B109.5
C34—O14—Ru3133.5 (4)C28—C29—H29C109.5
C2—N1—Ru2119.1 (4)H29A—C29—H29B109.5
C6—N1—Ru2124.0 (4)H29A—C29—H29C109.5
C6—N1—C2116.7 (5)H29B—C29—H29C109.5
C13—N2—Ru3120.7 (4)O9—C30—O10126.1 (5)
C13—N2—C17117.0 (5)O9—C30—C31117.7 (5)
C17—N2—Ru3122.0 (4)O10—C30—C31116.2 (5)
O2—C1—Ru1176.6 (5)C30—C31—H31A109.5
N1—C2—H2118.3C30—C31—H31B109.5
N1—C2—C3123.4 (6)C30—C31—H31C109.5
C3—C2—H2118.3H31A—C31—H31B109.5
C2—C3—H3120.2H31A—C31—H31C109.5
C2—C3—C4119.6 (6)H31B—C31—H31C109.5
C4—C3—H3120.2O11—C32—O12127.3 (5)
C3—C4—C7119.7 (5)O11—C32—C33117.0 (5)
C5—C4—C3117.3 (5)O12—C32—C33115.7 (5)
C5—C4—C7123.0 (5)C32—C33—H33A109.5
C4—C5—H5120.1C32—C33—H33B109.5
C4—C5—C6119.8 (6)C32—C33—H33C109.5
C6—C5—H5120.1H33A—C33—H33B109.5
N1—C6—C5123.1 (6)H33A—C33—H33C109.5
N1—C6—H6118.4H33B—C33—H33C109.5
C5—C6—H6118.4O13—C34—O14125.5 (5)
C8—C7—C4120.1 (5)O13—C34—C35117.9 (5)
C12—C7—C4119.6 (5)O14—C34—C35116.6 (5)
C12—C7—C8120.3 (6)C34—C35—H35A109.5
C7—C8—H8119.8C34—C35—H35B109.5
C7—C8—C9120.5 (6)C34—C35—H35C109.5
C9—C8—H8119.8H35A—C35—H35B109.5
C8—C9—H9120.4H35A—C35—H35C109.5
C10—C9—C8119.2 (6)H35B—C35—H35C109.5
C10—C9—H9120.4C1S—O1S—H1S109.5
C9—C10—H10120.0O1S—C1S—H1SA109.5
C9—C10—C11120.0 (6)O1S—C1S—H1SB109.5
C11—C10—H10120.0O1S—C1S—H1SC109.5
C10—C11—H11119.7H1SA—C1S—H1SB109.5
C10—C11—C12120.5 (6)H1SA—C1S—H1SC109.5
C12—C11—H11119.7H1SB—C1S—H1SC109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1S—H1S···O120.842.152.956 (6)161
Comparison of visible absorption bands (λmax, nm) for [1]PF6, [2]PF6, [3]PF6, 1-CO, and 3-CO. top
Lpyimidazolebenzimidazole4PP
[Ru3(OAc)6O(L)3]+690673678694
[Ru3(OAc)6O(L)2(CO)]585571NA592
Selected bond lengths (Å) and angles (°) for [1]PF6 and 3 compared to literature values for [Ru3O(OAc)66(pyridine)3]+ (Goeltz, Benson et al., 2010) top
[1]PF63[Ru3(OAc)6O(pyridine)3]+
Ru1—µ3-O1.9211 (4)1.934 (6)1.943
Ru2—µ3-O1.9212 (4)*1.899 (6)1.913
Ru3—µ3-O1.9212 (4)1.928 (6)1.947
Ru1—N2.093 (4)*2.124 (8)2.082
Ru2—N2.093 (4)2.128 (9)2.104
Ru3—N2.093 (4)2.111 (9)2.109
Ru1—O—Ru2119.965 (9)*119.8 (3)119.95
Ru2—O—Ru3119.964 (9)121.1 (3)120.33
Ru1—O—Ru3119.964 (9)119.0 (3)119.72
Symmetry operations for [1]PF6: (1) -y+1, z-1/2, -x+3/2; (2) -z+3/2, -x+1, y+1/2.
Selected bond lengths (Å) and angles (°) for 1-CO and 3-CO. top
1-CO3-CO
Ru1—µ3-O2.038 (3)2.060 (3)
Ru2—µ3-O1.893 (3)1.890 (3)
Ru3—µ3-O1.902 (3)1.891 (3)
Ru1—CCO1.853 (5)1.839 (6)
Ru2—N2.095 (4)2.130 (4)
Ru3—N2.097 (3)2.112 (4)
Ru1—O—Ru2120.39 (14)120.25 (16)
Ru2—O—Ru3119.92 (14)120.68 (16)
Ru1—O—Ru3119.67 (14)119.05 (17)
Electrochemical data (V) for [1]PF6, [2]PF6, [3]PF6, 1-CO, and 2-CO recorded in acetonitrile. Data for [Ru3(OAc)6O(py)3]+ and [Ru3(OAc)6O(py)2(CO)] were converted from SSCE values as reported (Baumann et al., 1978) top
Cluster/couple3+/2+2+/1+1+/00/1-1-/2-
[Ru3(OAc)6O(py)3]+1.880.92-0.10-1.37NA
[1]PF61.85†0.80-0.32-1.63†NA
[2]PF61.9†0.96-0.13-1.35†NA
[3]PF6NA1.100.08-1.14-1.65
[Ru3(OAc)6O(py)2(CO)]NA1.210.57-0.93NA
1-CONA1.30†0.66-0.99NA
3-CONA1.360.75-0.72-1.52
Note: (†) irreversible.
Electrochemical data (V) for [1]PF6 and [2]PF6 recorded in 9:1 (v/v) CH2Cl2–MeOH with 0.1 M TBAPF6, glassy carbon working electrode, Ag/AgCl reference electrode, and Pt wire counter electrode, scan rate 100 mV s-1 top
3+/2+2+/1+1+/00/1-
[1]PF6NA0.95-0.22-1.75†
[2]PF6NA0.97-0.15-1.56†
Note: (†) irreversible.
 

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