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Acta Cryst. (2013). E69, m1-m2
https://doi.org/10.1107/S1600536812048246
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cis-Bis(2,2′-bipyridine-κ2N,N′)carbonyl­chloridoruthenium(II) hexa­fluorido­phosphate

T. Takase, B. Mun and D. Oyama
In the title compound, [RuCl(C10H8N2)2(CO)]PF6, the RuII atom is coordinated in a distorted octa­hedral geometry by four N atoms of the bipyridine ligands, a carbonyl C atom and a chloride ion. The carbonyl and chloride ligands in the cation adopt a mutually cis arrangement and these are disordered over two sets of sites with site occupancies of 0.721 (6) and 0.279 (6). The Ru—N bond length [2.117 (2) Å] trans to the carbonyl ligand is slightly longer than the average of the other Ru—N bond lengths (2.08 Å), which can be explained by the expected trans influence of the carbonyl group. In the crystal, weak C—H...F inter­actions are observed between the complex cation and the PF6− anion, leading to the formation of a three-dimensional supramolecular structure. The crystal studied was an inversion twin with twin fractions of 0.78 (4) and 0.22 (4).
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536812048246/is5220sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536812048246/is5220Isup2.hkl
Contains datablock I

CCDC reference: 920169

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 93 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in main residue
  • R factor = 0.032
  • wR factor = 0.062
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found




Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O1     --  C21     ..        5.5 su
PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          6
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          4
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1


Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.42
           From the CIF: _reflns_number_total               5177
           Count of symmetry unique reflns         2942
           Completeness (_total/calc)            175.97%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      2235
           Fraction of Friedel pairs measured     0.760
           Are heavy atom types Z>Si present        yes
PLAT005_ALERT_5_G No _iucr_refine_instructions_details  in the CIF          ?
PLAT033_ALERT_4_G Flack x Value Deviates .gt. 2*sigma from Zero ..      0.220
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ru1    --  Cl1     ..        8.6 su
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ru1    --  C21     ..        5.5 su
PLAT301_ALERT_3_G Note: Main Residue  Disorder ...................         11 Perc.
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          6


   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   7 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check
Comment top

Ruthenium(II) complexes containing both carbonyl and polypyridyl-based supporting ligands have been studied as catalysts for the reduction of carbon dioxide and in the water-gas shift reaction (Ishida et al., 1986; Lehn & Ziessel, 1990). Of the series complexes, [Ru(bpy)2(CO)Cl]+ (bpy = 2,2'-bipyridine) has been used not only as catalysts but also as a precursor to a family of [Ru(bpy)2(CO)L]n+-type complexes (L = monodentate ligand). We have used the complex as the starting point for the preparation of more complex functional systems, and we report here the crystal structure of its hexafluoridophosphate salt.

The RuII atom has a distorted octahedral geometry, with four N atoms of the bidentate bipyridine ligands, a carbonyl carbon, and a chloride ion completing the first coordination sphere. The CO and Cl ligands in the cation are mutually cis arrangement (Fig. 1) and these are disordered over two sets of sites with site occupancies of 0.721 (6) and 0.279 (6). The Ru—N length trans to the CO ligand [2.117 (2) Å] is slightly longer than the average of other Ru—N lengths (2.08 Å) (Table 1). This can be explained by the expected trans influence of the CO group. In the crystal, the complex cation and the PF6- anion are linked via a number of weak C—H···F interactions, leading to the formation of a three-dimensional supramolecular structure. The crystal studied was an inversion twin with twin fractions of 0.78 (4) and 0.22 (4). The bond parameters of the complex are closely comparable to those of the reported ClO4- salt, although the corresponding ClO4- salt was refined using anisotropic temperature factors for Ru and Cl only (Clear et al., 1980).

Related literature top

For details of the synthesis, see: Oyama et al. (2012). For a related structure, see: Clear et al. (1980). For general background to catalytic reactions using [Ru(bpy)2(CO)Cl]+, see: Ishida et al. (1986); Lehn & Ziessel (1990).

Experimental top

The title compound was prepared according to a literature procedure (Oyama et al., 2012). X-ray quality crystals were grown by the diffusion of diethyl ether into an acetone solution of the complex over a week.

Refinement top

Aromatic H atoms were fixed at C—H distances of 0.95 Å and refined as riding, with Uiso(H) = 1.2Ueq(C). The C and O atoms in the CO group and the Cl atom are disordered over two sets of sites, occupancies refining to 0.721 (6) and complement. Both the highest residual electron density peak and the deepest hole are located within 1 Å from atom Ru1. The Hooft y parameter was 0.228 (15).

Structure description top

Ruthenium(II) complexes containing both carbonyl and polypyridyl-based supporting ligands have been studied as catalysts for the reduction of carbon dioxide and in the water-gas shift reaction (Ishida et al., 1986; Lehn & Ziessel, 1990). Of the series complexes, [Ru(bpy)2(CO)Cl]+ (bpy = 2,2'-bipyridine) has been used not only as catalysts but also as a precursor to a family of [Ru(bpy)2(CO)L]n+-type complexes (L = monodentate ligand). We have used the complex as the starting point for the preparation of more complex functional systems, and we report here the crystal structure of its hexafluoridophosphate salt.

The RuII atom has a distorted octahedral geometry, with four N atoms of the bidentate bipyridine ligands, a carbonyl carbon, and a chloride ion completing the first coordination sphere. The CO and Cl ligands in the cation are mutually cis arrangement (Fig. 1) and these are disordered over two sets of sites with site occupancies of 0.721 (6) and 0.279 (6). The Ru—N length trans to the CO ligand [2.117 (2) Å] is slightly longer than the average of other Ru—N lengths (2.08 Å) (Table 1). This can be explained by the expected trans influence of the CO group. In the crystal, the complex cation and the PF6- anion are linked via a number of weak C—H···F interactions, leading to the formation of a three-dimensional supramolecular structure. The crystal studied was an inversion twin with twin fractions of 0.78 (4) and 0.22 (4). The bond parameters of the complex are closely comparable to those of the reported ClO4- salt, although the corresponding ClO4- salt was refined using anisotropic temperature factors for Ru and Cl only (Clear et al., 1980).

For details of the synthesis, see: Oyama et al. (2012). For a related structure, see: Clear et al. (1980). For general background to catalytic reactions using [Ru(bpy)2(CO)Cl]+, see: Ishida et al. (1986); Lehn & Ziessel (1990).

Computing details top

Data collection: CrystalClear-SM (Rigaku, 2009); cell refinement: CrystalClear-SM (Rigaku, 2009); data reduction: CrystalClear-SM (Rigaku, 2009); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012); software used to prepare material for publication: CrystalStructure (Rigaku, 2006).

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. Only major component of the disordered CO and Cl ligands is shown.
cis-Bis(2,2'-bipyridine- κ2N,N')carbonylchloridoruthenium(II) hexafluoridophosphate top
Crystal data top
[RuCl(C10H8N2)2(CO)]·PF6F(000) = 1232.00
Mr = 621.87Dx = 1.807 Mg m−3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71075 Å
Hall symbol: P 2ac 2abCell parameters from 6659 reflections
a = 10.882 (5) Åθ = 3.4–27.4°
b = 12.063 (5) ŵ = 0.95 mm−1
c = 17.410 (7) ÅT = 93 K
V = 2285.2 (17) Å3Block, orange
Z = 40.20 × 0.10 × 0.02 mm
Data collection top
Rigaku Saturn
diffractometer		4689 reflections with F2 > 2σ(F2)
Detector resolution: 7.31 pixels mm-1Rint = 0.045
ω scansθmax = 27.4°
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		h = −14→14
Tmin = 0.897, Tmax = 0.981k = −15→15
22875 measured reflectionsl = −22→22
5177 independent reflections
Refinement top
Refinement on F2 w = 1/[σ2(Fo2) + (0.0116P)2 + 2.2808P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.032(Δ/σ)max = 0.001
wR(F2) = 0.062Δρmax = 1.37 e Å−3
S = 1.08Δρmin = −1.28 e Å−3
5177 reflectionsAbsolute structure: Flack (1983), 2249 Friedel pairs
330 parametersAbsolute structure parameter: 0.22 (4)
H-atom parameters constrained
Crystal data top
[RuCl(C10H8N2)2(CO)]·PF6V = 2285.2 (17) Å3
Mr = 621.87Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 10.882 (5) ŵ = 0.95 mm−1
b = 12.063 (5) ÅT = 93 K
c = 17.410 (7) Å0.20 × 0.10 × 0.02 mm
Data collection top
Rigaku Saturn
diffractometer		5177 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		4689 reflections with F2 > 2σ(F2)
Tmin = 0.897, Tmax = 0.981Rint = 0.045
22875 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.062Δρmax = 1.37 e Å−3
S = 1.08Δρmin = −1.28 e Å−3
5177 reflectionsAbsolute structure: Flack (1983), 2249 Friedel pairs
330 parametersAbsolute structure parameter: 0.22 (4)
Special details top

Refinement. Refinement was performed using all reflections. 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*/UeqOcc. (<1)
Ru10.02797 (3)0.23729 (2)0.135509 (15)0.01786 (6)
Cl1−0.09514 (14)0.07702 (15)0.13630 (11)0.0212 (5)0.721 (6)
Cl20.1924 (6)0.1234 (4)0.1216 (3)0.0179 (16)*0.279 (6)
P10.43909 (9)0.30250 (7)0.35040 (5)0.0207 (2)
F10.3130 (2)0.35010 (18)0.38378 (14)0.0404 (6)
F20.56516 (17)0.25391 (18)0.31614 (11)0.0265 (4)
F30.4530 (2)0.41078 (15)0.29742 (11)0.0267 (4)
F40.5138 (2)0.36277 (16)0.41762 (12)0.0366 (6)
F50.4261 (2)0.19318 (16)0.40319 (12)0.0366 (6)
F60.36435 (17)0.24099 (19)0.28323 (11)0.0254 (4)
O10.2506 (4)0.0882 (3)0.1258 (2)0.0295 (10)0.721 (6)
O2−0.1251 (10)0.0222 (11)0.1282 (6)0.027 (2)*0.279 (6)
N10.1347 (2)0.3805 (2)0.12773 (18)0.0172 (6)
N20.0354 (2)0.2586 (2)0.01763 (13)0.0158 (5)
N30.0041 (2)0.2422 (2)0.25340 (14)0.0159 (5)
N4−0.1287 (2)0.3405 (2)0.14489 (17)0.0168 (6)
C10.1837 (3)0.4363 (3)0.1868 (2)0.0207 (7)
C20.2568 (3)0.5285 (3)0.1763 (2)0.0226 (8)
C30.2804 (3)0.5650 (2)0.1025 (2)0.0230 (8)
C40.2297 (3)0.5082 (2)0.0408 (2)0.0200 (7)
C50.1558 (3)0.4162 (2)0.05464 (19)0.0153 (7)
C60.0964 (3)0.3508 (2)−0.00646 (19)0.0163 (7)
C70.0989 (3)0.3809 (2)−0.0836 (2)0.0183 (7)
C80.0351 (3)0.3163 (2)−0.1360 (2)0.0220 (6)
C9−0.0250 (3)0.2223 (2)−0.11146 (18)0.0203 (6)
C10−0.0236 (3)0.1960 (2)−0.03456 (19)0.0203 (7)
C110.0752 (3)0.1916 (2)0.3056 (2)0.0255 (8)
C120.0524 (3)0.1979 (2)0.3838 (2)0.0251 (8)
C13−0.0466 (3)0.2590 (3)0.40917 (18)0.0266 (7)
C14−0.1208 (3)0.3123 (2)0.3563 (2)0.0240 (7)
C15−0.0943 (3)0.3029 (2)0.27831 (19)0.0159 (7)
C16−0.1674 (3)0.3575 (2)0.2178 (2)0.0159 (7)
C17−0.2693 (3)0.4242 (2)0.2327 (2)0.0186 (7)
C18−0.3292 (3)0.4755 (2)0.1729 (2)0.0215 (8)
C19−0.2875 (3)0.4598 (3)0.0984 (2)0.0238 (8)
C20−0.1878 (3)0.3906 (3)0.0875 (2)0.0218 (8)
C210.1713 (8)0.1488 (6)0.1328 (5)0.0264 (19)0.721 (6)
C22−0.080 (2)0.1111 (17)0.1316 (15)0.033 (6)*0.279 (6)
H10.16740.41160.23760.025*
H20.29050.56640.21930.027*
H30.33070.62820.09400.028*
H40.24530.5319−0.01030.024*
H50.14340.4444−0.10000.022*
H60.03280.3368−0.18870.026*
H7−0.06680.1761−0.14710.024*
H8−0.06580.1315−0.01780.024*
H90.14390.14990.28840.031*
H100.10420.16060.41930.030*
H11−0.06370.26460.46260.032*
H12−0.18930.35480.37300.029*
H13−0.29710.43420.28400.022*
H14−0.39860.52120.18260.026*
H15−0.32620.49560.05620.029*
H16−0.16010.37810.03650.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.02530 (13)0.01498 (11)0.01331 (11)0.00333 (12)0.00509 (12)0.00234 (11)
Cl10.0230 (7)0.0190 (11)0.0215 (7)−0.0062 (6)−0.0010 (6)0.0016 (7)
P10.0266 (5)0.0181 (4)0.0175 (5)−0.0013 (3)0.0036 (3)−0.0010 (3)
F10.0323 (13)0.0377 (13)0.0512 (18)−0.0069 (10)0.0251 (11)−0.0185 (11)
F20.0229 (10)0.0255 (10)0.0311 (10)0.0082 (10)−0.0030 (8)0.0033 (10)
F30.0298 (13)0.0196 (9)0.0306 (12)0.0037 (9)0.0006 (9)0.0086 (8)
F40.0600 (17)0.0284 (10)0.0215 (11)−0.0152 (11)−0.0104 (11)−0.0022 (8)
F50.0713 (19)0.0218 (10)0.0167 (11)−0.0173 (11)0.0028 (11)0.0042 (8)
F60.0251 (10)0.0268 (11)0.0244 (10)−0.0022 (10)−0.0034 (8)−0.0066 (9)
O10.024 (2)0.026 (2)0.039 (2)0.0095 (19)−0.0004 (19)0.0067 (18)
N10.0216 (15)0.0180 (13)0.0121 (15)0.0040 (11)0.0011 (13)−0.0017 (12)
N20.0201 (14)0.0134 (12)0.0140 (12)−0.0018 (14)0.0044 (11)−0.0008 (10)
N30.0141 (14)0.0190 (13)0.0147 (12)−0.0027 (11)0.0012 (9)0.0025 (11)
N40.0239 (15)0.0151 (13)0.0116 (15)0.0003 (11)−0.0002 (13)−0.0018 (11)
C10.0169 (19)0.0297 (19)0.0153 (18)0.0050 (15)−0.0023 (14)−0.0040 (15)
C20.026 (2)0.020 (2)0.022 (2)0.0020 (16)−0.0089 (16)−0.0070 (15)
C30.024 (2)0.0150 (17)0.030 (2)−0.0003 (15)−0.0088 (16)−0.0019 (15)
C40.028 (2)0.0141 (17)0.0185 (18)−0.0008 (15)−0.0035 (15)0.0021 (13)
C50.0173 (18)0.0134 (16)0.0152 (17)0.0017 (13)−0.0033 (14)−0.0012 (13)
C60.0152 (17)0.0149 (16)0.0188 (18)0.0034 (13)0.0006 (13)−0.0007 (13)
C70.0173 (18)0.0190 (17)0.0186 (18)−0.0043 (14)−0.0007 (14)0.0027 (13)
C80.0235 (17)0.0278 (15)0.0146 (16)−0.0045 (15)−0.0016 (19)−0.0008 (14)
C90.0211 (16)0.0213 (15)0.0186 (16)−0.0009 (17)−0.0008 (14)−0.0059 (12)
C100.0223 (17)0.0141 (14)0.0243 (18)−0.0012 (16)0.0053 (16)−0.0044 (12)
C110.026 (2)0.0279 (19)0.0225 (19)0.0012 (16)−0.0009 (16)0.0075 (15)
C120.026 (2)0.0299 (18)0.0191 (19)−0.0031 (15)−0.0068 (14)0.0050 (13)
C130.038 (2)0.0280 (18)0.0140 (14)−0.0004 (19)−0.0012 (14)0.0008 (15)
C140.032 (2)0.0218 (16)0.0178 (18)0.0012 (14)0.0023 (17)−0.0022 (15)
C150.0179 (17)0.0160 (15)0.0140 (16)−0.0010 (13)0.0012 (13)0.0013 (12)
C160.0179 (18)0.0130 (16)0.0167 (17)−0.0040 (13)−0.0010 (13)−0.0008 (12)
C170.0165 (17)0.0177 (17)0.0216 (19)−0.0022 (13)0.0038 (14)−0.0015 (14)
C180.0165 (19)0.0169 (17)0.031 (2)0.0016 (15)0.0014 (16)0.0010 (15)
C190.021 (2)0.0210 (18)0.029 (2)0.0009 (15)−0.0025 (17)0.0074 (16)
C200.023 (2)0.0237 (19)0.0193 (19)0.0031 (15)−0.0012 (15)0.0017 (15)
C210.042 (5)0.015 (3)0.022 (3)−0.008 (3)−0.001 (3)0.006 (3)
Geometric parameters (Å, º) top
Ru1—Cl12.3521 (17)C6—C71.391 (4)
Ru1—Cl22.269 (6)C7—C81.387 (4)
Ru1—N12.086 (2)C8—C91.377 (4)
Ru1—N22.070 (2)C9—C101.376 (4)
Ru1—N32.070 (2)C11—C121.385 (5)
Ru1—N42.117 (2)C12—C131.378 (5)
Ru1—C211.890 (8)C13—C141.382 (4)
Ru1—C221.93 (2)C14—C151.393 (4)
P1—F11.597 (2)C15—C161.476 (4)
P1—F21.607 (2)C16—C171.394 (4)
P1—F31.606 (2)C17—C181.376 (5)
P1—F41.600 (2)C18—C191.387 (5)
P1—F51.614 (2)C19—C201.382 (5)
P1—F61.606 (2)C1—H10.950
O1—C211.138 (9)C2—H20.950
O2—C221.18 (2)C3—H30.950
N1—C11.339 (4)C4—H40.950
N1—C51.363 (4)C7—H50.950
N2—C61.362 (4)C8—H60.950
N2—C101.344 (4)C9—H70.950
N3—C111.341 (4)C10—H80.950
N3—C151.368 (4)C11—H90.950
N4—C161.353 (4)C12—H100.950
N4—C201.334 (4)C13—H110.950
C1—C21.380 (5)C14—H120.950
C2—C31.383 (5)C17—H130.950
C3—C41.388 (5)C18—H140.950
C4—C51.391 (4)C19—H150.950
C5—C61.474 (4)C20—H160.950
Cl1—Ru1—N1176.52 (9)C4—C5—C6123.7 (3)
Cl1—Ru1—N297.47 (8)N2—C6—C5115.4 (2)
Cl1—Ru1—N386.91 (8)N2—C6—C7121.3 (2)
Cl1—Ru1—N491.41 (8)C5—C6—C7123.3 (2)
Cl1—Ru1—C2190.3 (2)C6—C7—C8118.6 (3)
Cl2—Ru1—N193.18 (18)C7—C8—C9119.7 (3)
Cl2—Ru1—N286.45 (17)C8—C9—C10119.1 (3)
Cl2—Ru1—N3102.85 (17)N2—C10—C9122.3 (2)
Cl2—Ru1—N4177.80 (17)N3—C11—C12122.5 (3)
Cl2—Ru1—C2290.0 (6)C11—C12—C13119.0 (3)
N1—Ru1—N279.12 (11)C12—C13—C14119.5 (3)
N1—Ru1—N396.35 (11)C13—C14—C15119.3 (3)
N1—Ru1—N488.06 (10)N3—C15—C14121.0 (2)
N1—Ru1—C2190.4 (2)N3—C15—C16115.8 (2)
N1—Ru1—C22173.1 (7)C14—C15—C16123.2 (3)
N2—Ru1—N3169.95 (10)N4—C16—C15115.7 (2)
N2—Ru1—N492.01 (11)N4—C16—C17120.7 (3)
N2—Ru1—C2190.8 (2)C15—C16—C17123.6 (3)
N2—Ru1—C2295.0 (7)C16—C17—C18119.7 (3)
N3—Ru1—N478.80 (10)C17—C18—C19119.4 (3)
N3—Ru1—C2198.3 (2)C18—C19—C20117.9 (3)
N3—Ru1—C2288.9 (7)N4—C20—C19123.3 (3)
N4—Ru1—C21176.5 (2)Ru1—C21—O1172.4 (7)
N4—Ru1—C2288.6 (6)Ru1—C22—O2166.8 (18)
F1—P1—F2179.39 (12)N1—C1—H1118.9
F1—P1—F389.87 (11)C2—C1—H1118.9
F1—P1—F490.40 (13)C1—C2—H2120.5
F1—P1—F590.64 (13)C3—C2—H2120.5
F1—P1—F689.76 (11)C2—C3—H3120.4
F2—P1—F390.16 (11)C4—C3—H3120.4
F2—P1—F490.20 (12)C3—C4—H4120.4
F2—P1—F589.32 (12)C5—C4—H4120.4
F2—P1—F689.63 (10)C6—C7—H5120.7
F3—P1—F490.14 (10)C8—C7—H5120.7
F3—P1—F5179.47 (13)C7—C8—H6120.1
F3—P1—F690.31 (11)C9—C8—H6120.1
F4—P1—F589.96 (11)C8—C9—H7120.4
F4—P1—F6179.52 (12)C10—C9—H7120.4
F5—P1—F689.58 (11)N2—C10—H8118.9
Ru1—N1—C1126.0 (2)C9—C10—H8118.9
Ru1—N1—C5114.6 (2)N3—C11—H9118.8
C1—N1—C5119.4 (2)C12—C11—H9118.7
Ru1—N2—C6115.2 (2)C11—C12—H10120.5
Ru1—N2—C10125.6 (2)C13—C12—H10120.5
C6—N2—C10118.9 (2)C12—C13—H11120.3
Ru1—N3—C11126.0 (2)C14—C13—H11120.3
Ru1—N3—C15115.3 (2)C13—C14—H12120.3
C11—N3—C15118.7 (2)C15—C14—H12120.3
Ru1—N4—C16114.4 (2)C16—C17—H13120.1
Ru1—N4—C20126.7 (2)C18—C17—H13120.2
C16—N4—C20118.9 (2)C17—C18—H14120.3
N1—C1—C2122.3 (3)C19—C18—H14120.3
C1—C2—C3119.1 (3)C18—C19—H15121.1
C2—C3—C4119.3 (3)C20—C19—H15121.1
C3—C4—C5119.3 (3)N4—C20—H16118.3
N1—C5—C4120.7 (3)C19—C20—H16118.3
N1—C5—C6115.5 (2)
Cl1—Ru1—N2—C6176.6 (2)C22—Ru1—N3—C1192.0 (7)
Cl1—Ru1—N2—C103.3 (2)C22—Ru1—N3—C15−87.8 (6)
Cl1—Ru1—N3—C1188.8 (2)N4—Ru1—C22—Cl1−137 (12)
Cl1—Ru1—N3—C15−91.0 (2)N4—Ru1—C22—O2−180 (8)
N3—Ru1—Cl1—O2−150 (3)C22—Ru1—N4—C1688.3 (8)
N3—Ru1—Cl1—C22121 (12)C22—Ru1—N4—C20−93.7 (8)
Cl1—Ru1—N4—C1685.7 (2)Ru1—N1—C1—C2177.8 (2)
Cl1—Ru1—N4—C20−96.2 (2)Ru1—N1—C5—C4−177.4 (2)
N4—Ru1—Cl1—O2131 (3)Ru1—N1—C5—C62.2 (3)
C21—Ru1—Cl1—O2−52 (3)C1—N1—C5—C41.5 (4)
Cl2—Ru1—N1—C1−92.9 (3)C1—N1—C5—C6−178.9 (3)
Cl2—Ru1—N1—C585.9 (2)C5—N1—C1—C2−1.0 (5)
N1—Ru1—Cl2—O176 (3)Ru1—N2—C6—C54.6 (3)
N1—Ru1—Cl2—C2161 (3)Ru1—N2—C6—C7−174.0 (2)
Cl2—Ru1—N2—C6−96.6 (2)Ru1—N2—C10—C9172.8 (2)
Cl2—Ru1—N2—C1090.0 (3)C6—N2—C10—C9−0.3 (5)
N2—Ru1—Cl2—O1155 (3)C10—N2—C6—C5178.5 (3)
N2—Ru1—Cl2—C21139 (3)C10—N2—C6—C7−0.2 (4)
Cl2—Ru1—N3—C112.3 (3)Ru1—N3—C11—C12−179.3 (2)
Cl2—Ru1—N3—C15−177.5 (2)Ru1—N3—C15—C14179.6 (2)
N3—Ru1—Cl2—O1−21 (3)Ru1—N3—C15—C16−1.0 (3)
N3—Ru1—Cl2—C21−37 (3)C11—N3—C15—C14−0.2 (4)
Cl2—Ru1—C22—O22 (5)C11—N3—C15—C16179.2 (2)
N1—Ru1—N2—C6−2.7 (2)C15—N3—C11—C120.5 (5)
N1—Ru1—N2—C10−176.0 (2)Ru1—N4—C16—C150.6 (3)
N2—Ru1—N1—C1−178.6 (2)Ru1—N4—C16—C17179.7 (2)
N2—Ru1—N1—C50.2 (2)Ru1—N4—C20—C19−177.9 (2)
N1—Ru1—N3—C11−92.4 (2)C16—N4—C20—C190.1 (3)
N1—Ru1—N3—C1587.8 (2)C20—N4—C16—C15−177.6 (2)
N3—Ru1—N1—C110.4 (2)C20—N4—C16—C171.5 (4)
N3—Ru1—N1—C5−170.8 (2)N1—C1—C2—C30.2 (4)
N1—Ru1—N4—C16−97.8 (2)C1—C2—C3—C40.1 (4)
N1—Ru1—N4—C2080.3 (2)C2—C3—C4—C50.4 (5)
N4—Ru1—N1—C188.9 (2)C3—C4—C5—N1−1.2 (5)
N4—Ru1—N1—C5−92.3 (2)C3—C4—C5—C6179.3 (3)
C21—Ru1—N1—C1−87.9 (3)N1—C5—C6—N2−4.5 (4)
C21—Ru1—N1—C590.9 (3)N1—C5—C6—C7174.1 (3)
N2—Ru1—N3—C11−155.0 (5)C4—C5—C6—N2175.1 (3)
N2—Ru1—N3—C1525.2 (7)C4—C5—C6—C7−6.3 (5)
N3—Ru1—N2—C661.3 (6)N2—C6—C7—C81.5 (5)
N3—Ru1—N2—C10−112.1 (5)C5—C6—C7—C8−177.0 (3)
N2—Ru1—N4—C16−176.8 (2)C6—C7—C8—C9−2.4 (4)
N2—Ru1—N4—C201.3 (2)C7—C8—C9—C102.0 (5)
N4—Ru1—N2—C685.0 (2)C8—C9—C10—N2−0.6 (5)
N4—Ru1—N2—C10−88.4 (2)N3—C11—C12—C13−0.5 (5)
N2—Ru1—C21—Cl2−41 (3)C11—C12—C13—C140.2 (4)
C21—Ru1—N2—C6−92.9 (3)C12—C13—C14—C150.1 (3)
C21—Ru1—N2—C1093.7 (3)C13—C14—C15—N3−0.1 (3)
N2—Ru1—C22—O289 (9)C13—C14—C15—C16−179.4 (3)
C22—Ru1—N2—C6173.7 (7)N3—C15—C16—N40.3 (4)
C22—Ru1—N2—C100.4 (7)N3—C15—C16—C17−178.8 (3)
N3—Ru1—N4—C16−0.9 (2)C14—C15—C16—N4179.6 (3)
N3—Ru1—N4—C20177.2 (2)C14—C15—C16—C170.5 (5)
N4—Ru1—N3—C11−179.2 (2)N4—C16—C17—C18−1.6 (5)
N4—Ru1—N3—C151.0 (2)C15—C16—C17—C18177.4 (3)
C21—Ru1—N3—C11−1.1 (3)C16—C17—C18—C190.1 (4)
C21—Ru1—N3—C15179.1 (3)C17—C18—C19—C201.4 (5)
N3—Ru1—C22—O2−101 (9)C18—C19—C20—N4−1.6 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···F2i0.952.463.166 (4)131
C4—H4···F1ii0.952.413.257 (4)148
C7—H5···F1ii0.952.543.431 (4)156
C8—H6···F2iii0.952.503.265 (4)138
C13—H11···F5iv0.952.393.331 (4)168
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1/2, −y+1, z−1/2; (iii) x−1/2, −y+1/2, −z; (iv) x−1/2, −y+1/2, −z+1.

Experimental details

Crystal data
Chemical formula[RuCl(C10H8N2)2(CO)]·PF6
Mr621.87
Crystal system, space groupOrthorhombic, P212121
Temperature (K)93
a, b, c (Å)10.882 (5), 12.063 (5), 17.410 (7)
V (Å3)2285.2 (17)
Z4
Radiation typeMo Kα
µ (mm−1)0.95
Crystal size (mm)0.20 × 0.10 × 0.02
Data collection
DiffractometerRigaku Saturn
Absorption correctionMulti-scan
(REQAB; Jacobson, 1998)
Tmin, Tmax0.897, 0.981
No. of measured, independent and
observed [F2 > 2σ(F2)] reflections		22875, 5177, 4689
Rint0.045
(sin θ/λ)max (Å−1)0.648
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.062, 1.08
No. of reflections5177
No. of parameters330
No. of restraints?
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.37, −1.28
Absolute structureFlack (1983), 2249 Friedel pairs
Absolute structure parameter0.22 (4)

Computer programs: CrystalClear-SM (Rigaku, 2009), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 2012), CrystalStructure (Rigaku, 2006).

Selected bond lengths (Å) top
Ru1—Cl12.3521 (17)Ru1—N32.070 (2)
Ru1—N12.086 (2)Ru1—N42.117 (2)
Ru1—N22.070 (2)Ru1—C211.890 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C3—H3···F2i0.952.463.166 (4)131
C4—H4···F1ii0.952.413.257 (4)148
C7—H5···F1ii0.952.543.431 (4)156
C8—H6···F2iii0.952.503.265 (4)138
C13—H11···F5iv0.952.393.331 (4)168
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1/2, −y+1, z−1/2; (iii) x−1/2, −y+1/2, −z; (iv) x−1/2, −y+1/2, −z+1.
 

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