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The tetra­fluoro­borate salt of the mononuclear octahedral ruthenium(II) complex, [RuCl(L)(PPh3)2]BF4, where L = 2,6-bis(3,4-di­hydro-2H-pyrrol-5-yl)­pyridine, has been prepared as the di­chloro­methane solvate. The tri­phenyl­phosphine ligands adopt a trans configuration, with a P-Ru-P angle of 173.72 (2)°.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016343/wn6119sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016343/wn6119Isup2.hkl
Contains datablock I

CCDC reference: 198306

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.031
  • wR factor = 0.076
  • Data-to-parameter ratio = 13.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.86 From the CIF: _reflns_number_total 8322 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 8940 Completeness (_total/calc) 93.09% Alert C: < 95% complete PLAT_302 Alert C Anion/Solvent Disorder ....................... 27.00 Perc. PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 135 C9 -N2 -RU -CL1 -174.80 0.50 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 136 C5 -N2 -RU -CL1 4.70 0.70 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 166 C44 -P2 -RU -P1 105.50 0.20 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 167 C38 -P2 -RU -P1 -131.70 0.20 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 168 C32 -P2 -RU -P1 -10.70 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 181 C14 -P1 -RU -P2 -106.40 0.20 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 182 C20 -P1 -RU -P2 10.30 0.30 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 183 C26 -P1 -RU -P2 133.10 0.20 1.555 1.555 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
10 Alert Level C = Please check

Comment top

In the context of our study of hydrogenation reactions catalysed by ruthenium complexes, we have synthesized a ruthenium complex containing the tridentate ligand 2,6-bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine, one chlorine, and two triphenylphosphines, [RuCl(L)(PPh3)2]+. The cationic complex crystallizes as the tetrafluoroborate salt by slow diffusion of ether into a dichloromethane solution, yielding the dichloromethane solvate, (I). The molecular structure of the cationic moiety, depicted in Fig. 1, shows only small distortions from ideal octahedral geometry; selected bond lengths and angles are presented in Table 1.

The PPh3 groups bend in the direction of the chloride ion to minimize steric interactions with the 2,6-bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine ligand. The P—Ru—P angle is 173.72 (2)°, comparable to that in other trans-diphosphine complexes found in the literature, the values ranging between 173.64 (6) and 178.2 (2)° [Venegas-Yazigi et al., (2002); Perez et al., (1999) and references therein]. The Ru—N bond length, trans to the chloride ion, is shorter than the Ru—Npyrrole bonds, Ru—N2 1.970 (2) Å compared to 2.102 (2) and 2.131 (2) Å for Ru—N1 and Ru—N3, respectively. The same observation has been made in the trans-[RuL1(Cl)(PMe3)2]+ cation, (Bessel et al., 1991), where L1 = 2,6-bis(3-phenylpyrazol-1-yl)pyridine. As observed by Perez et al. in the complexes [RuCl(trpy)(PPh3)2] and [RuCl(trpy)(Ph2PC6H4CH2O(CO)(CH2)3(CO)OCH2C6H4PPh2)] where trpy = 2,2':6',2''-terpyridine (Perez et al., 1999), the phenyl groups of the phosphine ligands influence the geometry in the equatorial plane of the metal. The chloride ligand is pushed by the phenyl groups, creating a difference between the two Cl—Ru—Npyrrole bond angles, Cl—Ru—N3 being greater by 12.32° than Cl—Ru—N1.

Experimental top

To a dichloromethane solution (15 ml) of [RuCl2(PPh3)3] (Holm, 1970) (100 mg, 0.104 mmol) was added, dropwise, a 5 ml solution of 2,6-bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine (Bernauer & Gretillat, 1989) (24 mg, 0.11 mmol). The solution was stirred for 20 minutes and then NaBF4 (15 mg, 0.14 mmol) was added. After 10 minutes the volume was reduced to 5 ml. A red solid was precipitated by addition of ether (3 ml). The solid was filtered and washed three times with ether to give [RuCl(L)(PPh3)2](BF4) in 63% yield (63 mg). Suitable crystals for X-ray diffraction were grown by slow diffusion of ether into a dichloromethane solution at 4°C.

1H NMR (CDCl3): 7.39–7.45 (m, 12H), 7.29–7.34 (m, 7H), 7.18–7.23 (m, 14H), 3.75 (m, 4H), 2.75 (m, 4H), 1.60 (m, 4H). 31P NMR (CDCl3): 21.6 p.p.m.. MS (ESI, m/z): 874 Anal. Calcd. for C50H47BCl3F4N3P2Ru: C, 57.41; N, 4.02 H, 4.53 Found: C, 57.22; N, 4.37; H, 4.72.

Refinement top

Three fluorine atoms of the tetrafluoroborate anion have been treated as disordered with partial occupancy factors of 0.70:0.30. Hydrogen atoms were included in calculated positions and treated as riding atoms, using SHELXL97 default parameters.

Computing details top

Data collection: EXPOSE (Stoe & Cie, 2000); cell refinement: CELL (Stoe & Cie, 2000); data reduction: INTEGRATE (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of [RuCl(L)(PPh3)2]+; for clarity tetrafluoroborate, dichloromethane and hydrogen atoms have been omitted. Displacement ellipsoids are drawn at the 50% probability level.
[RuCl{2,6-bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine}(PPh3)2]BF4 dichloromethane solvate top
Crystal data top
[Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2Z = 2
Mr = 1046.08F(000) = 1068
Triclinic, P1Dx = 1.505 Mg m3
a = 10.3368 (8) ÅMo Kα radiation, λ = 0.71069 Å
b = 12.7939 (11) ÅCell parameters from 8000 reflections
c = 19.1336 (16) Åθ = 2.1–25.9°
α = 80.231 (10)°µ = 0.64 mm1
β = 89.193 (9)°T = 153 K
γ = 67.943 (9)°Rod, red
V = 2307.8 (3) Å30.5 × 0.3 × 0.15 mm
Data collection top
STOE IPDS
diffractometer
8322 independent reflections
Radiation source: fine-focus sealed tube6363 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
Detector resolution: 0.81Å pixels mm-1θmax = 25.9°, θmin = 2.1°
ϕ oscillation scansh = 1211
Absorption correction: part of the refinement model (ΔF)
(Walker & Stuart, 1983)
k = 1515
Tmin = 0.699, Tmax = 0.880l = 2323
16304 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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0452P)2]
where P = (Fo2 + 2Fc2)/3
8322 reflections(Δ/σ)max = 0.001
604 parametersΔρmax = 0.56 e Å3
0 restraintsΔρmin = 0.58 e Å3
Crystal data top
[Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2γ = 67.943 (9)°
Mr = 1046.08V = 2307.8 (3) Å3
Triclinic, P1Z = 2
a = 10.3368 (8) ÅMo Kα radiation
b = 12.7939 (11) ŵ = 0.64 mm1
c = 19.1336 (16) ÅT = 153 K
α = 80.231 (10)°0.5 × 0.3 × 0.15 mm
β = 89.193 (9)°
Data collection top
STOE IPDS
diffractometer
8322 independent reflections
Absorption correction: part of the refinement model (ΔF)
(Walker & Stuart, 1983)
6363 reflections with I > 2σ(I)
Tmin = 0.699, Tmax = 0.880Rint = 0.028
16304 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.076H-atom parameters constrained
S = 0.96Δρmax = 0.56 e Å3
8322 reflectionsΔρmin = 0.58 e Å3
604 parameters
Special details top

Experimental. A crystal was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. Image plate distance 70 mm, ϕ oscillation scans 0 − 180°, step Δϕ = 1.2°, 2 minutes per frame.

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*/UeqOcc. (<1)
C10.0136 (3)0.3809 (2)0.19238 (14)0.0244 (6)
H1B0.03490.44390.16360.029*
H1A0.01120.32700.16140.029*
C20.1217 (3)0.3191 (3)0.25483 (16)0.0375 (8)
H2B0.21250.32580.24390.045*
H2A0.13610.23700.26670.045*
C30.0556 (3)0.3824 (3)0.31604 (15)0.0305 (7)
H3B0.07410.32910.36210.037*
H3A0.08950.44410.31990.037*
C40.0955 (3)0.4296 (2)0.29238 (13)0.0207 (6)
C50.2152 (3)0.4762 (2)0.33478 (13)0.0201 (6)
C60.2140 (3)0.4911 (2)0.40460 (14)0.0260 (6)
H6A0.12810.47270.43040.031*
C70.3401 (3)0.5333 (2)0.43650 (14)0.0300 (7)
H7A0.34100.54410.48440.036*
C80.4657 (3)0.5600 (2)0.39806 (14)0.0279 (7)
H8A0.55260.58760.41960.033*
C90.4606 (3)0.5453 (2)0.32789 (13)0.0207 (6)
C100.5794 (3)0.5703 (2)0.27844 (13)0.0194 (6)
C110.7297 (3)0.6159 (2)0.29375 (16)0.0298 (7)
H11B0.75890.69340.30590.036*
H11A0.75090.56440.33300.036*
C120.7984 (4)0.6189 (4)0.2245 (2)0.0662 (13)
H12A0.84510.56340.23060.079*
H12B0.86950.69640.20730.079*
C130.6898 (3)0.5892 (3)0.17359 (17)0.0354 (8)
H13A0.70260.65650.13610.043*
H13B0.69410.52650.15090.043*
C140.3792 (3)0.2724 (2)0.32271 (13)0.0205 (6)
C150.2740 (3)0.2451 (2)0.37607 (14)0.0274 (7)
H150.18040.23150.36390.033*
C160.3081 (4)0.2380 (2)0.44705 (15)0.0376 (9)
H160.23720.21920.48330.045*
C170.4428 (4)0.2578 (3)0.46471 (16)0.0403 (9)
H170.46440.25120.51330.048*
C180.5479 (4)0.2872 (3)0.41265 (16)0.0375 (8)
H180.64160.30220.42530.045*
C190.5153 (3)0.2948 (2)0.34154 (14)0.0265 (7)
H190.58740.31550.30560.032*
C200.4688 (3)0.2626 (2)0.18366 (13)0.0180 (5)
C210.4885 (3)0.1599 (2)0.20761 (15)0.0260 (6)
H210.43430.10770.24760.031*
C220.5870 (3)0.1345 (3)0.17295 (16)0.0331 (7)
H220.59950.06470.18910.040*
C230.6678 (3)0.2106 (3)0.11466 (15)0.0315 (7)
H230.73650.19360.09170.038*
C240.6475 (3)0.3108 (3)0.09039 (14)0.0271 (7)
H240.70180.36260.05030.033*
C250.5479 (3)0.3361 (2)0.12445 (13)0.0205 (6)
H250.53370.40480.10690.025*
C260.1784 (3)0.1691 (2)0.22190 (14)0.0231 (6)
C270.1401 (3)0.0658 (2)0.27067 (16)0.0341 (8)
H270.19310.06050.31110.041*
C280.0241 (4)0.0289 (3)0.25957 (19)0.0459 (10)
H280.00170.09880.29250.055*
C290.0536 (4)0.0215 (3)0.2008 (2)0.0465 (10)
H290.13360.08600.19400.056*
C300.0154 (3)0.0792 (3)0.15200 (19)0.0386 (8)
H300.06840.08370.11140.046*
C310.1011 (3)0.1744 (2)0.16249 (15)0.0269 (7)
H310.12760.24340.12870.032*
C320.4927 (3)0.7657 (2)0.08809 (13)0.0176 (5)
C330.5546 (3)0.7164 (2)0.04652 (13)0.0182 (5)
H330.52720.63550.05440.022*
C340.6564 (3)0.7844 (2)0.00655 (14)0.0226 (6)
H340.69750.74960.03480.027*
C350.6979 (3)0.9020 (2)0.01836 (14)0.0253 (6)
H350.76820.94810.05420.030*
C360.6364 (3)0.9528 (2)0.02235 (15)0.0281 (7)
H360.66481.03380.01430.034*
C370.5340 (3)0.8857 (2)0.07471 (14)0.0234 (6)
H370.49130.92090.10180.028*
C380.2047 (3)0.7040 (2)0.11919 (13)0.0180 (6)
C390.1714 (3)0.7977 (2)0.12716 (15)0.0237 (6)
H390.22380.84890.15710.028*
C400.0618 (3)0.8159 (2)0.09139 (16)0.0304 (7)
H400.03920.87930.09750.036*
C410.0149 (3)0.7432 (3)0.04702 (16)0.0326 (7)
H410.08910.75680.02250.039*
C420.0176 (3)0.6502 (3)0.03867 (15)0.0308 (7)
H420.03430.59980.00820.037*
C430.1253 (3)0.6307 (2)0.07467 (14)0.0236 (6)
H430.14580.56610.06910.028*
C440.4053 (3)0.7597 (2)0.22992 (13)0.0189 (6)
C450.5466 (3)0.8159 (2)0.24115 (14)0.0244 (6)
H450.61580.81650.20880.029*
C460.5872 (3)0.8711 (2)0.29909 (15)0.0301 (7)
H460.68360.90900.30620.036*
C470.4876 (4)0.8708 (2)0.34613 (15)0.0351 (8)
H470.51510.91020.38500.042*
C480.3472 (4)0.8131 (2)0.33677 (15)0.0341 (8)
H480.27870.81180.36980.041*
C490.3058 (3)0.7570 (2)0.27932 (14)0.0253 (6)
H490.20930.71660.27370.030*
C1S0.1556 (4)0.0706 (3)0.49170 (19)0.0462 (9)
H1S10.09090.14660.50010.055*
H1S20.14990.01220.53150.055*
N10.1209 (2)0.42621 (17)0.22674 (11)0.0178 (5)
N20.3378 (2)0.50453 (16)0.29666 (10)0.0160 (5)
N30.5526 (2)0.55202 (18)0.21366 (11)0.0201 (5)
F10.0647 (3)0.32271 (18)0.47325 (12)0.0669 (7)
F20.0194 (4)0.3034 (4)0.35282 (17)0.0556 (10)0.70
F30.1141 (4)0.4557 (2)0.43033 (15)0.0537 (8)0.70
F40.1154 (5)0.2822 (5)0.4341 (2)0.0742 (12)0.70
F50.0022 (14)0.2113 (7)0.3939 (5)0.093 (4)0.30
F60.1726 (8)0.3757 (13)0.4432 (4)0.089 (4)0.30
F70.0037 (10)0.3768 (9)0.3746 (5)0.065 (3)0.30
P10.33733 (7)0.29524 (5)0.22936 (3)0.01592 (15)
P20.35576 (7)0.67793 (5)0.15724 (3)0.01494 (14)
Cl10.30326 (7)0.44977 (5)0.07328 (3)0.01897 (14)
Cl20.10273 (11)0.04416 (10)0.41220 (5)0.0633 (3)
Cl30.32484 (12)0.06745 (11)0.49062 (8)0.0831 (4)
B10.0340 (4)0.3352 (3)0.42247 (18)0.0362 (9)
Ru0.33465 (2)0.484403 (17)0.196759 (10)0.01416 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0127 (15)0.0338 (16)0.0263 (14)0.0060 (12)0.0026 (11)0.0110 (12)
C20.0192 (17)0.051 (2)0.0361 (17)0.0044 (14)0.0031 (13)0.0137 (15)
C30.0225 (17)0.0388 (17)0.0282 (15)0.0079 (13)0.0058 (12)0.0087 (13)
C40.0214 (16)0.0219 (14)0.0185 (13)0.0078 (11)0.0006 (11)0.0038 (10)
C50.0251 (16)0.0173 (13)0.0177 (13)0.0075 (11)0.0006 (11)0.0034 (10)
C60.0333 (18)0.0268 (15)0.0199 (14)0.0135 (13)0.0011 (12)0.0041 (11)
C70.044 (2)0.0336 (16)0.0162 (13)0.0165 (14)0.0075 (12)0.0092 (12)
C80.0336 (19)0.0284 (15)0.0223 (14)0.0113 (13)0.0129 (12)0.0077 (12)
C90.0237 (16)0.0165 (13)0.0206 (13)0.0062 (11)0.0063 (11)0.0031 (10)
C100.0181 (15)0.0139 (12)0.0232 (14)0.0048 (11)0.0080 (11)0.0007 (10)
C110.0211 (17)0.0264 (15)0.0385 (17)0.0065 (12)0.0133 (13)0.0037 (12)
C120.019 (2)0.120 (4)0.044 (2)0.011 (2)0.0018 (16)0.008 (2)
C130.0136 (16)0.053 (2)0.0398 (18)0.0120 (14)0.0011 (13)0.0112 (15)
C140.0291 (17)0.0154 (13)0.0174 (13)0.0098 (11)0.0010 (11)0.0005 (10)
C150.0355 (18)0.0211 (14)0.0221 (14)0.0081 (12)0.0068 (12)0.0001 (11)
C160.065 (3)0.0252 (16)0.0183 (14)0.0137 (15)0.0129 (15)0.0024 (12)
C170.072 (3)0.0316 (17)0.0183 (15)0.0213 (17)0.0104 (16)0.0043 (12)
C180.053 (2)0.0338 (17)0.0283 (16)0.0193 (16)0.0148 (15)0.0072 (13)
C190.0342 (19)0.0255 (15)0.0221 (14)0.0146 (13)0.0029 (12)0.0032 (11)
C200.0157 (14)0.0219 (13)0.0184 (12)0.0079 (11)0.0034 (10)0.0078 (10)
C210.0338 (18)0.0191 (14)0.0261 (14)0.0116 (12)0.0009 (12)0.0032 (11)
C220.040 (2)0.0289 (16)0.0396 (17)0.0210 (14)0.0092 (14)0.0137 (13)
C230.0296 (18)0.0442 (18)0.0321 (16)0.0211 (15)0.0068 (13)0.0207 (14)
C240.0238 (17)0.0409 (17)0.0186 (13)0.0136 (13)0.0013 (11)0.0071 (12)
C250.0201 (15)0.0262 (14)0.0168 (12)0.0109 (11)0.0024 (10)0.0032 (10)
C260.0207 (16)0.0190 (13)0.0276 (14)0.0036 (11)0.0062 (11)0.0072 (11)
C270.041 (2)0.0209 (15)0.0339 (16)0.0044 (13)0.0059 (14)0.0038 (12)
C280.046 (2)0.0227 (16)0.053 (2)0.0047 (15)0.0171 (18)0.0068 (15)
C290.0274 (19)0.0356 (19)0.064 (2)0.0089 (15)0.0116 (17)0.0230 (17)
C300.0224 (18)0.0420 (19)0.052 (2)0.0063 (14)0.0036 (15)0.0229 (16)
C310.0211 (16)0.0258 (15)0.0313 (15)0.0040 (12)0.0040 (12)0.0097 (12)
C320.0162 (14)0.0197 (13)0.0163 (12)0.0059 (11)0.0032 (10)0.0040 (10)
C330.0172 (15)0.0174 (13)0.0194 (13)0.0057 (11)0.0030 (10)0.0040 (10)
C340.0196 (16)0.0274 (14)0.0215 (13)0.0088 (12)0.0001 (11)0.0064 (11)
C350.0221 (16)0.0256 (15)0.0247 (14)0.0065 (12)0.0045 (12)0.0004 (11)
C360.0305 (18)0.0195 (14)0.0306 (15)0.0066 (12)0.0036 (13)0.0007 (11)
C370.0283 (17)0.0204 (14)0.0228 (14)0.0109 (12)0.0026 (11)0.0030 (11)
C380.0138 (14)0.0208 (13)0.0175 (12)0.0061 (11)0.0031 (10)0.0006 (10)
C390.0196 (16)0.0203 (14)0.0299 (15)0.0070 (11)0.0014 (12)0.0022 (11)
C400.0259 (18)0.0231 (15)0.0416 (17)0.0123 (13)0.0068 (14)0.0032 (13)
C410.0182 (17)0.0446 (19)0.0317 (16)0.0137 (14)0.0006 (12)0.0068 (13)
C420.0259 (18)0.0396 (17)0.0260 (15)0.0109 (14)0.0070 (12)0.0077 (13)
C430.0221 (16)0.0288 (15)0.0227 (14)0.0120 (12)0.0026 (11)0.0066 (11)
C440.0257 (16)0.0137 (12)0.0161 (12)0.0058 (11)0.0012 (11)0.0032 (10)
C450.0284 (17)0.0232 (14)0.0216 (14)0.0093 (12)0.0051 (12)0.0055 (11)
C460.0361 (19)0.0230 (14)0.0260 (15)0.0053 (13)0.0103 (13)0.0053 (12)
C470.055 (2)0.0257 (15)0.0219 (15)0.0093 (15)0.0089 (14)0.0107 (12)
C480.049 (2)0.0307 (16)0.0222 (15)0.0126 (15)0.0068 (14)0.0080 (12)
C490.0302 (17)0.0217 (14)0.0216 (13)0.0065 (12)0.0011 (12)0.0052 (11)
C1S0.044 (2)0.043 (2)0.053 (2)0.0170 (17)0.0059 (17)0.0146 (17)
N10.0160 (12)0.0191 (11)0.0187 (11)0.0063 (9)0.0008 (9)0.0048 (9)
N20.0178 (12)0.0130 (10)0.0169 (10)0.0059 (9)0.0023 (9)0.0015 (8)
N30.0155 (13)0.0186 (11)0.0252 (12)0.0064 (9)0.0033 (9)0.0020 (9)
F10.0765 (18)0.0539 (13)0.0588 (14)0.0112 (12)0.0409 (12)0.0144 (11)
F20.0293 (18)0.092 (3)0.0322 (17)0.013 (2)0.0037 (12)0.0031 (19)
F30.070 (2)0.0384 (16)0.0379 (16)0.0048 (16)0.0158 (15)0.0055 (13)
F40.085 (3)0.097 (3)0.075 (3)0.060 (3)0.012 (3)0.047 (3)
F50.161 (11)0.050 (5)0.067 (6)0.042 (6)0.054 (6)0.002 (4)
F60.034 (5)0.180 (12)0.017 (3)0.010 (6)0.002 (3)0.004 (6)
F70.063 (7)0.097 (7)0.075 (7)0.057 (7)0.036 (5)0.058 (6)
P10.0168 (4)0.0146 (3)0.0148 (3)0.0047 (3)0.0007 (3)0.0014 (2)
P20.0152 (4)0.0153 (3)0.0144 (3)0.0053 (3)0.0013 (3)0.0041 (2)
Cl10.0224 (4)0.0203 (3)0.0160 (3)0.0090 (3)0.0029 (2)0.0060 (2)
Cl20.0473 (6)0.0798 (7)0.0562 (6)0.0118 (5)0.0078 (5)0.0225 (5)
Cl30.0437 (7)0.0918 (8)0.1381 (11)0.0302 (6)0.0150 (7)0.0743 (8)
B10.037 (2)0.043 (2)0.0258 (18)0.0130 (18)0.0043 (15)0.0019 (16)
Ru0.01295 (12)0.01588 (11)0.01338 (10)0.00467 (8)0.00122 (7)0.00377 (7)
Geometric parameters (Å, º) top
C1—N11.483 (3)C30—C311.396 (4)
C1—C21.535 (4)C32—C331.389 (4)
C2—C31.542 (4)C32—C371.408 (4)
C3—C41.492 (4)C32—P21.836 (3)
C4—N11.298 (3)C33—C341.392 (4)
C4—C51.458 (4)C34—C351.379 (4)
C5—N21.364 (3)C35—C361.388 (4)
C5—C61.382 (4)C36—C371.385 (4)
C6—C71.387 (4)C38—C391.396 (4)
C7—C81.397 (4)C38—C431.398 (4)
C8—C91.385 (4)C38—P21.832 (3)
C9—N21.352 (3)C39—C401.389 (4)
C9—C101.463 (4)C40—C411.382 (4)
C10—N31.307 (3)C41—C421.385 (4)
C10—C111.485 (4)C42—C431.380 (4)
C11—C121.500 (5)C44—C491.393 (4)
C12—C131.458 (5)C44—C451.396 (4)
C13—N31.491 (4)C44—P21.834 (2)
C14—C191.382 (4)C45—C461.391 (4)
C14—C151.404 (4)C46—C471.376 (5)
C14—P11.833 (3)C47—C481.384 (5)
C15—C161.395 (4)C48—C491.389 (4)
C16—C171.367 (5)C1S—Cl31.734 (4)
C17—C181.382 (5)C1S—Cl21.750 (4)
C18—C191.393 (4)N1—Ru2.102 (2)
C20—C251.387 (4)N2—Ru1.970 (2)
C20—C211.405 (4)N3—Ru2.131 (2)
C20—P11.835 (3)F1—B11.383 (4)
C21—C221.387 (4)F2—B11.383 (5)
C22—C231.391 (4)F3—B11.433 (5)
C23—C241.378 (4)F4—B11.305 (5)
C24—C251.390 (4)F5—B11.496 (9)
C26—C311.388 (4)F6—B11.367 (9)
C26—C271.405 (4)F7—B11.267 (9)
C26—P11.844 (3)P1—Ru2.4051 (7)
C27—C281.392 (4)P2—Ru2.3902 (7)
C28—C291.384 (6)Cl1—Ru2.4717 (6)
C29—C301.381 (5)
N1—C1—C2104.1 (2)C46—C45—C44120.9 (3)
C1—C2—C3103.5 (2)C47—C46—C45119.9 (3)
C4—C3—C2100.8 (2)C46—C47—C48120.0 (3)
N1—C4—C5117.5 (2)C47—C48—C49120.4 (3)
N1—C4—C3115.1 (2)C48—C49—C44120.3 (3)
C5—C4—C3127.4 (2)Cl3—C1S—Cl2112.3 (2)
N2—C5—C6121.2 (3)C4—N1—C1109.0 (2)
N2—C5—C4111.1 (2)C4—N1—Ru114.18 (17)
C6—C5—C4127.8 (3)C1—N1—Ru136.83 (16)
C5—C6—C7119.0 (3)C9—N2—C5119.8 (2)
C6—C7—C8120.0 (2)C9—N2—Ru120.45 (17)
C9—C8—C7118.5 (3)C5—N2—Ru119.79 (17)
N2—C9—C8121.6 (3)C10—N3—C13107.1 (2)
N2—C9—C10111.4 (2)C10—N3—Ru113.10 (18)
C8—C9—C10127.0 (3)C13—N3—Ru139.78 (18)
N3—C10—C9117.7 (2)C14—P1—C20102.82 (13)
N3—C10—C11115.6 (2)C14—P1—C26104.60 (12)
C9—C10—C11126.7 (2)C20—P1—C26100.82 (11)
C10—C11—C12101.8 (2)C14—P1—Ru109.35 (8)
C13—C12—C11107.7 (3)C20—P1—Ru117.60 (9)
C12—C13—N3107.2 (3)C26—P1—Ru119.68 (10)
C19—C14—C15119.2 (3)C44—P2—C38106.04 (12)
C19—C14—P1121.1 (2)C44—P2—C32101.99 (11)
C15—C14—P1119.2 (2)C38—P2—C32100.60 (12)
C16—C15—C14119.5 (3)C44—P2—Ru110.58 (8)
C17—C16—C15120.4 (3)C38—P2—Ru118.62 (8)
C16—C17—C18120.7 (3)C32—P2—Ru117.14 (9)
C17—C18—C19119.4 (3)F7—B1—F4141.7 (6)
C14—C19—C18120.7 (3)F7—B1—F6118.7 (8)
C25—C20—C21118.6 (2)F4—B1—F648.6 (6)
C25—C20—P1121.5 (2)F7—B1—F1106.6 (5)
C21—C20—P1119.9 (2)F4—B1—F1110.0 (3)
C22—C21—C20120.1 (3)F6—B1—F1119.7 (4)
C21—C22—C23120.5 (3)F7—B1—F240.0 (5)
C24—C23—C22119.7 (3)F4—B1—F2111.2 (4)
C23—C24—C25120.1 (3)F6—B1—F2125.1 (4)
C20—C25—C24121.0 (3)F1—B1—F2115.2 (3)
C31—C26—C27119.1 (3)F7—B1—F369.5 (6)
C31—C26—P1118.1 (2)F4—B1—F3109.6 (4)
C27—C26—P1122.5 (2)F6—B1—F361.1 (7)
C28—C27—C26119.9 (3)F1—B1—F3106.0 (3)
C29—C28—C27120.2 (3)F2—B1—F3104.5 (3)
C30—C29—C28120.3 (3)F7—B1—F5107.5 (7)
C29—C30—C31119.9 (3)F4—B1—F556.3 (6)
C26—C31—C30120.6 (3)F6—B1—F5102.7 (9)
C33—C32—C37118.5 (2)F1—B1—F598.9 (4)
C33—C32—P2121.50 (19)F2—B1—F567.6 (5)
C37—C32—P2119.97 (19)F3—B1—F5154.8 (5)
C32—C33—C34120.6 (2)N2—Ru—N177.47 (8)
C35—C34—C33120.4 (2)N2—Ru—N377.35 (9)
C34—C35—C36119.8 (2)N1—Ru—N3154.81 (8)
C37—C36—C35120.2 (3)N2—Ru—P291.06 (6)
C36—C37—C32120.5 (2)N1—Ru—P293.80 (6)
C39—C38—C43118.2 (3)N3—Ru—P286.95 (6)
C39—C38—P2124.1 (2)N2—Ru—P191.96 (6)
C43—C38—P2117.5 (2)N1—Ru—P192.23 (6)
C40—C39—C38120.0 (3)N3—Ru—P188.34 (6)
C41—C40—C39121.0 (3)P2—Ru—P1173.72 (2)
C40—C41—C42119.4 (3)N2—Ru—Cl1173.88 (7)
C43—C42—C41120.0 (3)N1—Ru—Cl196.43 (6)
C42—C43—C38121.4 (3)N3—Ru—Cl1108.75 (6)
C49—C44—C45118.5 (2)P2—Ru—Cl189.76 (2)
C49—C44—P2121.5 (2)P1—Ru—Cl187.82 (2)
C45—C44—P2119.6 (2)
N1—C1—C2—C326.9 (3)C15—C14—P1—C2650.2 (2)
C1—C2—C3—C424.1 (3)C19—C14—P1—Ru93.2 (2)
C2—C3—C4—N113.8 (3)C15—C14—P1—Ru79.1 (2)
C2—C3—C4—C5164.9 (3)C25—C20—P1—C14131.0 (2)
N1—C4—C5—N22.7 (3)C21—C20—P1—C1450.6 (2)
C3—C4—C5—N2176.0 (3)C25—C20—P1—C26121.2 (2)
N1—C4—C5—C6178.2 (3)C21—C20—P1—C2657.3 (2)
C3—C4—C5—C63.2 (5)C25—C20—P1—Ru10.8 (2)
N2—C5—C6—C71.4 (4)C21—C20—P1—Ru170.75 (18)
C4—C5—C6—C7177.7 (3)C31—C26—P1—C14164.3 (2)
C5—C6—C7—C80.0 (4)C27—C26—P1—C1421.2 (3)
C6—C7—C8—C91.2 (4)C31—C26—P1—C2089.3 (2)
C7—C8—C9—N21.0 (4)C27—C26—P1—C2085.2 (2)
C7—C8—C9—C10178.6 (3)C31—C26—P1—Ru41.4 (2)
N2—C9—C10—N30.7 (3)C27—C26—P1—Ru144.1 (2)
C8—C9—C10—N3179.0 (3)C49—C44—P2—C3846.1 (2)
N2—C9—C10—C11179.9 (2)C45—C44—P2—C38141.2 (2)
C8—C9—C10—C110.4 (4)C49—C44—P2—C32151.0 (2)
N3—C10—C11—C122.6 (4)C45—C44—P2—C3236.3 (2)
C9—C10—C11—C12178.0 (3)C49—C44—P2—Ru83.7 (2)
C10—C11—C12—C136.3 (4)C45—C44—P2—Ru89.0 (2)
C11—C12—C13—N37.8 (5)C39—C38—P2—C4420.8 (2)
C19—C14—C15—C161.7 (4)C43—C38—P2—C44164.73 (19)
P1—C14—C15—C16174.1 (2)C39—C38—P2—C3285.1 (2)
C14—C15—C16—C170.2 (4)C43—C38—P2—C3289.4 (2)
C15—C16—C17—C181.2 (5)C39—C38—P2—Ru145.83 (19)
C16—C17—C18—C191.1 (5)C43—C38—P2—Ru39.7 (2)
C15—C14—C19—C181.8 (4)C33—C32—P2—C44138.5 (2)
P1—C14—C19—C18174.1 (2)C37—C32—P2—C4443.6 (2)
C17—C18—C19—C140.4 (4)C33—C32—P2—C38112.5 (2)
C25—C20—C21—C221.1 (4)C37—C32—P2—C3865.5 (2)
P1—C20—C21—C22179.6 (2)C33—C32—P2—Ru17.6 (3)
C20—C21—C22—C230.5 (4)C37—C32—P2—Ru164.42 (19)
C21—C22—C23—C241.3 (4)C9—N2—Ru—N1178.8 (2)
C22—C23—C24—C250.6 (4)C5—N2—Ru—N10.60 (18)
C21—C20—C25—C241.8 (4)C9—N2—Ru—N30.91 (18)
P1—C20—C25—C24179.7 (2)C5—N2—Ru—N3179.7 (2)
C23—C24—C25—C201.0 (4)C9—N2—Ru—P287.54 (18)
C31—C26—C27—C281.2 (4)C5—N2—Ru—P293.06 (18)
P1—C26—C27—C28175.6 (2)C9—N2—Ru—P186.95 (18)
C26—C27—C28—C290.1 (5)C5—N2—Ru—P192.45 (18)
C27—C28—C29—C301.1 (5)C9—N2—Ru—Cl1174.8 (5)
C28—C29—C30—C310.8 (5)C5—N2—Ru—Cl14.7 (7)
C27—C26—C31—C301.5 (4)C4—N1—Ru—N20.94 (18)
P1—C26—C31—C30176.2 (2)C1—N1—Ru—N2178.9 (3)
C29—C30—C31—C260.5 (5)C4—N1—Ru—N30.3 (3)
C37—C32—C33—C340.8 (4)C1—N1—Ru—N3179.6 (2)
P2—C32—C33—C34178.8 (2)C4—N1—Ru—P291.19 (18)
C32—C33—C34—C350.4 (4)C1—N1—Ru—P288.7 (2)
C33—C34—C35—C360.8 (4)C4—N1—Ru—P190.57 (18)
C34—C35—C36—C370.1 (5)C1—N1—Ru—P189.6 (2)
C35—C36—C37—C321.1 (5)C4—N1—Ru—Cl1178.62 (17)
C33—C32—C37—C361.5 (4)C1—N1—Ru—Cl11.5 (3)
P2—C32—C37—C36179.5 (2)C10—N3—Ru—N21.22 (17)
C43—C38—C39—C400.1 (4)C13—N3—Ru—N2176.8 (3)
P2—C38—C39—C40174.5 (2)C10—N3—Ru—N10.6 (3)
C38—C39—C40—C410.7 (4)C13—N3—Ru—N1177.4 (3)
C39—C40—C41—C420.6 (4)C10—N3—Ru—P293.00 (17)
C40—C41—C42—C430.2 (4)C13—N3—Ru—P285.0 (3)
C41—C42—C43—C380.9 (4)C10—N3—Ru—P191.16 (17)
C39—C38—C43—C420.7 (4)C13—N3—Ru—P190.8 (3)
P2—C38—C43—C42174.1 (2)C10—N3—Ru—Cl1178.29 (16)
C49—C44—C45—C462.0 (4)C13—N3—Ru—Cl13.7 (3)
P2—C44—C45—C46175.0 (2)C44—P2—Ru—N213.25 (12)
C44—C45—C46—C470.1 (4)C38—P2—Ru—N2109.52 (11)
C45—C46—C47—C481.7 (4)C32—P2—Ru—N2129.47 (11)
C46—C47—C48—C491.2 (5)C44—P2—Ru—N190.76 (11)
C47—C48—C49—C441.0 (4)C38—P2—Ru—N132.01 (11)
C45—C44—C49—C482.5 (4)C32—P2—Ru—N1153.02 (11)
P2—C44—C49—C48175.3 (2)C44—P2—Ru—N364.02 (11)
C5—C4—N1—C1177.7 (2)C38—P2—Ru—N3173.21 (11)
C3—C4—N1—C13.5 (3)C32—P2—Ru—N352.20 (11)
C5—C4—N1—Ru2.2 (3)C44—P2—Ru—P1105.5 (2)
C3—C4—N1—Ru176.60 (19)C38—P2—Ru—P1131.7 (2)
C2—C1—N1—C419.5 (3)C32—P2—Ru—P110.7 (3)
C2—C1—N1—Ru160.6 (2)C44—P2—Ru—Cl1172.82 (10)
C8—C9—N2—C50.5 (4)C38—P2—Ru—Cl164.42 (9)
C10—C9—N2—C5179.9 (2)C32—P2—Ru—Cl156.59 (9)
C8—C9—N2—Ru179.9 (2)C14—P1—Ru—N212.29 (12)
C10—C9—N2—Ru0.5 (3)C20—P1—Ru—N2128.97 (11)
C6—C5—N2—C91.7 (4)C26—P1—Ru—N2108.22 (11)
C4—C5—N2—C9177.6 (2)C14—P1—Ru—N189.82 (11)
C6—C5—N2—Ru178.91 (19)C20—P1—Ru—N1153.50 (11)
C4—C5—N2—Ru1.8 (3)C26—P1—Ru—N130.69 (11)
C9—C10—N3—C13177.3 (2)C14—P1—Ru—N364.99 (12)
C11—C10—N3—C132.2 (3)C20—P1—Ru—N351.69 (11)
C9—C10—N3—Ru1.4 (3)C26—P1—Ru—N3174.50 (11)
C11—C10—N3—Ru179.16 (18)C14—P1—Ru—P2106.4 (2)
C12—C13—N3—C106.3 (4)C20—P1—Ru—P210.3 (3)
C12—C13—N3—Ru175.7 (3)C26—P1—Ru—P2133.1 (2)
C19—C14—P1—C2032.5 (2)C14—P1—Ru—Cl1173.83 (10)
C15—C14—P1—C20155.2 (2)C20—P1—Ru—Cl157.15 (9)
C19—C14—P1—C26137.5 (2)C26—P1—Ru—Cl165.66 (10)

Experimental details

Crystal data
Chemical formula[Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2
Mr1046.08
Crystal system, space groupTriclinic, P1
Temperature (K)153
a, b, c (Å)10.3368 (8), 12.7939 (11), 19.1336 (16)
α, β, γ (°)80.231 (10), 89.193 (9), 67.943 (9)
V3)2307.8 (3)
Z2
Radiation typeMo Kα
µ (mm1)0.64
Crystal size (mm)0.5 × 0.3 × 0.15
Data collection
DiffractometerSTOE IPDS
diffractometer
Absorption correctionPart of the refinement model (ΔF)
(Walker & Stuart, 1983)
Tmin, Tmax0.699, 0.880
No. of measured, independent and
observed [I > 2σ(I)] reflections
16304, 8322, 6363
Rint0.028
(sin θ/λ)max1)0.614
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.076, 0.96
No. of reflections8322
No. of parameters604
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.56, 0.58

Computer programs: EXPOSE (Stoe & Cie, 2000), CELL (Stoe & Cie, 2000), INTEGRATE (Stoe & Cie, 2000), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
N1—Ru2.102 (2)P1—Ru2.4051 (7)
N2—Ru1.970 (2)P2—Ru2.3902 (7)
N3—Ru2.131 (2)Cl1—Ru2.4717 (6)
N2—Ru—N177.47 (8)N2—Ru—Cl1173.88 (7)
N2—Ru—N377.35 (9)N1—Ru—Cl196.43 (6)
N1—Ru—N3154.81 (8)N3—Ru—Cl1108.75 (6)
P2—Ru—P1173.72 (2)
 

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