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The title complex, [Ru2(C11H9N2)4(H2O)][SbF6]·C2H10O, has a diruthenium(II,III) unit bridged by four PhNpy ligands. There is an axial aqua ligand on the ruthenium(III) atom. The Ru...Ru distance is 2.288 (1) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803011760/ww6071sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803011760/ww6071Isup2.hkl
Contains datablock I

CCDC reference: 217357

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.018 Å
  • H-atom completeness 92%
  • R factor = 0.086
  • wR factor = 0.199
  • Data-to-parameter ratio = 13.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
CRYSC_01 Alert C The word below has not been recognised as a standard identifier. deep PLAT_362 Alert C Short C(sp3)-C(sp2) Bond C01 - C02 = 1.33 Ang. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C48 H48 F6 N8 O2 Ru2 Sb1 Atom count from the _atom_site data: C48 H44 F6 N8 O2 Ru2 Sb1 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C48 H48 F6 N8 O2 Ru2 Sb TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 192.00 192.00 0.00 H 192.00 176.00 16.00 F 24.00 24.00 0.00 N 32.00 32.00 0.00 O 8.00 8.00 0.00 Ru 8.00 8.00 0.00 Sb 4.00 4.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

In the chemistry of multiple-bonded diruthenium complexes, a variety of diruthenium compounds have been reported (Cotton & Walton, 1985; Tooze et al., 1984; Chakravarty & Cotton, 1975) many years ago. In most cases, spectral and electrochemical studies on the diruthenium complexes show that modification of the axial ligand usually results in dramatic shift of the visible band energy and the redox potentials. These complexes of RuII–RuIII are quite different from those of other dimetallic species. The cationic species [Ru22-PhNpy)4·H2O]+ consists of a diruthenium core held by four PhNpy ligands. The ruthenium(III) that is bonded to pyridine N atoms has an axial H2O while the axial site on the other ruthenium(II) is vacant. The molecular structure of Ru2Cl(PhNpy)4 has already been reported (Chakravarty et al., 1985). The two molecules are very similar in structure except that the Ru—Cl bond in Ru2Cl(PhNpy)4 is replaced by Ru—OH2. This change has a little effect on the Ru—Ru distance, which changes from 2.275 (3) Å in Ru2Cl(PhNpy)4 to 2.288 (1) Å in [Ru2(ap)4(H2O)](SbF6). The average RuII—N distance is 2.014 (6) Å but RuIII—N is 2.056 (8) Å in the title compound, with the O1—Ru1—Ru2 angle being 178.80 (18)°

Experimental top

The title compound was synthesized by the reaction of Ru2Cl(PhNpy)4 with a small excess of AgSbF6 in methanol–dichloromethane in the dark for 12 h. The solution changed from blue to deep red. After filtration, the filtrate was evaporated under vacuum to leave a red residue which was dissolved in dichloromethane. Well shaped crystals suitable for X-ray diffraction measurement were grown by layering diethyl ether onto the solution. [Author: "_chemical_formula_sum 'C48 H46 F6 N8 O2 Ru2 Sb'" does not match the number of H atoms in the structure, i.e. (4 x 9) + 2 + 10 = H48; please check]

Refinement top

The positions of the H atoms were genetared geometrically (C—H bond fixed at 0.96 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms before the final cycle of least-squares refinement.

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: SMART and SAINT (Siemens, 1996); data reduction: XPREP (Siemens, 1997); program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. A view of the cation of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity.
(I) top
Crystal data top
[Ru2(C11H9N2)4(H2O)][SbF6]·C4H10OF(000) = 2404
Mr = 1206.83Dx = 1.667 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5202 reflections
a = 10.1385 (1) Åθ = 1.3–22.5°
b = 22.5901 (5) ŵ = 1.25 mm1
c = 21.0672 (5) ÅT = 293 K
β = 94.860 (1)°Block, deep red
V = 4807.67 (16) Å30.72 × 0.46 × 0.30 mm
Z = 4
Data collection top
Siemens SMART CCD
diffractometer
8405 independent reflections
Radiation source: fine-focus sealed tube5834 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
Detector resolution: 0 pixels mm-1θmax = 25.1°, θmin = 1.3°
ϕ and ω scansh = 1111
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 2624
Tmin = 0.433, Tmax = 0.687l = 2514
15139 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.086Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.199H atoms treated by a mixture of independent and constrained refinement
S = 1.17 w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P]
where P = (Fo2 + 2Fc2)/3
8405 reflections(Δ/σ)max = 0.001
604 parametersΔρmax = 0.89 e Å3
0 restraintsΔρmin = 0.75 e Å3
Crystal data top
[Ru2(C11H9N2)4(H2O)][SbF6]·C4H10OV = 4807.67 (16) Å3
Mr = 1206.83Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.1385 (1) ŵ = 1.25 mm1
b = 22.5901 (5) ÅT = 293 K
c = 21.0672 (5) Å0.72 × 0.46 × 0.30 mm
β = 94.860 (1)°
Data collection top
Siemens SMART CCD
diffractometer
8405 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5834 reflections with I > 2σ(I)
Tmin = 0.433, Tmax = 0.687Rint = 0.048
15139 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0860 restraints
wR(F2) = 0.199H atoms treated by a mixture of independent and constrained refinement
S = 1.17 w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P]
where P = (Fo2 + 2Fc2)/3
8405 reflectionsΔρmax = 0.89 e Å3
604 parametersΔρmin = 0.75 e Å3
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.56687 (9)0.03481 (4)0.71563 (4)0.0453 (2)
Ru20.57751 (8)0.05181 (3)0.77213 (4)0.0386 (2)
Sb0.91245 (12)0.18550 (6)0.52021 (6)0.1028 (4)
O10.5563 (7)0.1118 (3)0.6675 (3)0.0474 (17)
O020.9038 (17)0.2341 (6)0.9673 (7)0.148 (5)
N10.5037 (8)0.0771 (4)0.7940 (4)0.046 (2)
N20.4719 (8)0.0150 (3)0.8383 (3)0.0422 (19)
N30.7603 (8)0.0518 (3)0.7474 (4)0.0426 (19)
N40.7466 (7)0.0231 (3)0.8209 (3)0.0372 (18)
N50.3745 (9)0.0139 (4)0.6830 (4)0.051 (2)
N60.4088 (8)0.0803 (4)0.7237 (3)0.0417 (19)
N70.6359 (8)0.0082 (4)0.6396 (3)0.048 (2)
N80.6852 (8)0.0880 (3)0.7065 (4)0.0422 (19)
F10.866 (3)0.2540 (7)0.4994 (12)0.391 (18)
F20.945 (2)0.1071 (9)0.5303 (13)0.339 (14)
F30.967 (2)0.1745 (13)0.4429 (10)0.326 (13)
F41.0718 (18)0.1928 (11)0.5543 (11)0.321 (12)
F50.8498 (18)0.1854 (10)0.5942 (6)0.270 (10)
F60.7503 (15)0.1608 (12)0.4869 (8)0.303 (12)
C010.917 (3)0.2865 (10)1.0009 (14)0.198 (13)
H01A0.90850.32260.97980.237*
C020.942 (4)0.2849 (11)1.0639 (13)0.26 (2)
H02A0.94750.32451.08030.388*
H02B1.02450.26481.07450.388*
H02C0.87210.26411.08240.388*
C030.821 (3)0.2307 (12)0.9105 (10)0.177 (11)
H03A0.76680.26090.89340.212*
C040.833 (2)0.1736 (8)0.8836 (8)0.123 (7)
H04A0.77660.17090.84480.184*
H04B0.80740.14420.91310.184*
H04C0.92320.16700.87480.184*
C120.4980 (12)0.1373 (5)0.7978 (6)0.064 (3)
H12A0.52910.15940.76500.077*
C130.4490 (13)0.1668 (5)0.8474 (6)0.068 (3)
H13A0.44800.20800.84870.081*
C140.4015 (13)0.1341 (5)0.8952 (6)0.066 (3)
H14A0.36560.15330.92870.079*
C150.4059 (11)0.0739 (5)0.8943 (5)0.053 (3)
H15A0.37460.05210.92730.064*
C160.4586 (9)0.0452 (4)0.8428 (4)0.041 (2)
C210.3929 (11)0.0508 (4)0.8760 (5)0.047 (2)
C220.2578 (11)0.0547 (5)0.8587 (5)0.054 (3)
H22A0.21980.03180.82530.065*
C230.1807 (12)0.0923 (5)0.8906 (6)0.066 (3)
H23A0.09020.09430.87890.079*
C240.2341 (13)0.1265 (6)0.9390 (6)0.071 (4)
H24A0.18090.15210.96010.086*
C250.3677 (14)0.1229 (6)0.9567 (6)0.081 (4)
H25A0.40460.14620.99000.098*
C260.4475 (13)0.0851 (6)0.9255 (5)0.069 (3)
H26A0.53760.08280.93780.083*
C320.8317 (12)0.0926 (5)0.7174 (5)0.057 (3)
H32A0.79080.11310.68280.068*
C330.9601 (13)0.1046 (6)0.7359 (6)0.072 (4)
H33A1.00570.13320.71470.086*
C341.0236 (12)0.0736 (5)0.7871 (6)0.065 (3)
H34A1.11220.08060.80000.079*
C350.9532 (10)0.0327 (5)0.8179 (5)0.056 (3)
H35A0.99360.01270.85300.067*
C360.8194 (10)0.0200 (4)0.7974 (4)0.042 (2)
C410.7863 (9)0.0461 (4)0.8824 (4)0.038 (2)
C420.7983 (11)0.1065 (5)0.8918 (5)0.053 (3)
H42A0.78240.13200.85740.064*
C430.8334 (13)0.1295 (6)0.9515 (6)0.069 (4)
H43A0.84130.17020.95710.083*
C440.8566 (12)0.0923 (7)1.0026 (5)0.071 (4)
H44A0.88180.10751.04280.085*
C450.8421 (13)0.0326 (6)0.9936 (6)0.073 (4)
H45A0.85750.00711.02820.087*
C460.8054 (12)0.0099 (5)0.9347 (5)0.056 (3)
H46A0.79320.03070.92990.068*
C520.3303 (10)0.0424 (5)0.6892 (4)0.046 (2)
C530.2013 (12)0.0563 (6)0.6614 (5)0.066 (3)
H53A0.16970.09480.66380.079*
C540.1235 (12)0.0140 (7)0.6313 (6)0.077 (4)
H54A0.03890.02330.61360.093*
C550.1717 (12)0.0429 (6)0.6273 (5)0.068 (4)
H55A0.12000.07210.60640.082*
C560.2935 (11)0.0560 (5)0.6537 (5)0.060 (3)
H56A0.32380.09470.65190.072*
C610.3826 (10)0.1419 (5)0.7209 (5)0.050 (3)
C620.3671 (13)0.1715 (6)0.6626 (6)0.076 (4)
H62A0.37000.15080.62460.091*
C630.3470 (17)0.2331 (7)0.6622 (9)0.109 (6)
H63A0.33550.25330.62360.131*
C640.3445 (15)0.2626 (6)0.7169 (9)0.100 (6)
H64A0.33030.30330.71570.120*
C650.3620 (14)0.2352 (6)0.7740 (7)0.078 (4)
H65A0.36050.25680.81160.093*
C660.3822 (11)0.1742 (5)0.7760 (6)0.058 (3)
H66A0.39570.15510.81510.069*
C720.6386 (13)0.0186 (6)0.5824 (5)0.071 (4)
H72A0.59720.05520.57640.085*
C730.6996 (15)0.0056 (7)0.5331 (6)0.083 (4)
H73A0.70170.01440.49460.100*
C740.7570 (14)0.0598 (7)0.5417 (6)0.079 (4)
H74A0.79750.07700.50830.095*
C750.7568 (12)0.0895 (6)0.5981 (5)0.063 (3)
H75A0.79700.12630.60360.076*
C760.6934 (10)0.0624 (5)0.6479 (4)0.048 (3)
C810.7720 (10)0.1356 (5)0.7259 (4)0.046 (2)
C820.9079 (12)0.1262 (6)0.7313 (5)0.063 (3)
H82A0.94230.09050.71810.076*
C830.9918 (13)0.1702 (6)0.7564 (6)0.075 (4)
H83A1.08290.16410.75920.090*
C840.9436 (15)0.2222 (6)0.7769 (6)0.079 (4)
H84A1.00110.25120.79420.095*
C850.8114 (15)0.2316 (5)0.7719 (6)0.073 (4)
H85A0.77790.26710.78610.088*
C860.7255 (12)0.1886 (5)0.7459 (6)0.061 (3)
H86A0.63500.19600.74200.074*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0501 (5)0.0453 (5)0.0407 (5)0.0049 (4)0.0048 (4)0.0099 (4)
Ru20.0382 (5)0.0405 (4)0.0369 (4)0.0010 (4)0.0019 (3)0.0030 (3)
Sb0.1013 (9)0.1135 (9)0.0932 (8)0.0261 (7)0.0060 (7)0.0350 (7)
O10.059 (4)0.038 (4)0.046 (4)0.007 (3)0.008 (3)0.023 (3)
O020.214 (16)0.112 (11)0.120 (11)0.014 (11)0.020 (11)0.001 (9)
N10.040 (5)0.044 (5)0.055 (5)0.010 (4)0.007 (4)0.013 (4)
N20.052 (5)0.038 (4)0.037 (4)0.001 (4)0.007 (4)0.005 (3)
N30.046 (5)0.037 (4)0.045 (4)0.001 (4)0.009 (4)0.010 (4)
N40.027 (4)0.045 (5)0.040 (4)0.001 (4)0.006 (3)0.008 (4)
N50.052 (6)0.063 (6)0.036 (4)0.011 (5)0.003 (4)0.009 (4)
N60.037 (5)0.052 (5)0.035 (4)0.002 (4)0.000 (4)0.014 (4)
N70.051 (5)0.059 (5)0.031 (4)0.011 (4)0.003 (4)0.004 (4)
N80.041 (5)0.042 (5)0.042 (5)0.006 (4)0.002 (4)0.003 (4)
F10.68 (5)0.130 (13)0.39 (3)0.17 (2)0.24 (3)0.122 (16)
F20.33 (3)0.200 (18)0.46 (4)0.054 (18)0.14 (3)0.00 (2)
F30.25 (2)0.51 (4)0.226 (19)0.11 (2)0.105 (16)0.01 (2)
F40.167 (15)0.43 (3)0.36 (3)0.104 (18)0.038 (17)0.09 (2)
F50.28 (2)0.44 (3)0.097 (9)0.013 (19)0.054 (11)0.062 (13)
F60.148 (13)0.58 (4)0.172 (14)0.053 (19)0.054 (11)0.027 (19)
C010.34 (4)0.083 (15)0.16 (2)0.01 (2)0.02 (3)0.015 (16)
C020.47 (6)0.14 (2)0.15 (2)0.03 (3)0.09 (3)0.033 (19)
C030.27 (3)0.17 (2)0.084 (14)0.03 (2)0.037 (17)0.029 (15)
C040.169 (19)0.111 (14)0.085 (12)0.005 (13)0.005 (12)0.026 (11)
C120.079 (9)0.045 (7)0.068 (8)0.006 (6)0.006 (7)0.011 (6)
C130.082 (9)0.042 (6)0.079 (9)0.013 (6)0.007 (7)0.007 (6)
C140.077 (9)0.066 (8)0.056 (7)0.013 (7)0.012 (6)0.008 (6)
C150.059 (7)0.051 (7)0.051 (6)0.003 (6)0.011 (5)0.006 (5)
C160.037 (5)0.042 (6)0.043 (5)0.000 (5)0.006 (4)0.002 (4)
C210.055 (7)0.046 (6)0.042 (5)0.004 (5)0.008 (5)0.002 (5)
C220.056 (7)0.051 (6)0.056 (6)0.001 (6)0.007 (5)0.003 (5)
C230.054 (7)0.073 (8)0.073 (8)0.017 (7)0.017 (6)0.004 (7)
C240.074 (9)0.073 (9)0.070 (8)0.027 (7)0.018 (7)0.003 (7)
C250.081 (10)0.104 (11)0.058 (8)0.013 (8)0.000 (7)0.037 (7)
C260.068 (8)0.089 (9)0.047 (7)0.013 (7)0.006 (6)0.024 (6)
C320.069 (8)0.055 (7)0.047 (6)0.003 (6)0.008 (6)0.007 (5)
C330.069 (9)0.074 (9)0.074 (9)0.016 (7)0.011 (7)0.010 (7)
C340.056 (8)0.070 (8)0.071 (8)0.019 (6)0.014 (6)0.002 (7)
C350.045 (7)0.067 (7)0.056 (7)0.011 (6)0.004 (5)0.007 (6)
C360.050 (6)0.035 (5)0.042 (5)0.000 (5)0.005 (5)0.001 (4)
C410.026 (5)0.046 (6)0.040 (5)0.001 (4)0.002 (4)0.002 (4)
C420.066 (7)0.044 (6)0.050 (6)0.002 (5)0.010 (5)0.006 (5)
C430.088 (10)0.059 (7)0.064 (8)0.011 (7)0.021 (7)0.027 (6)
C440.067 (8)0.104 (11)0.041 (7)0.010 (8)0.001 (6)0.020 (7)
C450.077 (9)0.094 (10)0.046 (7)0.014 (8)0.002 (6)0.012 (7)
C460.074 (8)0.051 (6)0.043 (6)0.006 (6)0.004 (6)0.000 (5)
C520.042 (6)0.060 (7)0.035 (5)0.000 (5)0.003 (4)0.001 (5)
C530.057 (7)0.082 (9)0.057 (7)0.006 (7)0.008 (6)0.003 (6)
C540.040 (7)0.128 (13)0.061 (8)0.004 (8)0.005 (6)0.027 (8)
C550.050 (7)0.094 (10)0.059 (7)0.021 (7)0.007 (6)0.026 (7)
C560.052 (7)0.074 (8)0.054 (7)0.008 (6)0.006 (5)0.025 (6)
C610.045 (6)0.045 (6)0.059 (7)0.007 (5)0.002 (5)0.003 (5)
C620.082 (9)0.074 (9)0.067 (8)0.015 (7)0.023 (7)0.024 (7)
C630.128 (15)0.064 (9)0.125 (14)0.017 (10)0.058 (12)0.038 (10)
C640.090 (11)0.053 (8)0.147 (16)0.001 (8)0.046 (11)0.002 (10)
C650.083 (10)0.059 (8)0.088 (10)0.010 (7)0.015 (8)0.016 (7)
C660.058 (7)0.046 (6)0.069 (8)0.001 (5)0.002 (6)0.000 (6)
C720.078 (9)0.083 (9)0.051 (7)0.001 (7)0.006 (6)0.019 (6)
C730.107 (12)0.102 (11)0.041 (7)0.018 (9)0.012 (7)0.009 (7)
C740.095 (11)0.100 (11)0.046 (7)0.008 (9)0.021 (7)0.004 (7)
C750.062 (8)0.079 (8)0.048 (7)0.004 (7)0.000 (6)0.004 (6)
C760.050 (6)0.061 (7)0.033 (5)0.002 (5)0.005 (5)0.002 (5)
C810.049 (6)0.055 (6)0.035 (5)0.004 (5)0.007 (5)0.016 (5)
C820.054 (7)0.076 (8)0.058 (7)0.016 (7)0.002 (6)0.006 (6)
C830.052 (8)0.090 (10)0.081 (9)0.014 (8)0.001 (7)0.029 (8)
C840.085 (11)0.062 (8)0.086 (10)0.028 (8)0.021 (8)0.017 (7)
C850.095 (11)0.045 (7)0.078 (9)0.006 (7)0.008 (8)0.006 (6)
C860.058 (8)0.056 (7)0.070 (8)0.002 (6)0.004 (6)0.011 (6)
Geometric parameters (Å, º) top
Ru1—O12.012 (6)C25—C261.382 (16)
Ru1—N72.048 (8)C25—H25A0.9300
Ru1—N32.054 (8)C26—H26A0.9300
Ru1—N12.056 (8)C32—C331.354 (16)
Ru1—N52.067 (9)C32—H32A0.9300
Ru1—Ru22.2882 (11)C33—C341.397 (17)
Ru2—N82.007 (8)C33—H33A0.9300
Ru2—N22.008 (8)C34—C351.365 (15)
Ru2—N62.022 (8)C34—H34A0.9300
Ru2—N42.029 (7)C35—C361.417 (14)
Sb—F11.666 (14)C35—H35A0.9300
Sb—F41.719 (17)C41—C461.373 (13)
Sb—F51.732 (13)C41—C421.382 (13)
Sb—F31.781 (18)C42—C431.379 (14)
Sb—F21.810 (19)C42—H42A0.9300
Sb—F61.820 (17)C43—C441.369 (17)
O02—C011.38 (3)C43—H43A0.9300
O02—C031.40 (2)C44—C451.369 (17)
N1—C121.364 (13)C44—H44A0.9300
N1—C161.368 (12)C45—C461.366 (15)
N2—C161.371 (12)C45—H45A0.9300
N2—C211.426 (12)C46—H46A0.9300
N3—C321.361 (13)C52—C531.422 (15)
N3—C361.370 (12)C53—C541.362 (16)
N4—C361.343 (12)C53—H53A0.9300
N4—C411.421 (11)C54—C551.379 (18)
N5—C521.357 (13)C54—H54A0.9300
N5—C561.369 (13)C55—C561.343 (16)
N6—C521.341 (12)C55—H55A0.9300
N6—C611.417 (12)C56—H56A0.9300
N7—C721.351 (13)C61—C661.370 (15)
N7—C761.359 (13)C61—C621.395 (15)
N8—C761.371 (12)C62—C631.406 (19)
N8—C811.428 (12)C62—H62A0.9300
C01—C021.33 (3)C63—C641.33 (2)
C01—H01A0.9300C63—H63A0.9300
C02—H02A0.9600C64—C651.35 (2)
C02—H02B0.9600C64—H64A0.9300
C02—H02C0.9600C65—C661.394 (16)
C03—C041.42 (3)C65—H65A0.9300
C03—H03A0.9300C66—H66A0.9300
C04—H04A0.9600C72—C731.368 (17)
C04—H04B0.9600C72—H72A0.9300
C04—H04C0.9600C73—C741.361 (18)
C12—C131.368 (16)C73—H73A0.9300
C12—H12A0.9300C74—C751.364 (16)
C13—C141.368 (16)C74—H74A0.9300
C13—H13A0.9300C75—C761.416 (14)
C14—C151.360 (15)C75—H75A0.9300
C14—H14A0.9300C81—C861.368 (15)
C15—C161.408 (14)C81—C821.389 (15)
C15—H15A0.9300C82—C831.385 (16)
C21—C261.376 (14)C82—H82A0.9300
C21—C221.390 (14)C83—C841.357 (19)
C22—C231.369 (15)C83—H83A0.9300
C22—H22A0.9300C84—C851.352 (18)
C23—C241.356 (17)C84—H84A0.9300
C23—H23A0.9300C85—C861.385 (16)
C24—C251.377 (17)C85—H85A0.9300
C24—H24A0.9300C86—H86A0.9300
O1—Ru1—N791.3 (3)C23—C24—H24A120.3
O1—Ru1—N390.6 (3)C25—C24—H24A120.3
N7—Ru1—N387.9 (3)C24—C25—C26120.6 (12)
O1—Ru1—N189.8 (3)C24—C25—H25A119.7
N7—Ru1—N1177.9 (3)C26—C25—H25A119.7
N3—Ru1—N190.3 (3)C21—C26—C25119.7 (12)
O1—Ru1—N591.3 (3)C21—C26—H26A120.2
N7—Ru1—N590.4 (3)C25—C26—H26A120.2
N3—Ru1—N5177.5 (3)C33—C32—N3122.5 (11)
N1—Ru1—N591.4 (3)C33—C32—H32A118.8
O1—Ru1—Ru2178.9 (2)N3—C32—H32A118.8
N7—Ru1—Ru289.8 (2)C32—C33—C34119.4 (12)
N3—Ru1—Ru289.4 (2)C32—C33—H33A120.3
N1—Ru1—Ru289.1 (2)C34—C33—H33A120.3
N5—Ru1—Ru288.8 (2)C35—C34—C33118.8 (12)
N8—Ru2—N2179.2 (3)C35—C34—H34A120.6
N8—Ru2—N690.5 (3)C33—C34—H34A120.6
N2—Ru2—N690.3 (3)C34—C35—C36121.1 (11)
N8—Ru2—N489.6 (3)C34—C35—H35A119.4
N2—Ru2—N489.6 (3)C36—C35—H35A119.4
N6—Ru2—N4179.9 (4)N4—C36—N3116.5 (9)
N8—Ru2—Ru189.6 (2)N4—C36—C35125.1 (9)
N2—Ru2—Ru190.2 (2)N3—C36—C35118.3 (9)
N6—Ru2—Ru190.5 (2)C46—C41—C42117.9 (9)
N4—Ru2—Ru189.5 (2)C46—C41—N4121.5 (9)
F1—Sb—F4104.8 (14)C42—C41—N4120.4 (9)
F1—Sb—F597.0 (10)C43—C42—C41121.0 (11)
F4—Sb—F591.6 (10)C43—C42—H42A119.5
F1—Sb—F389.5 (11)C41—C42—H42A119.5
F4—Sb—F392.4 (11)C44—C43—C42120.0 (11)
F5—Sb—F3171.3 (12)C44—C43—H43A120.0
F1—Sb—F2169.8 (13)C42—C43—H43A120.0
F4—Sb—F283.8 (11)C45—C44—C43119.2 (11)
F5—Sb—F288.2 (12)C45—C44—H44A120.4
F3—Sb—F284.5 (12)C43—C44—H44A120.4
F1—Sb—F687.6 (13)C46—C45—C44120.8 (11)
F4—Sb—F6167.6 (12)C46—C45—H45A119.6
F5—Sb—F687.6 (8)C44—C45—H45A119.6
F3—Sb—F686.9 (10)C45—C46—C41121.0 (11)
F2—Sb—F683.8 (11)C45—C46—H46A119.5
C01—O02—C03121 (2)C41—C46—H46A119.5
C12—N1—C16117.6 (9)N6—C52—N5117.7 (9)
C12—N1—Ru1121.9 (7)N6—C52—C53124.4 (10)
C16—N1—Ru1120.4 (7)N5—C52—C53117.8 (10)
C16—N2—C21117.4 (8)C54—C53—C52120.9 (13)
C16—N2—Ru2121.4 (6)C54—C53—H53A119.6
C21—N2—Ru2120.7 (6)C52—C53—H53A119.6
C32—N3—C36119.8 (9)C53—C54—C55119.2 (12)
C32—N3—Ru1120.4 (7)C53—C54—H54A120.4
C36—N3—Ru1119.7 (6)C55—C54—H54A120.4
C36—N4—C41118.7 (8)C56—C55—C54119.8 (11)
C36—N4—Ru2120.8 (6)C56—C55—H55A120.1
C41—N4—Ru2120.4 (6)C54—C55—H55A120.1
C52—N5—C56120.2 (10)C55—C56—N5122.0 (12)
C52—N5—Ru1119.5 (7)C55—C56—H56A119.0
C56—N5—Ru1120.3 (8)N5—C56—H56A119.0
C52—N6—C61120.3 (8)C66—C61—C62118.8 (11)
C52—N6—Ru2120.5 (7)C66—C61—N6120.1 (9)
C61—N6—Ru2118.8 (6)C62—C61—N6120.9 (10)
C72—N7—C76118.6 (9)C61—C62—C63119.0 (14)
C72—N7—Ru1121.2 (8)C61—C62—H62A120.5
C76—N7—Ru1119.8 (6)C63—C62—H62A120.5
C76—N8—C81119.6 (8)C64—C63—C62120.2 (14)
C76—N8—Ru2121.8 (7)C64—C63—H63A119.9
C81—N8—Ru2117.8 (6)C62—C63—H63A119.9
C02—C01—O02119 (2)C63—C64—C65122.0 (14)
C02—C01—H01A120.3C63—C64—H64A119.0
O02—C01—H01A120.3C65—C64—H64A119.0
C01—C02—H02A109.5C64—C65—C66119.1 (13)
C01—C02—H02B109.5C64—C65—H65A120.4
H02A—C02—H02B109.5C66—C65—H65A120.4
C01—C02—H02C109.5C61—C66—C65120.8 (12)
H02A—C02—H02C109.5C61—C66—H66A119.6
H02B—C02—H02C109.5C65—C66—H66A119.6
O02—C03—C04109.0 (19)N7—C72—C73122.8 (12)
O02—C03—H03A125.5N7—C72—H72A118.6
C04—C03—H03A125.5C73—C72—H72A118.6
C03—C04—H04A109.5C74—C73—C72118.3 (12)
C03—C04—H04B109.5C74—C73—H73A120.8
H04A—C04—H04B109.5C72—C73—H73A120.8
C03—C04—H04C109.5C73—C74—C75121.7 (12)
H04A—C04—H04C109.5C73—C74—H74A119.1
H04B—C04—H04C109.5C75—C74—H74A119.1
N1—C12—C13123.5 (11)C74—C75—C76117.9 (12)
N1—C12—H12A118.3C74—C75—H75A121.1
C13—C12—H12A118.3C76—C75—H75A121.1
C12—C13—C14118.1 (11)N7—C76—N8116.0 (9)
C12—C13—H13A120.9N7—C76—C75120.6 (9)
C14—C13—H13A120.9N8—C76—C75123.4 (10)
C15—C14—C13121.1 (11)C86—C81—C82118.3 (11)
C15—C14—H14A119.5C86—C81—N8121.9 (10)
C13—C14—H14A119.5C82—C81—N8119.4 (10)
C14—C15—C16119.1 (11)C83—C82—C81119.6 (12)
C14—C15—H15A120.4C83—C82—H82A120.2
C16—C15—H15A120.4C81—C82—H82A120.2
N1—C16—N2115.4 (9)C84—C83—C82121.2 (13)
N1—C16—C15120.6 (9)C84—C83—H83A119.4
N2—C16—C15123.9 (9)C82—C83—H83A119.4
C26—C21—C22119.2 (10)C85—C84—C83119.5 (12)
C26—C21—N2122.1 (10)C85—C84—H84A120.3
C22—C21—N2118.5 (9)C83—C84—H84A120.3
C23—C22—C21120.1 (11)C84—C85—C86120.4 (13)
C23—C22—H22A119.9C84—C85—H85A119.8
C21—C22—H22A119.9C86—C85—H85A119.8
C24—C23—C22121.0 (12)C81—C86—C85121.0 (12)
C24—C23—H23A119.5C81—C86—H86A119.5
C22—C23—H23A119.5C85—C86—H86A119.5
C23—C24—C25119.5 (12)

Experimental details

Crystal data
Chemical formula[Ru2(C11H9N2)4(H2O)][SbF6]·C4H10O
Mr1206.83
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)10.1385 (1), 22.5901 (5), 21.0672 (5)
β (°) 94.860 (1)
V3)4807.67 (16)
Z4
Radiation typeMo Kα
µ (mm1)1.25
Crystal size (mm)0.72 × 0.46 × 0.30
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.433, 0.687
No. of measured, independent and
observed [I > 2σ(I)] reflections
15139, 8405, 5834
Rint0.048
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.086, 0.199, 1.17
No. of reflections8405
No. of parameters604
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.89, 0.75

Computer programs: SMART (Siemens, 1994), SMART and SAINT (Siemens, 1996), XPREP (Siemens, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

Selected geometric parameters (Å, º) top
Ru1—O12.012 (6)Sb—F41.719 (17)
Ru1—N72.048 (8)Sb—F31.781 (18)
Ru1—N32.054 (8)Sb—F61.820 (17)
Ru1—N12.056 (8)C44—C451.369 (17)
Ru1—N52.067 (9)C45—C461.366 (15)
Ru1—Ru22.2882 (11)C52—C531.422 (15)
Ru2—N82.007 (8)C83—C841.357 (19)
Ru2—N62.022 (8)C85—C861.385 (16)
O1—Ru1—N791.3 (3)C76—N8—C81119.6 (8)
N7—Ru1—N387.9 (3)H02A—C02—H02B109.5
N3—Ru1—N190.3 (3)O02—C03—C04109.0 (19)
N1—Ru1—N591.4 (3)N1—C12—C13123.5 (11)
N7—Ru1—Ru289.8 (2)C14—C15—C16119.1 (11)
N8—Ru2—N2179.2 (3)C23—C22—C21120.1 (11)
N2—Ru2—N489.6 (3)C43—C42—C41121.0 (11)
N4—Ru2—Ru189.5 (2)C46—C45—C44120.8 (11)
F4—Sb—F591.6 (10)C54—C53—C52120.9 (13)
F4—Sb—F283.8 (11)C64—C63—C62120.2 (14)
F4—Sb—F6167.6 (12)C74—C75—C76117.9 (12)
C12—N1—Ru1121.9 (7)C83—C82—C81119.6 (12)
C36—N4—Ru2120.8 (6)C84—C85—C86120.4 (13)
C52—N6—Ru2120.5 (7)
 

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