Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016343/wn6119sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016343/wn6119Isup2.hkl |
CCDC reference: 198306
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.
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.
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.
[Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2 | Z = 2 |
Mr = 1046.08 | F(000) = 1068 |
Triclinic, P1 | Dx = 1.505 Mg m−3 |
a = 10.3368 (8) Å | Mo Kα radiation, λ = 0.71069 Å |
b = 12.7939 (11) Å | Cell parameters from 8000 reflections |
c = 19.1336 (16) Å | θ = 2.1–25.9° |
α = 80.231 (10)° | µ = 0.64 mm−1 |
β = 89.193 (9)° | T = 153 K |
γ = 67.943 (9)° | Rod, red |
V = 2307.8 (3) Å3 | 0.5 × 0.3 × 0.15 mm |
STOE IPDS diffractometer | 8322 independent reflections |
Radiation source: fine-focus sealed tube | 6363 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
Detector resolution: 0.81Å pixels mm-1 | θmax = 25.9°, θmin = 2.1° |
ϕ oscillation scans | h = −12→11 |
Absorption correction: part of the refinement model (ΔF) (Walker & Stuart, 1983) | k = −15→15 |
Tmin = 0.699, Tmax = 0.880 | l = −23→23 |
16304 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H-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 parameters | Δρmax = 0.56 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
[Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2 | γ = 67.943 (9)° |
Mr = 1046.08 | V = 2307.8 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.3368 (8) Å | Mo Kα radiation |
b = 12.7939 (11) Å | µ = 0.64 mm−1 |
c = 19.1336 (16) Å | T = 153 K |
α = 80.231 (10)° | 0.5 × 0.3 × 0.15 mm |
β = 89.193 (9)° |
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 = 0.880 | Rint = 0.028 |
16304 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 0 restraints |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 0.96 | Δρmax = 0.56 e Å−3 |
8322 reflections | Δρmin = −0.58 e Å−3 |
604 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
C1 | 0.0136 (3) | 0.3809 (2) | 0.19238 (14) | 0.0244 (6) | |
H1B | 0.0349 | 0.4439 | 0.1636 | 0.029* | |
H1A | 0.0112 | 0.3270 | 0.1614 | 0.029* | |
C2 | 0.1217 (3) | 0.3191 (3) | 0.25483 (16) | 0.0375 (8) | |
H2B | 0.2125 | 0.3258 | 0.2439 | 0.045* | |
H2A | 0.1361 | 0.2370 | 0.2667 | 0.045* | |
C3 | 0.0556 (3) | 0.3824 (3) | 0.31604 (15) | 0.0305 (7) | |
H3B | 0.0741 | 0.3291 | 0.3621 | 0.037* | |
H3A | 0.0895 | 0.4441 | 0.3199 | 0.037* | |
C4 | −0.0955 (3) | 0.4296 (2) | 0.29238 (13) | 0.0207 (6) | |
C5 | −0.2152 (3) | 0.4762 (2) | 0.33478 (13) | 0.0201 (6) | |
C6 | −0.2140 (3) | 0.4911 (2) | 0.40460 (14) | 0.0260 (6) | |
H6A | −0.1281 | 0.4727 | 0.4304 | 0.031* | |
C7 | −0.3401 (3) | 0.5333 (2) | 0.43650 (14) | 0.0300 (7) | |
H7A | −0.3410 | 0.5441 | 0.4844 | 0.036* | |
C8 | −0.4657 (3) | 0.5600 (2) | 0.39806 (14) | 0.0279 (7) | |
H8A | −0.5526 | 0.5876 | 0.4196 | 0.033* | |
C9 | −0.4606 (3) | 0.5453 (2) | 0.32789 (13) | 0.0207 (6) | |
C10 | −0.5794 (3) | 0.5703 (2) | 0.27844 (13) | 0.0194 (6) | |
C11 | −0.7297 (3) | 0.6159 (2) | 0.29375 (16) | 0.0298 (7) | |
H11B | −0.7589 | 0.6934 | 0.3059 | 0.036* | |
H11A | −0.7509 | 0.5644 | 0.3330 | 0.036* | |
C12 | −0.7984 (4) | 0.6189 (4) | 0.2245 (2) | 0.0662 (13) | |
H12A | −0.8451 | 0.5634 | 0.2306 | 0.079* | |
H12B | −0.8695 | 0.6964 | 0.2073 | 0.079* | |
C13 | −0.6898 (3) | 0.5892 (3) | 0.17359 (17) | 0.0354 (8) | |
H13A | −0.7026 | 0.6565 | 0.1361 | 0.043* | |
H13B | −0.6941 | 0.5265 | 0.1509 | 0.043* | |
C14 | −0.3792 (3) | 0.2724 (2) | 0.32271 (13) | 0.0205 (6) | |
C15 | −0.2740 (3) | 0.2451 (2) | 0.37607 (14) | 0.0274 (7) | |
H15 | −0.1804 | 0.2315 | 0.3639 | 0.033* | |
C16 | −0.3081 (4) | 0.2380 (2) | 0.44705 (15) | 0.0376 (9) | |
H16 | −0.2372 | 0.2192 | 0.4833 | 0.045* | |
C17 | −0.4428 (4) | 0.2578 (3) | 0.46471 (16) | 0.0403 (9) | |
H17 | −0.4644 | 0.2512 | 0.5133 | 0.048* | |
C18 | −0.5479 (4) | 0.2872 (3) | 0.41265 (16) | 0.0375 (8) | |
H18 | −0.6416 | 0.3022 | 0.4253 | 0.045* | |
C19 | −0.5153 (3) | 0.2948 (2) | 0.34154 (14) | 0.0265 (7) | |
H19 | −0.5874 | 0.3155 | 0.3056 | 0.032* | |
C20 | −0.4688 (3) | 0.2626 (2) | 0.18366 (13) | 0.0180 (5) | |
C21 | −0.4885 (3) | 0.1599 (2) | 0.20761 (15) | 0.0260 (6) | |
H21 | −0.4343 | 0.1077 | 0.2476 | 0.031* | |
C22 | −0.5870 (3) | 0.1345 (3) | 0.17295 (16) | 0.0331 (7) | |
H22 | −0.5995 | 0.0647 | 0.1891 | 0.040* | |
C23 | −0.6678 (3) | 0.2106 (3) | 0.11466 (15) | 0.0315 (7) | |
H23 | −0.7365 | 0.1936 | 0.0917 | 0.038* | |
C24 | −0.6475 (3) | 0.3108 (3) | 0.09039 (14) | 0.0271 (7) | |
H24 | −0.7018 | 0.3626 | 0.0503 | 0.033* | |
C25 | −0.5479 (3) | 0.3361 (2) | 0.12445 (13) | 0.0205 (6) | |
H25 | −0.5337 | 0.4048 | 0.1069 | 0.025* | |
C26 | −0.1784 (3) | 0.1691 (2) | 0.22190 (14) | 0.0231 (6) | |
C27 | −0.1401 (3) | 0.0658 (2) | 0.27067 (16) | 0.0341 (8) | |
H27 | −0.1931 | 0.0605 | 0.3111 | 0.041* | |
C28 | −0.0241 (4) | −0.0289 (3) | 0.25957 (19) | 0.0459 (10) | |
H28 | 0.0017 | −0.0988 | 0.2925 | 0.055* | |
C29 | 0.0536 (4) | −0.0215 (3) | 0.2008 (2) | 0.0465 (10) | |
H29 | 0.1336 | −0.0860 | 0.1940 | 0.056* | |
C30 | 0.0154 (3) | 0.0792 (3) | 0.15200 (19) | 0.0386 (8) | |
H30 | 0.0684 | 0.0837 | 0.1114 | 0.046* | |
C31 | −0.1011 (3) | 0.1744 (2) | 0.16249 (15) | 0.0269 (7) | |
H31 | −0.1276 | 0.2434 | 0.1287 | 0.032* | |
C32 | −0.4927 (3) | 0.7657 (2) | 0.08809 (13) | 0.0176 (5) | |
C33 | −0.5546 (3) | 0.7164 (2) | 0.04652 (13) | 0.0182 (5) | |
H33 | −0.5272 | 0.6355 | 0.0544 | 0.022* | |
C34 | −0.6564 (3) | 0.7844 (2) | −0.00655 (14) | 0.0226 (6) | |
H34 | −0.6975 | 0.7496 | −0.0348 | 0.027* | |
C35 | −0.6979 (3) | 0.9020 (2) | −0.01836 (14) | 0.0253 (6) | |
H35 | −0.7682 | 0.9481 | −0.0542 | 0.030* | |
C36 | −0.6364 (3) | 0.9528 (2) | 0.02235 (15) | 0.0281 (7) | |
H36 | −0.6648 | 1.0338 | 0.0143 | 0.034* | |
C37 | −0.5340 (3) | 0.8857 (2) | 0.07471 (14) | 0.0234 (6) | |
H37 | −0.4913 | 0.9209 | 0.1018 | 0.028* | |
C38 | −0.2047 (3) | 0.7040 (2) | 0.11919 (13) | 0.0180 (6) | |
C39 | −0.1714 (3) | 0.7977 (2) | 0.12716 (15) | 0.0237 (6) | |
H39 | −0.2238 | 0.8489 | 0.1571 | 0.028* | |
C40 | −0.0618 (3) | 0.8159 (2) | 0.09139 (16) | 0.0304 (7) | |
H40 | −0.0392 | 0.8793 | 0.0975 | 0.036* | |
C41 | 0.0149 (3) | 0.7432 (3) | 0.04702 (16) | 0.0326 (7) | |
H41 | 0.0891 | 0.7568 | 0.0225 | 0.039* | |
C42 | −0.0176 (3) | 0.6502 (3) | 0.03867 (15) | 0.0308 (7) | |
H42 | 0.0343 | 0.5998 | 0.0082 | 0.037* | |
C43 | −0.1253 (3) | 0.6307 (2) | 0.07467 (14) | 0.0236 (6) | |
H43 | −0.1458 | 0.5661 | 0.0691 | 0.028* | |
C44 | −0.4053 (3) | 0.7597 (2) | 0.22992 (13) | 0.0189 (6) | |
C45 | −0.5466 (3) | 0.8159 (2) | 0.24115 (14) | 0.0244 (6) | |
H45 | −0.6158 | 0.8165 | 0.2088 | 0.029* | |
C46 | −0.5872 (3) | 0.8711 (2) | 0.29909 (15) | 0.0301 (7) | |
H46 | −0.6836 | 0.9090 | 0.3062 | 0.036* | |
C47 | −0.4876 (4) | 0.8708 (2) | 0.34613 (15) | 0.0351 (8) | |
H47 | −0.5151 | 0.9102 | 0.3850 | 0.042* | |
C48 | −0.3472 (4) | 0.8131 (2) | 0.33677 (15) | 0.0341 (8) | |
H48 | −0.2787 | 0.8118 | 0.3698 | 0.041* | |
C49 | −0.3058 (3) | 0.7570 (2) | 0.27932 (14) | 0.0253 (6) | |
H49 | −0.2093 | 0.7166 | 0.2737 | 0.030* | |
C1S | 0.1556 (4) | 0.0706 (3) | 0.49170 (19) | 0.0462 (9) | |
H1S1 | 0.0909 | 0.1466 | 0.5001 | 0.055* | |
H1S2 | 0.1499 | 0.0122 | 0.5315 | 0.055* | |
N1 | −0.1209 (2) | 0.42621 (17) | 0.22674 (11) | 0.0178 (5) | |
N2 | −0.3378 (2) | 0.50453 (16) | 0.29666 (10) | 0.0160 (5) | |
N3 | −0.5526 (2) | 0.55202 (18) | 0.21366 (11) | 0.0201 (5) | |
F1 | 0.0647 (3) | 0.32271 (18) | −0.47325 (12) | 0.0669 (7) | |
F2 | 0.0194 (4) | 0.3034 (4) | −0.35282 (17) | 0.0556 (10) | 0.70 |
F3 | −0.1141 (4) | 0.4557 (2) | −0.43033 (15) | 0.0537 (8) | 0.70 |
F4 | −0.1154 (5) | 0.2822 (5) | −0.4341 (2) | 0.0742 (12) | 0.70 |
F5 | −0.0022 (14) | 0.2113 (7) | −0.3939 (5) | 0.093 (4) | 0.30 |
F6 | −0.1726 (8) | 0.3757 (13) | −0.4432 (4) | 0.089 (4) | 0.30 |
F7 | 0.0037 (10) | 0.3768 (9) | −0.3746 (5) | 0.065 (3) | 0.30 |
P1 | −0.33733 (7) | 0.29524 (5) | 0.22936 (3) | 0.01592 (15) | |
P2 | −0.35576 (7) | 0.67793 (5) | 0.15724 (3) | 0.01494 (14) | |
Cl1 | −0.30326 (7) | 0.44977 (5) | 0.07328 (3) | 0.01897 (14) | |
Cl2 | 0.10273 (11) | 0.04416 (10) | 0.41220 (5) | 0.0633 (3) | |
Cl3 | 0.32484 (12) | 0.06745 (11) | 0.49062 (8) | 0.0831 (4) | |
B1 | −0.0340 (4) | 0.3352 (3) | −0.42247 (18) | 0.0362 (9) | |
Ru | −0.33465 (2) | 0.484403 (17) | 0.196759 (10) | 0.01416 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0127 (15) | 0.0338 (16) | 0.0263 (14) | −0.0060 (12) | 0.0026 (11) | −0.0110 (12) |
C2 | 0.0192 (17) | 0.051 (2) | 0.0361 (17) | −0.0044 (14) | −0.0031 (13) | −0.0137 (15) |
C3 | 0.0225 (17) | 0.0388 (17) | 0.0282 (15) | −0.0079 (13) | −0.0058 (12) | −0.0087 (13) |
C4 | 0.0214 (16) | 0.0219 (14) | 0.0185 (13) | −0.0078 (11) | −0.0006 (11) | −0.0038 (10) |
C5 | 0.0251 (16) | 0.0173 (13) | 0.0177 (13) | −0.0075 (11) | 0.0006 (11) | −0.0034 (10) |
C6 | 0.0333 (18) | 0.0268 (15) | 0.0199 (14) | −0.0135 (13) | −0.0011 (12) | −0.0041 (11) |
C7 | 0.044 (2) | 0.0336 (16) | 0.0162 (13) | −0.0165 (14) | 0.0075 (12) | −0.0092 (12) |
C8 | 0.0336 (19) | 0.0284 (15) | 0.0223 (14) | −0.0113 (13) | 0.0129 (12) | −0.0077 (12) |
C9 | 0.0237 (16) | 0.0165 (13) | 0.0206 (13) | −0.0062 (11) | 0.0063 (11) | −0.0031 (10) |
C10 | 0.0181 (15) | 0.0139 (12) | 0.0232 (14) | −0.0048 (11) | 0.0080 (11) | 0.0007 (10) |
C11 | 0.0211 (17) | 0.0264 (15) | 0.0385 (17) | −0.0065 (12) | 0.0133 (13) | −0.0037 (12) |
C12 | 0.019 (2) | 0.120 (4) | 0.044 (2) | −0.011 (2) | 0.0018 (16) | −0.008 (2) |
C13 | 0.0136 (16) | 0.053 (2) | 0.0398 (18) | −0.0120 (14) | 0.0011 (13) | −0.0112 (15) |
C14 | 0.0291 (17) | 0.0154 (13) | 0.0174 (13) | −0.0098 (11) | −0.0010 (11) | −0.0005 (10) |
C15 | 0.0355 (18) | 0.0211 (14) | 0.0221 (14) | −0.0081 (12) | −0.0068 (12) | 0.0001 (11) |
C16 | 0.065 (3) | 0.0252 (16) | 0.0183 (14) | −0.0137 (15) | −0.0129 (15) | 0.0024 (12) |
C17 | 0.072 (3) | 0.0316 (17) | 0.0183 (15) | −0.0213 (17) | 0.0104 (16) | −0.0043 (12) |
C18 | 0.053 (2) | 0.0338 (17) | 0.0283 (16) | −0.0193 (16) | 0.0148 (15) | −0.0072 (13) |
C19 | 0.0342 (19) | 0.0255 (15) | 0.0221 (14) | −0.0146 (13) | 0.0029 (12) | −0.0032 (11) |
C20 | 0.0157 (14) | 0.0219 (13) | 0.0184 (12) | −0.0079 (11) | 0.0034 (10) | −0.0078 (10) |
C21 | 0.0338 (18) | 0.0191 (14) | 0.0261 (14) | −0.0116 (12) | 0.0009 (12) | −0.0032 (11) |
C22 | 0.040 (2) | 0.0289 (16) | 0.0396 (17) | −0.0210 (14) | 0.0092 (14) | −0.0137 (13) |
C23 | 0.0296 (18) | 0.0442 (18) | 0.0321 (16) | −0.0211 (15) | 0.0068 (13) | −0.0207 (14) |
C24 | 0.0238 (17) | 0.0409 (17) | 0.0186 (13) | −0.0136 (13) | 0.0013 (11) | −0.0071 (12) |
C25 | 0.0201 (15) | 0.0262 (14) | 0.0168 (12) | −0.0109 (11) | 0.0024 (10) | −0.0032 (10) |
C26 | 0.0207 (16) | 0.0190 (13) | 0.0276 (14) | −0.0036 (11) | −0.0062 (11) | −0.0072 (11) |
C27 | 0.041 (2) | 0.0209 (15) | 0.0339 (16) | −0.0044 (13) | −0.0059 (14) | −0.0038 (12) |
C28 | 0.046 (2) | 0.0227 (16) | 0.053 (2) | 0.0047 (15) | −0.0171 (18) | −0.0068 (15) |
C29 | 0.0274 (19) | 0.0356 (19) | 0.064 (2) | 0.0089 (15) | −0.0116 (17) | −0.0230 (17) |
C30 | 0.0224 (18) | 0.0420 (19) | 0.052 (2) | −0.0063 (14) | 0.0036 (15) | −0.0229 (16) |
C31 | 0.0211 (16) | 0.0258 (15) | 0.0313 (15) | −0.0040 (12) | −0.0040 (12) | −0.0097 (12) |
C32 | 0.0162 (14) | 0.0197 (13) | 0.0163 (12) | −0.0059 (11) | 0.0032 (10) | −0.0040 (10) |
C33 | 0.0172 (15) | 0.0174 (13) | 0.0194 (13) | −0.0057 (11) | 0.0030 (10) | −0.0040 (10) |
C34 | 0.0196 (16) | 0.0274 (14) | 0.0215 (13) | −0.0088 (12) | 0.0001 (11) | −0.0064 (11) |
C35 | 0.0221 (16) | 0.0256 (15) | 0.0247 (14) | −0.0065 (12) | −0.0045 (12) | −0.0004 (11) |
C36 | 0.0305 (18) | 0.0195 (14) | 0.0306 (15) | −0.0066 (12) | −0.0036 (13) | −0.0007 (11) |
C37 | 0.0283 (17) | 0.0204 (14) | 0.0228 (14) | −0.0109 (12) | −0.0026 (11) | −0.0030 (11) |
C38 | 0.0138 (14) | 0.0208 (13) | 0.0175 (12) | −0.0061 (11) | −0.0031 (10) | 0.0006 (10) |
C39 | 0.0196 (16) | 0.0203 (14) | 0.0299 (15) | −0.0070 (11) | −0.0014 (12) | −0.0022 (11) |
C40 | 0.0259 (18) | 0.0231 (15) | 0.0416 (17) | −0.0123 (13) | −0.0068 (14) | 0.0032 (13) |
C41 | 0.0182 (17) | 0.0446 (19) | 0.0317 (16) | −0.0137 (14) | 0.0006 (12) | 0.0068 (13) |
C42 | 0.0259 (18) | 0.0396 (17) | 0.0260 (15) | −0.0109 (14) | 0.0070 (12) | −0.0077 (13) |
C43 | 0.0221 (16) | 0.0288 (15) | 0.0227 (14) | −0.0120 (12) | 0.0026 (11) | −0.0066 (11) |
C44 | 0.0257 (16) | 0.0137 (12) | 0.0161 (12) | −0.0058 (11) | 0.0012 (11) | −0.0032 (10) |
C45 | 0.0284 (17) | 0.0232 (14) | 0.0216 (14) | −0.0093 (12) | 0.0051 (12) | −0.0055 (11) |
C46 | 0.0361 (19) | 0.0230 (14) | 0.0260 (15) | −0.0053 (13) | 0.0103 (13) | −0.0053 (12) |
C47 | 0.055 (2) | 0.0257 (15) | 0.0219 (15) | −0.0093 (15) | 0.0089 (14) | −0.0107 (12) |
C48 | 0.049 (2) | 0.0307 (16) | 0.0222 (15) | −0.0126 (15) | −0.0068 (14) | −0.0080 (12) |
C49 | 0.0302 (17) | 0.0217 (14) | 0.0216 (13) | −0.0065 (12) | −0.0011 (12) | −0.0052 (11) |
C1S | 0.044 (2) | 0.043 (2) | 0.053 (2) | −0.0170 (17) | 0.0059 (17) | −0.0146 (17) |
N1 | 0.0160 (12) | 0.0191 (11) | 0.0187 (11) | −0.0063 (9) | 0.0008 (9) | −0.0048 (9) |
N2 | 0.0178 (12) | 0.0130 (10) | 0.0169 (10) | −0.0059 (9) | 0.0023 (9) | −0.0015 (8) |
N3 | 0.0155 (13) | 0.0186 (11) | 0.0252 (12) | −0.0064 (9) | 0.0033 (9) | −0.0020 (9) |
F1 | 0.0765 (18) | 0.0539 (13) | 0.0588 (14) | −0.0112 (12) | 0.0409 (12) | −0.0144 (11) |
F2 | 0.0293 (18) | 0.092 (3) | 0.0322 (17) | −0.013 (2) | −0.0037 (12) | 0.0031 (19) |
F3 | 0.070 (2) | 0.0384 (16) | 0.0379 (16) | −0.0048 (16) | 0.0158 (15) | −0.0055 (13) |
F4 | 0.085 (3) | 0.097 (3) | 0.075 (3) | −0.060 (3) | 0.012 (3) | −0.047 (3) |
F5 | 0.161 (11) | 0.050 (5) | 0.067 (6) | −0.042 (6) | 0.054 (6) | −0.002 (4) |
F6 | 0.034 (5) | 0.180 (12) | 0.017 (3) | −0.010 (6) | −0.002 (3) | 0.004 (6) |
F7 | 0.063 (7) | 0.097 (7) | 0.075 (7) | −0.057 (7) | 0.036 (5) | −0.058 (6) |
P1 | 0.0168 (4) | 0.0146 (3) | 0.0148 (3) | −0.0047 (3) | −0.0007 (3) | −0.0014 (2) |
P2 | 0.0152 (4) | 0.0153 (3) | 0.0144 (3) | −0.0053 (3) | 0.0013 (3) | −0.0041 (2) |
Cl1 | 0.0224 (4) | 0.0203 (3) | 0.0160 (3) | −0.0090 (3) | 0.0029 (2) | −0.0060 (2) |
Cl2 | 0.0473 (6) | 0.0798 (7) | 0.0562 (6) | −0.0118 (5) | −0.0078 (5) | −0.0225 (5) |
Cl3 | 0.0437 (7) | 0.0918 (8) | 0.1381 (11) | −0.0302 (6) | 0.0150 (7) | −0.0743 (8) |
B1 | 0.037 (2) | 0.043 (2) | 0.0258 (18) | −0.0130 (18) | 0.0043 (15) | −0.0019 (16) |
Ru | 0.01295 (12) | 0.01588 (11) | 0.01338 (10) | −0.00467 (8) | 0.00122 (7) | −0.00377 (7) |
C1—N1 | 1.483 (3) | C30—C31 | 1.396 (4) |
C1—C2 | 1.535 (4) | C32—C33 | 1.389 (4) |
C2—C3 | 1.542 (4) | C32—C37 | 1.408 (4) |
C3—C4 | 1.492 (4) | C32—P2 | 1.836 (3) |
C4—N1 | 1.298 (3) | C33—C34 | 1.392 (4) |
C4—C5 | 1.458 (4) | C34—C35 | 1.379 (4) |
C5—N2 | 1.364 (3) | C35—C36 | 1.388 (4) |
C5—C6 | 1.382 (4) | C36—C37 | 1.385 (4) |
C6—C7 | 1.387 (4) | C38—C39 | 1.396 (4) |
C7—C8 | 1.397 (4) | C38—C43 | 1.398 (4) |
C8—C9 | 1.385 (4) | C38—P2 | 1.832 (3) |
C9—N2 | 1.352 (3) | C39—C40 | 1.389 (4) |
C9—C10 | 1.463 (4) | C40—C41 | 1.382 (4) |
C10—N3 | 1.307 (3) | C41—C42 | 1.385 (4) |
C10—C11 | 1.485 (4) | C42—C43 | 1.380 (4) |
C11—C12 | 1.500 (5) | C44—C49 | 1.393 (4) |
C12—C13 | 1.458 (5) | C44—C45 | 1.396 (4) |
C13—N3 | 1.491 (4) | C44—P2 | 1.834 (2) |
C14—C19 | 1.382 (4) | C45—C46 | 1.391 (4) |
C14—C15 | 1.404 (4) | C46—C47 | 1.376 (5) |
C14—P1 | 1.833 (3) | C47—C48 | 1.384 (5) |
C15—C16 | 1.395 (4) | C48—C49 | 1.389 (4) |
C16—C17 | 1.367 (5) | C1S—Cl3 | 1.734 (4) |
C17—C18 | 1.382 (5) | C1S—Cl2 | 1.750 (4) |
C18—C19 | 1.393 (4) | N1—Ru | 2.102 (2) |
C20—C25 | 1.387 (4) | N2—Ru | 1.970 (2) |
C20—C21 | 1.405 (4) | N3—Ru | 2.131 (2) |
C20—P1 | 1.835 (3) | F1—B1 | 1.383 (4) |
C21—C22 | 1.387 (4) | F2—B1 | 1.383 (5) |
C22—C23 | 1.391 (4) | F3—B1 | 1.433 (5) |
C23—C24 | 1.378 (4) | F4—B1 | 1.305 (5) |
C24—C25 | 1.390 (4) | F5—B1 | 1.496 (9) |
C26—C31 | 1.388 (4) | F6—B1 | 1.367 (9) |
C26—C27 | 1.405 (4) | F7—B1 | 1.267 (9) |
C26—P1 | 1.844 (3) | P1—Ru | 2.4051 (7) |
C27—C28 | 1.392 (4) | P2—Ru | 2.3902 (7) |
C28—C29 | 1.384 (6) | Cl1—Ru | 2.4717 (6) |
C29—C30 | 1.381 (5) | ||
N1—C1—C2 | 104.1 (2) | C46—C45—C44 | 120.9 (3) |
C1—C2—C3 | 103.5 (2) | C47—C46—C45 | 119.9 (3) |
C4—C3—C2 | 100.8 (2) | C46—C47—C48 | 120.0 (3) |
N1—C4—C5 | 117.5 (2) | C47—C48—C49 | 120.4 (3) |
N1—C4—C3 | 115.1 (2) | C48—C49—C44 | 120.3 (3) |
C5—C4—C3 | 127.4 (2) | Cl3—C1S—Cl2 | 112.3 (2) |
N2—C5—C6 | 121.2 (3) | C4—N1—C1 | 109.0 (2) |
N2—C5—C4 | 111.1 (2) | C4—N1—Ru | 114.18 (17) |
C6—C5—C4 | 127.8 (3) | C1—N1—Ru | 136.83 (16) |
C5—C6—C7 | 119.0 (3) | C9—N2—C5 | 119.8 (2) |
C6—C7—C8 | 120.0 (2) | C9—N2—Ru | 120.45 (17) |
C9—C8—C7 | 118.5 (3) | C5—N2—Ru | 119.79 (17) |
N2—C9—C8 | 121.6 (3) | C10—N3—C13 | 107.1 (2) |
N2—C9—C10 | 111.4 (2) | C10—N3—Ru | 113.10 (18) |
C8—C9—C10 | 127.0 (3) | C13—N3—Ru | 139.78 (18) |
N3—C10—C9 | 117.7 (2) | C14—P1—C20 | 102.82 (13) |
N3—C10—C11 | 115.6 (2) | C14—P1—C26 | 104.60 (12) |
C9—C10—C11 | 126.7 (2) | C20—P1—C26 | 100.82 (11) |
C10—C11—C12 | 101.8 (2) | C14—P1—Ru | 109.35 (8) |
C13—C12—C11 | 107.7 (3) | C20—P1—Ru | 117.60 (9) |
C12—C13—N3 | 107.2 (3) | C26—P1—Ru | 119.68 (10) |
C19—C14—C15 | 119.2 (3) | C44—P2—C38 | 106.04 (12) |
C19—C14—P1 | 121.1 (2) | C44—P2—C32 | 101.99 (11) |
C15—C14—P1 | 119.2 (2) | C38—P2—C32 | 100.60 (12) |
C16—C15—C14 | 119.5 (3) | C44—P2—Ru | 110.58 (8) |
C17—C16—C15 | 120.4 (3) | C38—P2—Ru | 118.62 (8) |
C16—C17—C18 | 120.7 (3) | C32—P2—Ru | 117.14 (9) |
C17—C18—C19 | 119.4 (3) | F7—B1—F4 | 141.7 (6) |
C14—C19—C18 | 120.7 (3) | F7—B1—F6 | 118.7 (8) |
C25—C20—C21 | 118.6 (2) | F4—B1—F6 | 48.6 (6) |
C25—C20—P1 | 121.5 (2) | F7—B1—F1 | 106.6 (5) |
C21—C20—P1 | 119.9 (2) | F4—B1—F1 | 110.0 (3) |
C22—C21—C20 | 120.1 (3) | F6—B1—F1 | 119.7 (4) |
C21—C22—C23 | 120.5 (3) | F7—B1—F2 | 40.0 (5) |
C24—C23—C22 | 119.7 (3) | F4—B1—F2 | 111.2 (4) |
C23—C24—C25 | 120.1 (3) | F6—B1—F2 | 125.1 (4) |
C20—C25—C24 | 121.0 (3) | F1—B1—F2 | 115.2 (3) |
C31—C26—C27 | 119.1 (3) | F7—B1—F3 | 69.5 (6) |
C31—C26—P1 | 118.1 (2) | F4—B1—F3 | 109.6 (4) |
C27—C26—P1 | 122.5 (2) | F6—B1—F3 | 61.1 (7) |
C28—C27—C26 | 119.9 (3) | F1—B1—F3 | 106.0 (3) |
C29—C28—C27 | 120.2 (3) | F2—B1—F3 | 104.5 (3) |
C30—C29—C28 | 120.3 (3) | F7—B1—F5 | 107.5 (7) |
C29—C30—C31 | 119.9 (3) | F4—B1—F5 | 56.3 (6) |
C26—C31—C30 | 120.6 (3) | F6—B1—F5 | 102.7 (9) |
C33—C32—C37 | 118.5 (2) | F1—B1—F5 | 98.9 (4) |
C33—C32—P2 | 121.50 (19) | F2—B1—F5 | 67.6 (5) |
C37—C32—P2 | 119.97 (19) | F3—B1—F5 | 154.8 (5) |
C32—C33—C34 | 120.6 (2) | N2—Ru—N1 | 77.47 (8) |
C35—C34—C33 | 120.4 (2) | N2—Ru—N3 | 77.35 (9) |
C34—C35—C36 | 119.8 (2) | N1—Ru—N3 | 154.81 (8) |
C37—C36—C35 | 120.2 (3) | N2—Ru—P2 | 91.06 (6) |
C36—C37—C32 | 120.5 (2) | N1—Ru—P2 | 93.80 (6) |
C39—C38—C43 | 118.2 (3) | N3—Ru—P2 | 86.95 (6) |
C39—C38—P2 | 124.1 (2) | N2—Ru—P1 | 91.96 (6) |
C43—C38—P2 | 117.5 (2) | N1—Ru—P1 | 92.23 (6) |
C40—C39—C38 | 120.0 (3) | N3—Ru—P1 | 88.34 (6) |
C41—C40—C39 | 121.0 (3) | P2—Ru—P1 | 173.72 (2) |
C40—C41—C42 | 119.4 (3) | N2—Ru—Cl1 | 173.88 (7) |
C43—C42—C41 | 120.0 (3) | N1—Ru—Cl1 | 96.43 (6) |
C42—C43—C38 | 121.4 (3) | N3—Ru—Cl1 | 108.75 (6) |
C49—C44—C45 | 118.5 (2) | P2—Ru—Cl1 | 89.76 (2) |
C49—C44—P2 | 121.5 (2) | P1—Ru—Cl1 | 87.82 (2) |
C45—C44—P2 | 119.6 (2) | ||
N1—C1—C2—C3 | −26.9 (3) | C15—C14—P1—C26 | 50.2 (2) |
C1—C2—C3—C4 | 24.1 (3) | C19—C14—P1—Ru | 93.2 (2) |
C2—C3—C4—N1 | −13.8 (3) | C15—C14—P1—Ru | −79.1 (2) |
C2—C3—C4—C5 | 164.9 (3) | C25—C20—P1—C14 | 131.0 (2) |
N1—C4—C5—N2 | 2.7 (3) | C21—C20—P1—C14 | −50.6 (2) |
C3—C4—C5—N2 | −176.0 (3) | C25—C20—P1—C26 | −121.2 (2) |
N1—C4—C5—C6 | −178.2 (3) | C21—C20—P1—C26 | 57.3 (2) |
C3—C4—C5—C6 | 3.2 (5) | C25—C20—P1—Ru | 10.8 (2) |
N2—C5—C6—C7 | 1.4 (4) | C21—C20—P1—Ru | −170.75 (18) |
C4—C5—C6—C7 | −177.7 (3) | C31—C26—P1—C14 | −164.3 (2) |
C5—C6—C7—C8 | 0.0 (4) | C27—C26—P1—C14 | 21.2 (3) |
C6—C7—C8—C9 | −1.2 (4) | C31—C26—P1—C20 | 89.3 (2) |
C7—C8—C9—N2 | 1.0 (4) | C27—C26—P1—C20 | −85.2 (2) |
C7—C8—C9—C10 | −178.6 (3) | C31—C26—P1—Ru | −41.4 (2) |
N2—C9—C10—N3 | −0.7 (3) | C27—C26—P1—Ru | 144.1 (2) |
C8—C9—C10—N3 | 179.0 (3) | C49—C44—P2—C38 | −46.1 (2) |
N2—C9—C10—C11 | 179.9 (2) | C45—C44—P2—C38 | 141.2 (2) |
C8—C9—C10—C11 | −0.4 (4) | C49—C44—P2—C32 | −151.0 (2) |
N3—C10—C11—C12 | 2.6 (4) | C45—C44—P2—C32 | 36.3 (2) |
C9—C10—C11—C12 | −178.0 (3) | C49—C44—P2—Ru | 83.7 (2) |
C10—C11—C12—C13 | −6.3 (4) | C45—C44—P2—Ru | −89.0 (2) |
C11—C12—C13—N3 | 7.8 (5) | C39—C38—P2—C44 | −20.8 (2) |
C19—C14—C15—C16 | 1.7 (4) | C43—C38—P2—C44 | 164.73 (19) |
P1—C14—C15—C16 | 174.1 (2) | C39—C38—P2—C32 | 85.1 (2) |
C14—C15—C16—C17 | −0.2 (4) | C43—C38—P2—C32 | −89.4 (2) |
C15—C16—C17—C18 | −1.2 (5) | C39—C38—P2—Ru | −145.83 (19) |
C16—C17—C18—C19 | 1.1 (5) | C43—C38—P2—Ru | 39.7 (2) |
C15—C14—C19—C18 | −1.8 (4) | C33—C32—P2—C44 | −138.5 (2) |
P1—C14—C19—C18 | −174.1 (2) | C37—C32—P2—C44 | 43.6 (2) |
C17—C18—C19—C14 | 0.4 (4) | C33—C32—P2—C38 | 112.5 (2) |
C25—C20—C21—C22 | −1.1 (4) | C37—C32—P2—C38 | −65.5 (2) |
P1—C20—C21—C22 | −179.6 (2) | C33—C32—P2—Ru | −17.6 (3) |
C20—C21—C22—C23 | −0.5 (4) | C37—C32—P2—Ru | 164.42 (19) |
C21—C22—C23—C24 | 1.3 (4) | C9—N2—Ru—N1 | −178.8 (2) |
C22—C23—C24—C25 | −0.6 (4) | C5—N2—Ru—N1 | 0.60 (18) |
C21—C20—C25—C24 | 1.8 (4) | C9—N2—Ru—N3 | 0.91 (18) |
P1—C20—C25—C24 | −179.7 (2) | C5—N2—Ru—N3 | −179.7 (2) |
C23—C24—C25—C20 | −1.0 (4) | C9—N2—Ru—P2 | 87.54 (18) |
C31—C26—C27—C28 | 1.2 (4) | C5—N2—Ru—P2 | −93.06 (18) |
P1—C26—C27—C28 | 175.6 (2) | C9—N2—Ru—P1 | −86.95 (18) |
C26—C27—C28—C29 | 0.1 (5) | C5—N2—Ru—P1 | 92.45 (18) |
C27—C28—C29—C30 | −1.1 (5) | C9—N2—Ru—Cl1 | −174.8 (5) |
C28—C29—C30—C31 | 0.8 (5) | C5—N2—Ru—Cl1 | 4.7 (7) |
C27—C26—C31—C30 | −1.5 (4) | C4—N1—Ru—N2 | 0.94 (18) |
P1—C26—C31—C30 | −176.2 (2) | C1—N1—Ru—N2 | −178.9 (3) |
C29—C30—C31—C26 | 0.5 (5) | C4—N1—Ru—N3 | 0.3 (3) |
C37—C32—C33—C34 | −0.8 (4) | C1—N1—Ru—N3 | −179.6 (2) |
P2—C32—C33—C34 | −178.8 (2) | C4—N1—Ru—P2 | 91.19 (18) |
C32—C33—C34—C35 | −0.4 (4) | C1—N1—Ru—P2 | −88.7 (2) |
C33—C34—C35—C36 | 0.8 (4) | C4—N1—Ru—P1 | −90.57 (18) |
C34—C35—C36—C37 | −0.1 (5) | C1—N1—Ru—P1 | 89.6 (2) |
C35—C36—C37—C32 | −1.1 (5) | C4—N1—Ru—Cl1 | −178.62 (17) |
C33—C32—C37—C36 | 1.5 (4) | C1—N1—Ru—Cl1 | 1.5 (3) |
P2—C32—C37—C36 | 179.5 (2) | C10—N3—Ru—N2 | −1.22 (17) |
C43—C38—C39—C40 | −0.1 (4) | C13—N3—Ru—N2 | 176.8 (3) |
P2—C38—C39—C40 | −174.5 (2) | C10—N3—Ru—N1 | −0.6 (3) |
C38—C39—C40—C41 | 0.7 (4) | C13—N3—Ru—N1 | 177.4 (3) |
C39—C40—C41—C42 | −0.6 (4) | C10—N3—Ru—P2 | −93.00 (17) |
C40—C41—C42—C43 | −0.2 (4) | C13—N3—Ru—P2 | 85.0 (3) |
C41—C42—C43—C38 | 0.9 (4) | C10—N3—Ru—P1 | 91.16 (17) |
C39—C38—C43—C42 | −0.7 (4) | C13—N3—Ru—P1 | −90.8 (3) |
P2—C38—C43—C42 | 174.1 (2) | C10—N3—Ru—Cl1 | 178.29 (16) |
C49—C44—C45—C46 | 2.0 (4) | C13—N3—Ru—Cl1 | −3.7 (3) |
P2—C44—C45—C46 | 175.0 (2) | C44—P2—Ru—N2 | −13.25 (12) |
C44—C45—C46—C47 | 0.1 (4) | C38—P2—Ru—N2 | 109.52 (11) |
C45—C46—C47—C48 | −1.7 (4) | C32—P2—Ru—N2 | −129.47 (11) |
C46—C47—C48—C49 | 1.2 (5) | C44—P2—Ru—N1 | −90.76 (11) |
C47—C48—C49—C44 | 1.0 (4) | C38—P2—Ru—N1 | 32.01 (11) |
C45—C44—C49—C48 | −2.5 (4) | C32—P2—Ru—N1 | 153.02 (11) |
P2—C44—C49—C48 | −175.3 (2) | C44—P2—Ru—N3 | 64.02 (11) |
C5—C4—N1—C1 | 177.7 (2) | C38—P2—Ru—N3 | −173.21 (11) |
C3—C4—N1—C1 | −3.5 (3) | C32—P2—Ru—N3 | −52.20 (11) |
C5—C4—N1—Ru | −2.2 (3) | C44—P2—Ru—P1 | 105.5 (2) |
C3—C4—N1—Ru | 176.60 (19) | C38—P2—Ru—P1 | −131.7 (2) |
C2—C1—N1—C4 | 19.5 (3) | C32—P2—Ru—P1 | −10.7 (3) |
C2—C1—N1—Ru | −160.6 (2) | C44—P2—Ru—Cl1 | 172.82 (10) |
C8—C9—N2—C5 | 0.5 (4) | C38—P2—Ru—Cl1 | −64.42 (9) |
C10—C9—N2—C5 | −179.9 (2) | C32—P2—Ru—Cl1 | 56.59 (9) |
C8—C9—N2—Ru | 179.9 (2) | C14—P1—Ru—N2 | 12.29 (12) |
C10—C9—N2—Ru | −0.5 (3) | C20—P1—Ru—N2 | 128.97 (11) |
C6—C5—N2—C9 | −1.7 (4) | C26—P1—Ru—N2 | −108.22 (11) |
C4—C5—N2—C9 | 177.6 (2) | C14—P1—Ru—N1 | 89.82 (11) |
C6—C5—N2—Ru | 178.91 (19) | C20—P1—Ru—N1 | −153.50 (11) |
C4—C5—N2—Ru | −1.8 (3) | C26—P1—Ru—N1 | −30.69 (11) |
C9—C10—N3—C13 | −177.3 (2) | C14—P1—Ru—N3 | −64.99 (12) |
C11—C10—N3—C13 | 2.2 (3) | C20—P1—Ru—N3 | 51.69 (11) |
C9—C10—N3—Ru | 1.4 (3) | C26—P1—Ru—N3 | 174.50 (11) |
C11—C10—N3—Ru | −179.16 (18) | C14—P1—Ru—P2 | −106.4 (2) |
C12—C13—N3—C10 | −6.3 (4) | C20—P1—Ru—P2 | 10.3 (3) |
C12—C13—N3—Ru | 175.7 (3) | C26—P1—Ru—P2 | 133.1 (2) |
C19—C14—P1—C20 | −32.5 (2) | C14—P1—Ru—Cl1 | −173.83 (10) |
C15—C14—P1—C20 | 155.2 (2) | C20—P1—Ru—Cl1 | −57.15 (9) |
C19—C14—P1—C26 | −137.5 (2) | C26—P1—Ru—Cl1 | 65.66 (10) |
Experimental details
Crystal data | |
Chemical formula | [Ru(C13H15N3)(C18H15P)2Cl]BF4·CH2Cl2 |
Mr | 1046.08 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 2307.8 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.5 × 0.3 × 0.15 |
Data collection | |
Diffractometer | STOE IPDS diffractometer |
Absorption correction | Part of the refinement model (ΔF) (Walker & Stuart, 1983) |
Tmin, Tmax | 0.699, 0.880 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 16304, 8322, 6363 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.614 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.076, 0.96 |
No. of reflections | 8322 |
No. of parameters | 604 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 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.
N1—Ru | 2.102 (2) | P1—Ru | 2.4051 (7) |
N2—Ru | 1.970 (2) | P2—Ru | 2.3902 (7) |
N3—Ru | 2.131 (2) | Cl1—Ru | 2.4717 (6) |
N2—Ru—N1 | 77.47 (8) | N2—Ru—Cl1 | 173.88 (7) |
N2—Ru—N3 | 77.35 (9) | N1—Ru—Cl1 | 96.43 (6) |
N1—Ru—N3 | 154.81 (8) | N3—Ru—Cl1 | 108.75 (6) |
P2—Ru—P1 | 173.72 (2) |
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.