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Acta Cryst. (2008). E64, m442-m443    [ doi:10.1107/S1600536808003188 ]

cis,trans-Dicarbonyldichlorido[2-(2-pyridyl)-1,8-naphthyridine-[kappa]N1,N2]ruthenium(II)

D. Oyama and T. Hamada

Abstract top

The asymmetric unit of the title compound, [RuCl2(C13H9N3)(CO)2], consists of four crystallographically independent RuII complexes. Each RuII atom is in a distorted octahedral environment coordinated by two carbonyl ligands, two Cl atoms and a chelating 2-(2-pyridyl)-1,8-naphthyridine (pynp) ligand. The carbonyl ligands are cis to each other, while the Cl atoms are trans. Relatively short interatomic distances (2.60-2.67 Å) between the uncoordinated N atom of pynp and the C atom of the carbonyl imply a donor-acceptor interaction between the pynp and carbonyl ligands.

Comment top

[Ru(bpy)(CO)2Cl2] (bpy = 2,2'-bipyridine) is known as an excellent catalyst for the photochemical reduction of CO2 into formate (Lehn & Ziesel, 1990). On the other hand, some interesting redox properties of ruthenium polypyridyl complexes with a 1,8-naphthyridine (napy) as a redox active ligand have been reported so far (Nakajima & Tanaka, 1995; Mizukawa et al., 1999; Tomon et al., 2005). In the present work, [Ru(pynp)(CO)2Cl2] [pynp = 2-(2-pyridyl)-1,8-naphthyridine] was newly prepared. Pynp (Campos-Fernandez et al., 2002) is a ligand which has the combined properties of 2,2'-bipyridine and 1,8-naphthyridine.

The crystal structure of the title compound contains four [Ru(pynp)(CO)2Cl2] complexes of crystallization in the asymmetric unit. The ruthenium(II) complex displays a cis orientation of the carbonyl ligands and a trans orientation of the chloro ligands (Fig. 1). Two Ru—C—O bond angles of the complex [173.4 (5)–177.7 (7)°] are nearly linear, and the C—O [1.126 (9)–1.150 (7) Å], Ru—Cl [2.3883 (13)–2.3996 (13) Å], Ru—N [2.113 (5)–2.160 (4) Å] distances are in the expected ranges (Table 1). On the other hand, the Ru—C bond distances [1.851 (6)–1.903 (7) Å] are longer than those of [Ru(bpy)(CO)2Cl2] [1.817 (8), 1.835 (17) Å; Haukka et al., 1995]. The naphthyridine moiety of the pynp ligand is directed toward the adjacent terminal carbonyl ligand. The relatively short interatomic distances between the non-bonded nitrogen atom of pynp and the carbon atom of one of carbonyls [2.60—2.67 Å] are comparable to that of [Ru(bpy)2(napy)(CO)]2+ [2.765 (7) Å; Tomon et al., 2005], which exhibits intramolecular metallacyclization between the non-bonded nitrogen atom of the napy ligand and the carbonyl carbon atom driven by the napy-based redox reaction.

Related literature top

For related synthetic details, see: Anderson et al. (1995); Campos-Fernandez et al. (2002). For related structures, see: Haukka et al. (1995); Tomon et al. (2005). For related literatures on the redox behaviors of ruthenium polypyridyl complexes with a 1,8-naphthyridine ligand, see: Nakajima & Tanaka (1995); Mizukawa et al. (1999); Tomon et al. (2005). For general background on the photochemical reduction of CO2, see: Lehn & Ziesel (1990).

Experimental top

A methanol solution (10 ml) containing [Ru(CO)2Cl2]n (31 mg) and pynp (30 mg) was refluxed for 1.5 h. The reaction mixture was then concentrated to 2 ml under reduced pressure. The yellow-green color precipitate was collected by filtration and washed with methanol and diethyl ether, and then dried under vacuum. Single crystals suitable for X-ray diffraction were prepared by the diffusion of diethyl ether into an acetonitrile solution of the complex over a week.

Refinement top

All H atoms were positioned geometrically (C—H = 0.95 Å) and refined as riding, with Uiso(H) = 1.2Ueq(C). Refinement was carried out using reflections with F2 > 0.0σ(F2).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2001); cell refinement: CrystalClear (Rigaku/MSC, 2001); data reduction: TEXSAN (Rigaku/MSC, 2000); program(s) used to solve structure: DIRDIF94 (Beurskens et al., 1994); program(s) used to refine structure: TEXSAN (Rigaku/MSC, 2000); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: CrystalStructure (Rigaku/MSC, 2004).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound, with atom labels and 50% probability displacement ellipsoids for non-H atoms. H atoms have been omitted for clarity.
cis,trans-Dicarbonyldichlorido[2-(2-pyridyl)-1,8-naphthyridine-\ κN1,N2]ruthenium(II) top
Crystal data top
[RuCl2(C13H9N3)(CO)2]F000 = 3424.00
Mr = 435.23Dx = 1.850 Mg m−3
Monoclinic, P21/nMo Kα radiation
λ = 0.71070 Å
Hall symbol: -P 2ynCell parameters from 13888 reflections
a = 16.6297 (14) Åθ = 3.1–27.5º
b = 21.6048 (14) ŵ = 1.36 mm−1
c = 19.0585 (16) ÅT = 173 (1) K
β = 114.082 (3)ºPrism, yellow–green
V = 6251.4 (9) Å30.20 × 0.20 × 0.20 mm
Z = 16
Data collection top
Rigaku/MSC Mercury CCD
diffractometer		12059 reflections with F2 > 2σ(F2)
Detector resolution: 14.62 pixels mm-1Rint = 0.063
ω scansθmax = 27.5º
Absorption correction: noneh = −21→21
49009 measured reflectionsk = −26→28
14039 independent reflectionsl = −24→24
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.078  w = 1/[0.001Fo2 + 3σ(Fo2) + 0.5]/(4Fo2)
wR(F2) = 0.152(Δ/σ)max = 0.001
S = 1.50Δρmax = 1.43 e Å−3
14038 reflectionsΔρmin = −1.40 e Å−3
829 parametersExtinction correction: none
Crystal data top
[RuCl2(C13H9N3)(CO)2]V = 6251.4 (9) Å3
Mr = 435.23Z = 16
Monoclinic, P21/nMo Kα
a = 16.6297 (14) ŵ = 1.36 mm−1
b = 21.6048 (14) ÅT = 173 (1) K
c = 19.0585 (16) Å0.20 × 0.20 × 0.20 mm
β = 114.082 (3)º
Data collection top
Rigaku/MSC Mercury CCD
diffractometer		14039 independent reflections
Absorption correction: none12059 reflections with F2 > 2σ(F2)
49009 measured reflectionsRint = 0.063
Refinement top
R[F2 > 2σ(F2)] = 0.078? restraints
wR(F2) = 0.152H-atom parameters constrained
S = 1.50Δρmax = 1.43 e Å−3
14038 reflectionsΔρmin = −1.40 e Å−3
829 parameters
Special details top

Refinement. Refinement using reflections with F2 > 2.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ru10.17626 (3)0.20501 (2)0.48235 (2)0.02146 (12)
Ru20.26702 (3)0.52889 (2)0.25696 (2)0.02210 (12)
Ru30.17269 (3)0.18945 (2)−0.02197 (2)0.02201 (12)
Ru40.24140 (3)0.52453 (2)−0.23420 (2)0.02233 (12)
Cl10.06386 (9)0.19503 (6)0.35501 (8)0.0272 (3)
Cl20.29508 (9)0.22208 (6)0.60516 (8)0.0303 (3)
Cl30.37956 (10)0.49259 (7)0.37431 (8)0.0325 (4)
Cl40.15511 (10)0.55566 (7)0.13358 (8)0.0313 (4)
Cl50.06215 (9)0.17790 (7)−0.15037 (8)0.0315 (4)
Cl60.29082 (9)0.20463 (6)0.10162 (8)0.0272 (3)
Cl70.13015 (10)0.55219 (6)−0.35724 (8)0.0315 (3)
Cl80.34896 (9)0.48759 (7)−0.11404 (8)0.0309 (3)
O10.0528 (3)0.1442 (2)0.5419 (2)0.0419 (14)
O20.2435 (3)0.07537 (19)0.4855 (2)0.0370 (13)
O30.1594 (3)0.5568 (2)0.3487 (2)0.0390 (13)
O40.3353 (3)0.6589 (2)0.2864 (2)0.0458 (15)
O50.0451 (3)0.1371 (2)0.0398 (2)0.0490 (15)
O60.2341 (3)0.0586 (2)−0.0194 (2)0.0459 (14)
O70.1349 (3)0.5783 (2)−0.1535 (2)0.0466 (15)
O80.3278 (3)0.6493 (2)−0.2133 (2)0.0496 (15)
N10.2545 (2)0.2500 (2)0.4331 (2)0.0235 (12)
N20.1470 (2)0.3014 (2)0.4864 (2)0.0217 (12)
N30.0393 (3)0.2824 (2)0.5304 (2)0.0273 (13)
N40.3478 (2)0.5031 (2)0.1998 (2)0.0242 (12)
N50.2342 (3)0.4342 (2)0.2289 (2)0.0221 (12)
N60.1209 (3)0.4358 (2)0.2691 (2)0.0270 (13)
N70.2548 (2)0.2286 (2)−0.0705 (2)0.0229 (12)
N80.1508 (2)0.2878 (2)−0.0192 (2)0.0225 (12)
N90.0415 (3)0.2756 (2)0.0245 (2)0.0338 (15)
N100.3154 (3)0.4833 (2)−0.2900 (2)0.0299 (14)
N110.1944 (3)0.4317 (2)−0.2534 (2)0.0237 (12)
N120.0846 (3)0.4522 (2)−0.2121 (2)0.0300 (14)
C10.0986 (4)0.1699 (2)0.5221 (3)0.0287 (16)
C20.2171 (3)0.1240 (2)0.4817 (3)0.0265 (16)
C30.3024 (3)0.2213 (2)0.4009 (3)0.0275 (16)
C40.3575 (3)0.2538 (3)0.3755 (3)0.0328 (17)
C50.3647 (3)0.3165 (3)0.3837 (3)0.0314 (17)
C60.3145 (3)0.3469 (2)0.4158 (3)0.0286 (16)
C70.2584 (3)0.3125 (2)0.4388 (3)0.0251 (15)
C80.1980 (3)0.3408 (2)0.4695 (3)0.0255 (15)
C90.1934 (4)0.4047 (2)0.4771 (3)0.0298 (16)
C100.1364 (4)0.4294 (2)0.5042 (3)0.0312 (16)
C110.0804 (3)0.3891 (2)0.5228 (3)0.0262 (15)
C120.0190 (4)0.4090 (2)0.5517 (3)0.0319 (16)
C13−0.0312 (3)0.3665 (3)0.5673 (3)0.0322 (17)
C14−0.0183 (3)0.3038 (3)0.5565 (3)0.0317 (17)
C150.0888 (3)0.3250 (2)0.5135 (3)0.0212 (14)
C160.1963 (4)0.5453 (2)0.3120 (3)0.0285 (16)
C170.3079 (4)0.6102 (2)0.2762 (3)0.0301 (17)
C180.3990 (3)0.5412 (2)0.1807 (3)0.0274 (15)
C190.4506 (3)0.5218 (3)0.1436 (3)0.0340 (17)
C200.4517 (4)0.4605 (3)0.1271 (3)0.0390 (19)
C210.3998 (4)0.4196 (2)0.1471 (3)0.0357 (18)
C220.3472 (3)0.4423 (2)0.1825 (3)0.0272 (15)
C230.2847 (3)0.4038 (2)0.2001 (3)0.0228 (14)
C240.2748 (4)0.3405 (2)0.1839 (3)0.0289 (16)
C250.2118 (4)0.3078 (2)0.1962 (3)0.0316 (17)
C260.1582 (4)0.3375 (2)0.2271 (3)0.0280 (16)
C270.0924 (4)0.3081 (2)0.2431 (3)0.0364 (18)
C280.0434 (4)0.3433 (3)0.2707 (3)0.0383 (19)
C290.0595 (4)0.4064 (3)0.2827 (3)0.0351 (18)
C300.1705 (3)0.4018 (2)0.2417 (3)0.0247 (15)
C310.0923 (4)0.1593 (2)0.0177 (3)0.0315 (17)
C320.2082 (4)0.1082 (2)−0.0216 (3)0.0285 (16)
C330.2991 (4)0.1963 (3)−0.1035 (3)0.0320 (17)
C340.3558 (4)0.2241 (3)−0.1298 (3)0.041 (2)
C350.3681 (4)0.2869 (3)−0.1227 (3)0.042 (2)
C360.3212 (4)0.3214 (3)−0.0905 (3)0.0381 (19)
C370.2633 (3)0.2914 (2)−0.0657 (3)0.0244 (15)
C380.2055 (3)0.3238 (2)−0.0365 (3)0.0254 (15)
C390.2083 (4)0.3883 (2)−0.0276 (3)0.0358 (18)
C400.1516 (4)0.4168 (2)−0.0026 (3)0.043 (2)
C410.0926 (4)0.3805 (3)0.0156 (3)0.0371 (18)
C420.0311 (5)0.4049 (3)0.0423 (3)0.047 (2)
C43−0.0223 (4)0.3649 (4)0.0575 (3)0.052 (2)
C44−0.0142 (4)0.3012 (3)0.0495 (3)0.045 (2)
C450.0930 (3)0.3147 (2)0.0063 (3)0.0261 (15)
C460.1725 (3)0.5554 (2)−0.1843 (3)0.0277 (16)
C470.2939 (4)0.6024 (3)−0.2205 (3)0.0332 (17)
C480.3730 (4)0.5126 (3)−0.3110 (3)0.041 (2)
C490.4207 (4)0.4819 (4)−0.3452 (3)0.051 (2)
C500.4124 (4)0.4188 (4)−0.3541 (4)0.058 (2)
C510.3538 (4)0.3882 (3)−0.3325 (3)0.049 (2)
C520.3036 (4)0.4213 (3)−0.3025 (3)0.0336 (17)
C530.2367 (3)0.3931 (2)−0.2814 (3)0.0265 (15)
C540.2144 (4)0.3291 (2)−0.2920 (3)0.0367 (18)
C550.1492 (4)0.3065 (2)−0.2738 (4)0.0398 (19)
C560.1030 (4)0.3463 (2)−0.2453 (3)0.0337 (17)
C570.0326 (4)0.3282 (3)−0.2259 (4)0.047 (2)
C58−0.0097 (4)0.3712 (3)−0.2026 (4)0.045 (2)
C590.0205 (4)0.4325 (3)−0.1949 (3)0.0374 (19)
C600.1265 (3)0.4096 (2)−0.2367 (3)0.0260 (15)
H10.29850.17750.39520.033*
H20.39030.23230.35240.039*
H30.40340.33900.36770.038*
H40.31820.39060.42220.034*
H50.23020.43110.46320.036*
H60.13410.47290.51060.037*
H70.01290.45180.56010.038*
H8−0.07430.37890.58520.039*
H9−0.05310.27440.56870.038*
H100.39990.58380.19330.033*
H110.48470.55070.12980.041*
H120.48740.44590.10240.047*
H130.40020.37660.13670.043*
H140.31200.32030.16430.035*
H150.20400.26490.18390.038*
H160.08210.26490.23490.044*
H17−0.00180.32460.28170.046*
H180.02410.42960.30170.042*
H190.29090.1528−0.10890.038*
H200.38630.2000−0.15280.049*
H210.40810.3066−0.13950.050*
H220.32860.3650−0.08540.046*
H230.24950.4121−0.03900.043*
H240.15190.46060.00240.051*
H250.02750.44820.04940.056*
H26−0.06560.38020.07360.063*
H27−0.05110.27450.06290.054*
H280.38150.5558−0.30210.050*
H290.45860.5042−0.36240.062*
H300.44690.3965−0.37490.070*
H310.34760.3446−0.33810.059*
H320.24530.3021−0.31180.044*
H330.13480.2637−0.28030.048*
H340.01550.2860−0.22920.056*
H35−0.05880.3603−0.19170.054*
H36−0.00790.4620−0.17580.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.0231 (2)0.0193 (2)0.0243 (2)0.00155 (18)0.0120 (2)0.00087 (18)
Ru20.0253 (2)0.0177 (2)0.0249 (2)0.00077 (18)0.0119 (2)−0.00137 (18)
Ru30.0232 (2)0.0202 (2)0.0247 (2)0.00118 (18)0.0120 (2)0.00049 (19)
Ru40.0232 (2)0.0211 (2)0.0242 (2)−0.00135 (18)0.0112 (2)−0.00071 (18)
Cl10.0265 (7)0.0283 (7)0.0276 (7)−0.0001 (5)0.0117 (6)0.0016 (6)
Cl20.0304 (8)0.0308 (7)0.0272 (7)0.0050 (6)0.0094 (6)−0.0026 (6)
Cl30.0310 (8)0.0315 (7)0.0306 (8)−0.0013 (6)0.0080 (6)0.0037 (6)
Cl40.0304 (8)0.0338 (8)0.0299 (8)0.0044 (6)0.0125 (6)0.0054 (6)
Cl50.0285 (7)0.0334 (7)0.0306 (8)−0.0013 (6)0.0099 (6)0.0015 (6)
Cl60.0270 (7)0.0267 (7)0.0276 (7)0.0037 (5)0.0107 (6)−0.0029 (5)
Cl70.0298 (7)0.0307 (7)0.0301 (8)0.0007 (6)0.0084 (6)0.0035 (6)
Cl80.0280 (7)0.0340 (7)0.0285 (8)−0.0010 (6)0.0093 (6)0.0036 (6)
O10.045 (2)0.035 (2)0.059 (3)−0.001 (2)0.036 (2)0.013 (2)
O20.048 (2)0.022 (2)0.043 (2)0.011 (2)0.021 (2)0.0034 (19)
O30.050 (2)0.033 (2)0.050 (2)−0.005 (2)0.036 (2)−0.012 (2)
O40.073 (3)0.024 (2)0.058 (3)−0.013 (2)0.044 (2)−0.009 (2)
O50.040 (2)0.057 (3)0.061 (3)−0.004 (2)0.031 (2)0.023 (2)
O60.061 (3)0.027 (2)0.042 (2)0.012 (2)0.012 (2)0.001 (2)
O70.043 (2)0.049 (3)0.055 (3)−0.004 (2)0.028 (2)−0.024 (2)
O80.064 (3)0.034 (2)0.050 (3)−0.021 (2)0.022 (2)−0.001 (2)
N10.020 (2)0.027 (2)0.026 (2)0.000 (2)0.011 (2)0.000 (2)
N20.021 (2)0.020 (2)0.025 (2)0.0022 (18)0.010 (2)−0.0024 (19)
N30.028 (2)0.028 (2)0.027 (2)0.003 (2)0.012 (2)−0.001 (2)
N40.024 (2)0.023 (2)0.028 (2)0.002 (2)0.013 (2)−0.001 (2)
N50.026 (2)0.018 (2)0.021 (2)0.0011 (19)0.008 (2)0.0019 (19)
N60.025 (2)0.027 (2)0.031 (2)−0.001 (2)0.012 (2)0.000 (2)
N70.019 (2)0.031 (2)0.017 (2)0.003 (2)0.006 (2)0.000 (2)
N80.019 (2)0.023 (2)0.023 (2)0.0040 (19)0.007 (2)−0.0005 (19)
N90.022 (2)0.049 (3)0.032 (2)0.004 (2)0.012 (2)−0.007 (2)
N100.017 (2)0.049 (3)0.025 (2)0.007 (2)0.011 (2)0.002 (2)
N110.027 (2)0.023 (2)0.021 (2)−0.001 (2)0.009 (2)−0.0041 (19)
N120.030 (2)0.029 (2)0.036 (2)−0.002 (2)0.019 (2)0.002 (2)
C10.035 (3)0.027 (3)0.028 (3)0.008 (2)0.018 (2)0.006 (2)
C20.025 (3)0.031 (3)0.022 (3)−0.002 (2)0.008 (2)0.004 (2)
C30.022 (3)0.032 (3)0.031 (3)0.003 (2)0.014 (2)0.001 (2)
C40.024 (3)0.048 (4)0.030 (3)0.008 (2)0.015 (2)0.002 (2)
C50.017 (2)0.050 (3)0.025 (3)−0.004 (2)0.007 (2)0.009 (2)
C60.025 (3)0.034 (3)0.024 (3)−0.001 (2)0.007 (2)0.003 (2)
C70.023 (3)0.025 (2)0.029 (3)0.000 (2)0.012 (2)0.002 (2)
C80.023 (3)0.028 (3)0.025 (3)−0.003 (2)0.009 (2)0.002 (2)
C90.033 (3)0.023 (3)0.033 (3)−0.003 (2)0.014 (2)0.001 (2)
C100.038 (3)0.020 (2)0.033 (3)0.003 (2)0.013 (3)−0.003 (2)
C110.020 (2)0.029 (3)0.025 (3)0.004 (2)0.004 (2)0.000 (2)
C120.033 (3)0.030 (3)0.027 (3)0.013 (2)0.006 (2)−0.002 (2)
C130.026 (3)0.041 (3)0.032 (3)0.004 (2)0.013 (2)−0.005 (2)
C140.024 (3)0.042 (3)0.032 (3)−0.003 (2)0.016 (2)−0.004 (2)
C150.017 (2)0.024 (2)0.020 (2)0.004 (2)0.005 (2)0.000 (2)
C160.035 (3)0.020 (2)0.025 (3)−0.004 (2)0.007 (2)−0.003 (2)
C170.037 (3)0.026 (3)0.036 (3)0.001 (2)0.024 (3)−0.003 (2)
C180.025 (3)0.024 (2)0.031 (3)0.000 (2)0.008 (2)0.003 (2)
C190.021 (3)0.040 (3)0.044 (3)−0.002 (2)0.017 (2)0.004 (3)
C200.030 (3)0.049 (4)0.046 (4)−0.003 (3)0.024 (3)−0.011 (3)
C210.036 (3)0.031 (3)0.046 (4)0.003 (2)0.023 (3)−0.002 (3)
C220.027 (3)0.025 (3)0.026 (3)0.000 (2)0.009 (2)−0.003 (2)
C230.031 (3)0.019 (2)0.018 (2)0.006 (2)0.010 (2)0.000 (2)
C240.034 (3)0.023 (2)0.028 (3)0.001 (2)0.011 (2)−0.002 (2)
C250.043 (3)0.022 (3)0.026 (3)−0.004 (2)0.009 (3)−0.003 (2)
C260.035 (3)0.024 (2)0.021 (3)0.000 (2)0.008 (2)0.005 (2)
C270.040 (3)0.027 (3)0.041 (3)−0.007 (2)0.015 (3)0.002 (2)
C280.032 (3)0.042 (3)0.044 (4)−0.006 (3)0.018 (3)0.006 (3)
C290.034 (3)0.036 (3)0.039 (3)−0.003 (2)0.018 (3)0.006 (2)
C300.025 (3)0.027 (3)0.020 (3)0.001 (2)0.008 (2)0.003 (2)
C310.028 (3)0.035 (3)0.026 (3)0.001 (2)0.005 (2)0.005 (2)
C320.034 (3)0.027 (3)0.021 (3)−0.002 (2)0.007 (2)0.000 (2)
C330.029 (3)0.043 (3)0.024 (3)0.011 (2)0.010 (2)0.000 (2)
C340.026 (3)0.071 (5)0.027 (3)0.020 (3)0.013 (2)0.007 (3)
C350.028 (3)0.065 (5)0.042 (4)−0.001 (3)0.023 (3)0.015 (3)
C360.023 (3)0.052 (4)0.037 (3)−0.007 (2)0.010 (3)0.010 (3)
C370.022 (2)0.031 (3)0.018 (2)−0.001 (2)0.005 (2)0.003 (2)
C380.023 (3)0.025 (2)0.025 (3)−0.003 (2)0.007 (2)−0.002 (2)
C390.038 (3)0.029 (3)0.036 (3)0.002 (2)0.009 (3)0.002 (2)
C400.054 (4)0.024 (3)0.043 (4)0.010 (3)0.013 (3)−0.002 (3)
C410.037 (3)0.037 (3)0.030 (3)0.014 (3)0.006 (3)−0.005 (2)
C420.051 (4)0.052 (4)0.031 (3)0.028 (3)0.010 (3)−0.004 (3)
C430.036 (4)0.085 (6)0.031 (4)0.033 (4)0.008 (3)−0.006 (3)
C440.024 (3)0.078 (5)0.031 (3)0.005 (3)0.009 (3)−0.013 (3)
C450.021 (2)0.031 (3)0.024 (3)0.008 (2)0.007 (2)−0.004 (2)
C460.030 (3)0.021 (2)0.031 (3)−0.004 (2)0.011 (2)−0.002 (2)
C470.031 (3)0.041 (3)0.023 (3)0.001 (2)0.006 (2)0.004 (2)
C480.029 (3)0.065 (4)0.029 (3)0.005 (3)0.012 (3)0.011 (3)
C490.030 (3)0.100 (7)0.029 (3)0.009 (4)0.017 (3)0.013 (4)
C500.035 (4)0.106 (7)0.035 (4)0.021 (4)0.015 (3)−0.009 (4)
C510.044 (4)0.067 (5)0.041 (4)0.015 (3)0.021 (3)−0.009 (3)
C520.026 (3)0.044 (3)0.026 (3)0.011 (2)0.005 (2)−0.008 (2)
C530.030 (3)0.026 (3)0.020 (3)0.011 (2)0.007 (2)0.002 (2)
C540.045 (4)0.028 (3)0.025 (3)0.014 (2)0.002 (3)−0.009 (2)
C550.035 (3)0.024 (3)0.049 (4)−0.003 (2)0.005 (3)−0.006 (3)
C560.038 (3)0.017 (2)0.035 (3)−0.006 (2)0.004 (3)0.002 (2)
C570.034 (4)0.034 (3)0.060 (4)−0.007 (3)0.006 (3)0.020 (3)
C580.031 (3)0.044 (4)0.065 (5)0.002 (3)0.024 (3)0.024 (3)
C590.030 (3)0.041 (3)0.046 (4)0.003 (2)0.020 (3)0.012 (3)
C600.029 (3)0.022 (2)0.021 (3)−0.005 (2)0.004 (2)0.000 (2)
Geometric parameters (Å, °) top
Ru1—Cl12.3933 (12)C20—C211.392 (10)
Ru1—Cl22.3968 (13)C21—C221.394 (10)
Ru1—N12.124 (5)C22—C231.474 (9)
Ru1—N22.148 (4)C23—C241.398 (7)
Ru1—C11.901 (7)C24—C251.361 (10)
Ru1—C21.880 (6)C25—C261.408 (10)
Ru2—Cl32.3883 (13)C26—C271.401 (10)
Ru2—Cl42.3992 (13)C26—C301.416 (8)
Ru2—N42.121 (5)C27—C281.365 (11)
Ru2—N52.129 (4)C28—C291.390 (9)
Ru2—C161.903 (7)C33—C341.375 (11)
Ru2—C171.865 (6)C34—C351.369 (11)
Ru3—Cl52.3996 (13)C35—C361.389 (11)
Ru3—Cl62.3955 (12)C36—C371.394 (10)
Ru3—N72.113 (5)C37—C381.469 (9)
Ru3—N82.160 (4)C38—C391.403 (8)
Ru3—C311.900 (7)C39—C401.365 (11)
Ru3—C321.851 (6)C40—C411.406 (11)
Ru4—Cl72.3955 (13)C41—C421.416 (12)
Ru4—Cl82.3953 (13)C41—C451.434 (9)
Ru4—N102.124 (5)C42—C431.352 (12)
Ru4—N112.128 (4)C43—C441.396 (12)
Ru4—C461.884 (7)C48—C491.383 (12)
Ru4—C471.863 (6)C49—C501.375 (14)
O1—C11.126 (9)C50—C511.372 (13)
O2—C21.129 (7)C51—C521.387 (11)
O3—C161.129 (9)C52—C531.462 (10)
O4—C171.131 (7)C53—C541.425 (8)
O5—C311.136 (9)C54—C551.358 (11)
O6—C321.150 (7)C55—C561.401 (10)
O7—C461.132 (9)C56—C571.419 (11)
O8—C471.140 (8)C56—C601.415 (8)
N1—C31.340 (9)C57—C581.344 (11)
N1—C71.354 (7)C58—C591.402 (9)
N2—C81.331 (8)C3—H10.950
N2—C151.368 (8)C4—H20.950
N3—C141.329 (9)C5—H30.950
N3—C151.357 (8)C6—H40.950
N4—C181.337 (8)C9—H50.950
N4—C221.352 (7)C10—H60.950
N5—C231.345 (8)C12—H70.950
N5—C301.373 (8)C13—H80.950
N6—C291.314 (9)C14—H90.950
N6—C301.357 (8)C18—H100.950
N7—C331.344 (9)C19—H110.950
N7—C371.363 (7)C20—H120.950
N8—C381.335 (8)C21—H130.950
N8—C451.372 (8)C24—H140.950
N9—C441.324 (10)C25—H150.950
N9—C451.344 (9)C27—H160.950
N10—C481.339 (10)C28—H170.950
N10—C521.360 (8)C29—H180.950
N11—C531.336 (8)C33—H190.950
N11—C601.377 (9)C34—H200.950
N12—C591.308 (10)C35—H210.950
N12—C601.348 (8)C36—H220.950
C3—C41.389 (10)C39—H230.950
C4—C51.364 (9)C40—H240.950
C5—C61.386 (10)C42—H250.950
C6—C71.396 (9)C43—H260.950
C7—C81.485 (9)C44—H270.950
C8—C91.392 (8)C48—H280.950
C9—C101.359 (10)C49—H290.950
C10—C111.422 (9)C50—H300.950
C11—C121.411 (10)C51—H310.950
C11—C151.412 (8)C54—H320.950
C12—C131.354 (10)C55—H330.950
C13—C141.400 (9)C57—H340.950
C18—C191.380 (10)C58—H350.950
C19—C201.364 (9)C59—H360.950
Cl1—Ru1—Cl2174.66 (6)C25—C26—C30117.7 (6)
Cl1—Ru1—N187.63 (11)C27—C26—C30117.7 (6)
Cl1—Ru1—N291.66 (10)C26—C27—C28118.2 (5)
Cl1—Ru1—C189.55 (16)C27—C28—C29120.3 (7)
Cl1—Ru1—C292.51 (15)N6—C29—C28123.6 (7)
Cl2—Ru1—N187.24 (11)N5—C30—N6115.4 (5)
Cl2—Ru1—N285.67 (10)N5—C30—C26121.7 (6)
Cl2—Ru1—C195.47 (16)N6—C30—C26123.0 (6)
Cl2—Ru1—C289.65 (15)Ru3—C31—O5175.1 (6)
N1—Ru1—N276.2 (2)Ru3—C32—O6176.9 (5)
N1—Ru1—C1175.1 (2)N7—C33—C34122.2 (6)
N1—Ru1—C297.7 (2)C33—C34—C35119.5 (7)
N2—Ru1—C199.9 (2)C34—C35—C36119.2 (7)
N2—Ru1—C2172.5 (2)C35—C36—C37119.3 (6)
C1—Ru1—C286.4 (2)N7—C37—C36120.5 (6)
Cl3—Ru2—Cl4174.31 (5)N7—C37—C38115.7 (5)
Cl3—Ru2—N488.64 (11)C36—C37—C38123.8 (5)
Cl3—Ru2—N586.68 (10)N8—C38—C37115.6 (5)
Cl3—Ru2—C1688.23 (16)N8—C38—C39122.8 (6)
Cl3—Ru2—C1792.39 (16)C37—C38—C39121.6 (6)
Cl4—Ru2—N487.73 (11)C38—C39—C40119.8 (6)
Cl4—Ru2—N588.21 (11)C39—C40—C41119.1 (6)
Cl4—Ru2—C1695.10 (16)C40—C41—C42124.1 (6)
Cl4—Ru2—C1792.31 (16)C40—C41—C45118.9 (7)
N4—Ru2—N576.7 (2)C42—C41—C45117.0 (6)
N4—Ru2—C16175.2 (2)C41—C42—C43118.2 (7)
N4—Ru2—C1795.3 (2)C42—C43—C44120.3 (8)
N5—Ru2—C1699.5 (2)N9—C44—C43124.3 (7)
N5—Ru2—C17171.9 (2)N8—C45—N9115.9 (5)
C16—Ru2—C1788.6 (3)N8—C45—C41120.3 (6)
Cl5—Ru3—Cl6175.22 (6)N9—C45—C41123.7 (6)
Cl5—Ru3—N787.61 (11)Ru4—C46—O7174.4 (5)
Cl5—Ru3—N893.47 (10)Ru4—C47—O8177.7 (7)
Cl5—Ru3—C3189.95 (16)N10—C48—C49122.1 (7)
Cl5—Ru3—C3290.91 (16)C48—C49—C50119.0 (8)
Cl6—Ru3—N787.61 (11)C49—C50—C51119.2 (8)
Cl6—Ru3—N885.42 (10)C50—C51—C52119.8 (7)
Cl6—Ru3—C3194.82 (16)N10—C52—C51120.7 (6)
Cl6—Ru3—C3289.63 (15)N10—C52—C53115.7 (6)
N7—Ru3—N876.2 (2)C51—C52—C53123.6 (6)
N7—Ru3—C31175.4 (2)N11—C53—C52115.8 (5)
N7—Ru3—C3296.8 (2)N11—C53—C54120.9 (6)
N8—Ru3—C31100.1 (2)C52—C53—C54123.3 (6)
N8—Ru3—C32171.6 (2)C53—C54—C55120.1 (6)
C31—Ru3—C3287.1 (3)C54—C55—C56120.0 (5)
Cl7—Ru4—Cl8174.97 (5)C55—C56—C57125.0 (5)
Cl7—Ru4—N1089.32 (12)C55—C56—C60118.0 (6)
Cl7—Ru4—N1189.08 (11)C57—C56—C60116.9 (6)
Cl7—Ru4—C4691.14 (16)C56—C57—C58119.7 (6)
Cl7—Ru4—C4792.41 (16)C57—C58—C59118.2 (7)
Cl8—Ru4—N1088.85 (12)N12—C59—C58125.1 (7)
Cl8—Ru4—N1185.94 (11)N11—C60—N12115.6 (5)
Cl8—Ru4—C4690.35 (16)N11—C60—C56121.5 (6)
Cl8—Ru4—C4792.45 (16)N12—C60—C56122.9 (6)
N10—Ru4—N1176.5 (2)N1—C3—H1119.1
N10—Ru4—C46175.9 (2)C4—C3—H1119.1
N10—Ru4—C4796.6 (2)C3—C4—H2119.9
N11—Ru4—C4699.4 (2)C5—C4—H2119.9
N11—Ru4—C47172.9 (2)C4—C5—H3120.6
C46—Ru4—C4787.5 (3)C6—C5—H3120.6
Ru1—N1—C3125.2 (4)C5—C6—H4120.4
Ru1—N1—C7116.0 (4)C7—C6—H4120.4
C3—N1—C7118.7 (5)C8—C9—H5119.8
Ru1—N2—C8115.8 (4)C10—C9—H5119.8
Ru1—N2—C15125.5 (3)C9—C10—H6120.6
C8—N2—C15118.2 (4)C11—C10—H6120.6
C14—N3—C15116.9 (5)C11—C12—H7120.3
Ru2—N4—C18125.8 (4)C13—C12—H7120.4
Ru2—N4—C22115.9 (4)C12—C13—H8120.7
C18—N4—C22118.3 (5)C14—C13—H8120.7
Ru2—N5—C23115.6 (3)N3—C14—H9117.7
Ru2—N5—C30125.6 (4)C13—C14—H9117.7
C23—N5—C30118.7 (4)N4—C18—H10118.3
C29—N6—C30117.3 (5)C19—C18—H10118.3
Ru3—N7—C33124.9 (4)C18—C19—H11120.6
Ru3—N7—C37115.9 (4)C20—C19—H11120.6
C33—N7—C37119.1 (5)C19—C20—H12120.5
Ru3—N8—C38115.4 (4)C21—C20—H12120.5
Ru3—N8—C45125.1 (4)C20—C21—H13120.3
C38—N8—C45119.1 (5)C22—C21—H13120.3
C44—N9—C45116.3 (6)C23—C24—H14120.0
Ru4—N10—C48125.7 (4)C25—C24—H14120.0
Ru4—N10—C52115.4 (4)C24—C25—H15120.1
C48—N10—C52118.9 (6)C26—C25—H15120.1
Ru4—N11—C53116.1 (4)C26—C27—H16120.9
Ru4—N11—C60124.4 (4)C28—C27—H16120.9
C53—N11—C60119.4 (4)C27—C28—H17119.9
C59—N12—C60117.0 (5)C29—C28—H17119.8
Ru1—C1—O1173.4 (5)N6—C29—H18118.2
Ru1—C2—O2176.3 (5)C28—C29—H18118.2
N1—C3—C4121.7 (5)N7—C33—H19118.9
C3—C4—C5120.1 (6)C34—C33—H19118.9
C4—C5—C6118.7 (6)C33—C34—H20120.2
C5—C6—C7119.1 (5)C35—C34—H20120.2
N1—C7—C6121.5 (6)C34—C35—H21120.4
N1—C7—C8115.2 (5)C36—C35—H21120.4
C6—C7—C8123.3 (5)C35—C36—H22120.3
N2—C8—C7115.5 (5)C37—C36—H22120.3
N2—C8—C9122.8 (6)C38—C39—H23120.1
C7—C8—C9121.7 (6)C40—C39—H23120.1
C8—C9—C10120.4 (6)C39—C40—H24120.5
C9—C10—C11118.9 (5)C41—C40—H24120.4
C10—C11—C12124.3 (5)C41—C42—H25120.9
C10—C11—C15117.5 (6)C43—C42—H25120.9
C12—C11—C15118.2 (6)C42—C43—H26119.8
C11—C12—C13119.3 (5)C44—C43—H26119.8
C12—C13—C14118.6 (6)N9—C44—H27117.9
N3—C14—C13124.6 (6)C43—C44—H27117.9
N2—C15—N3115.4 (5)N10—C48—H28118.9
N2—C15—C11122.3 (5)C49—C48—H28118.9
N3—C15—C11122.3 (6)C48—C49—H29120.5
Ru2—C16—O3175.1 (4)C50—C49—H29120.5
Ru2—C17—O4177.0 (7)C49—C50—H30120.4
N4—C18—C19123.4 (5)C51—C50—H30120.4
C18—C19—C20118.8 (6)C50—C51—H31120.1
C19—C20—C21119.0 (7)C52—C51—H31120.1
C20—C21—C22119.4 (6)C53—C54—H32119.9
N4—C22—C21121.1 (6)C55—C54—H32119.9
N4—C22—C23115.3 (6)C54—C55—H33120.0
C21—C22—C23123.5 (5)C56—C55—H33120.0
N5—C23—C22115.7 (4)C56—C57—H34120.2
N5—C23—C24122.0 (6)C58—C57—H34120.2
C22—C23—C24122.2 (6)C57—C58—H35120.9
C23—C24—C25120.0 (6)C59—C58—H35120.9
C24—C25—C26119.9 (5)N12—C59—H36117.4
C25—C26—C27124.6 (5)C58—C59—H36117.4
Cl1—Ru1—N1—C3−81.7 (3)C45—N8—C38—C37−178.1 (4)
Cl1—Ru1—N1—C7101.7 (3)C45—N8—C38—C391.9 (7)
Cl1—Ru1—N2—C8−97.1 (3)C44—N9—C45—N8179.7 (4)
Cl1—Ru1—N2—C1591.4 (3)C44—N9—C45—C412.7 (7)
Cl2—Ru1—N1—C399.8 (3)C45—N9—C44—C430.2 (6)