Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802002957/tk6053sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802002957/tk6053Isup2.hkl |
CCDC reference: 182584
A mixture of Ru3(CO)12 (200 mg, 0.31 mmol) and potassium dihydrobis(1-pyrazolyl)borate (58 mg, 0.31 mmol) was dissolved in MeOH (30 ml), under an N2 atmosphere using standard Schlenk techniques. The solution was refluxed for 20 min, the solution became red–brown, and the characteristic Ru3(CO)12 absorption at νCO = 2061 cm-1 had disappeared. The solution was cooled, concentrated to 1 ml, and chromatographed on a silica-gel (60 GF254, Merck) column, using hexane as eluent, until the first yellow fraction [a mixture of Ru3(CO)12 and Ru4H4(CO)12 (15%)] separated. Then an orange–red fraction containing (I) was extracted using acetone as eluent. The product was isolated by evaporation of the solvent and recrystalization from cyclohexane, and dried in vacuo. Yield: 52%; 1H NMR (200 MHz, CDCl3): -13.42 (s, 1H), 6.23 (t, 1H), 7.24 (d, 2H); IR (KBr, cm-1, CO): 2106 (w), 2093 (w), 2069 (s), 2060 (s), 2026 (s), 2019 (m), 2011 (m), 1991 (w). An orange crystal of compound (I) was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite-monochromated radiation (Image plate distance 90 mm, ϕ oscillation scans 0–195°, step Δϕ = 0.7°, 2θ range 2.15–22.5°, dmax-dmin = 16.00–0.93 Å).
The hydride ions were located from difference Fourier maps and fixed in their positions, while the remaining H atoms were included in calculated positions and treated as riding atoms using SHELXL97 default parameters. [Please describe what the extra C1.5H3 in the chemical formula is and indicate how best this can be described in the name and formula]
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.
Fig. 1. The molecular structure of one molecule of [Ru3(µ-H)(µ-N2C3H3)(CO)10]. Displacement ellipsoids are drawn at the 50% probability level. |
[Ru3H(C3H3N2)(CO)10]·C1.50H3 | F(000) = 5120 |
Mr = 672.43 | Dx = 2.290 Mg m−3 |
Monoclinic, I2/a | Mo Kα radiation, λ = 0.71073 Å |
a = 14.2248 (11) Å | Cell parameters from 8000 reflections |
b = 9.1670 (5) Å | θ = 2.2–22.5° |
c = 59.834 (5) Å | µ = 2.35 mm−1 |
β = 90.380 (9)° | T = 153 K |
V = 7802.1 (10) Å3 | Block, orange |
Z = 16 | 0.50 × 0.45 × 0.40 mm |
Stoe IPDS diffractometer | 4743 independent reflections |
Radiation source: fine-focus sealed tube | 4474 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 0 pixels mm-1 | θmax = 22.3°, θmin = 2.0° |
ϕ oscillation scans | h = −15→15 |
Absorption correction: multi-scan (Blessing, 1995) | k = −8→9 |
Tmin = 0.224, Tmax = 0.251 | l = −60→63 |
18544 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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.36 | w = 1/[σ2(Fo2) + 252.1712P] where P = (Fo2 + 2Fc2)/3 |
4743 reflections | (Δ/σ)max < 0.001 |
532 parameters | Δρmax = 1.00 e Å−3 |
0 restraints | Δρmin = −0.81 e Å−3 |
[Ru3H(C3H3N2)(CO)10]·C1.50H3 | V = 7802.1 (10) Å3 |
Mr = 672.43 | Z = 16 |
Monoclinic, I2/a | Mo Kα radiation |
a = 14.2248 (11) Å | µ = 2.35 mm−1 |
b = 9.1670 (5) Å | T = 153 K |
c = 59.834 (5) Å | 0.50 × 0.45 × 0.40 mm |
β = 90.380 (9)° |
Stoe IPDS diffractometer | 4743 independent reflections |
Absorption correction: multi-scan (Blessing, 1995) | 4474 reflections with I > 2σ(I) |
Tmin = 0.224, Tmax = 0.251 | Rint = 0.041 |
18544 measured reflections | θmax = 22.3° |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.36 | w = 1/[σ2(Fo2) + 252.1712P] where P = (Fo2 + 2Fc2)/3 |
4743 reflections | Δρmax = 1.00 e Å−3 |
532 parameters | Δρmin = −0.81 e Å−3 |
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 | ||
Ru1 | 0.49279 (6) | 0.94266 (9) | 0.053746 (13) | 0.0155 (2) | |
H1 | 0.4462 | 0.8556 | 0.0760 | 0.050* | |
Ru2 | 0.50356 (5) | 0.69385 (9) | 0.083565 (13) | 0.0163 (2) | |
Ru3 | 0.54938 (6) | 0.66363 (9) | 0.037485 (13) | 0.0181 (2) | |
Ru4 | 0.66421 (6) | 1.32018 (10) | 0.197832 (13) | 0.0203 (2) | |
H2 | 0.7280 | 1.2394 | 0.1809 | 0.050* | |
Ru5 | 0.66041 (6) | 1.15837 (10) | 0.155947 (13) | 0.0201 (2) | |
Ru6 | 0.52559 (6) | 1.37891 (10) | 0.164521 (14) | 0.0198 (2) | |
C1 | 0.3754 (8) | 0.9254 (12) | 0.03840 (16) | 0.020 (2) | |
C2 | 0.5550 (7) | 1.0169 (12) | 0.02797 (18) | 0.021 (2) | |
C3 | 0.4572 (7) | 1.1287 (13) | 0.06658 (17) | 0.022 (3) | |
C4 | 0.4754 (7) | 0.7340 (12) | 0.11441 (18) | 0.019 (2) | |
C5 | 0.5716 (8) | 0.5154 (14) | 0.08797 (19) | 0.028 (3) | |
C6 | 0.3902 (8) | 0.5900 (13) | 0.07846 (17) | 0.024 (3) | |
C7 | 0.6760 (8) | 0.7253 (11) | 0.04577 (17) | 0.021 (2) | |
C8 | 0.5872 (8) | 0.4611 (15) | 0.03824 (17) | 0.027 (3) | |
C9 | 0.4172 (9) | 0.6159 (13) | 0.03119 (18) | 0.030 (3) | |
C10 | 0.5720 (8) | 0.7080 (12) | 0.00662 (18) | 0.026 (3) | |
C11 | 0.7179 (8) | 1.5032 (16) | 0.19033 (18) | 0.033 (3) | |
C12 | 0.5831 (8) | 1.4084 (14) | 0.21910 (18) | 0.032 (3) | |
C13 | 0.7653 (8) | 1.2709 (13) | 0.21846 (19) | 0.027 (3) | |
C14 | 0.7531 (9) | 1.0064 (15) | 0.15208 (18) | 0.034 (3) | |
C15 | 0.5716 (8) | 1.0957 (13) | 0.13378 (19) | 0.030 (3) | |
C16 | 0.7224 (7) | 1.2771 (13) | 0.13502 (18) | 0.026 (3) | |
C17 | 0.4534 (8) | 1.2308 (13) | 0.18054 (18) | 0.026 (3) | |
C18 | 0.4464 (8) | 1.3675 (12) | 0.1384 (2) | 0.027 (3) | |
C19 | 0.6121 (8) | 1.5101 (14) | 0.15011 (18) | 0.028 (3) | |
C20 | 0.4618 (8) | 1.5336 (15) | 0.17916 (19) | 0.033 (3) | |
C21 | 0.6877 (7) | 1.0353 (12) | 0.07774 (17) | 0.021 (2) | |
H21A | 0.6995 | 1.1257 | 0.0705 | 0.025* | |
C22 | 0.7444 (7) | 0.9723 (12) | 0.09416 (16) | 0.022 (2) | |
H22A | 0.8008 | 1.0107 | 0.1004 | 0.026* | |
C23 | 0.7016 (7) | 0.8439 (13) | 0.09942 (16) | 0.023 (3) | |
H23A | 0.7238 | 0.7757 | 0.1102 | 0.028* | |
C24 | 0.5712 (8) | 1.0272 (13) | 0.21818 (18) | 0.028 (3) | |
H24A | 0.5663 | 1.0524 | 0.2335 | 0.034* | |
C25 | 0.5437 (9) | 0.8955 (14) | 0.20850 (19) | 0.037 (3) | |
H25A | 0.5166 | 0.8142 | 0.2159 | 0.045* | |
C26 | 0.5635 (9) | 0.9066 (13) | 0.1861 (2) | 0.035 (3) | |
H26A | 0.5524 | 0.8337 | 0.1751 | 0.042* | |
C27 | 0.2375 (14) | 1.095 (3) | 0.2549 (3) | 0.094 (7) | |
H27A | 0.2803 | 1.0695 | 0.2674 | 0.112* | |
H27B | 0.1990 | 1.0089 | 0.2509 | 0.112* | |
C28 | 0.2835 (17) | 1.143 (3) | 0.2379 (4) | 0.114 (9) | |
H28A | 0.2415 | 1.1392 | 0.2247 | 0.137* | |
H28B | 0.3363 | 1.0749 | 0.2351 | 0.137* | |
C29 | 0.3199 (13) | 1.283 (2) | 0.2397 (3) | 0.071 (5) | |
H29A | 0.3498 | 1.3060 | 0.2252 | 0.085* | |
H29B | 0.3709 | 1.2797 | 0.2510 | 0.085* | |
N1 | 0.6142 (5) | 0.9482 (9) | 0.07381 (12) | 0.0159 (19) | |
N2 | 0.6224 (5) | 0.8288 (9) | 0.08690 (13) | 0.0169 (19) | |
N3 | 0.6061 (6) | 1.1120 (10) | 0.20190 (14) | 0.026 (2) | |
N4 | 0.6011 (6) | 1.0382 (10) | 0.18253 (13) | 0.023 (2) | |
O1 | 0.3039 (6) | 0.9206 (9) | 0.03019 (12) | 0.033 (2) | |
O2 | 0.5914 (5) | 1.0604 (9) | 0.01271 (12) | 0.0288 (18) | |
O3 | 0.4389 (5) | 1.2394 (9) | 0.07338 (13) | 0.0325 (19) | |
O4 | 0.4596 (5) | 0.7516 (9) | 0.13268 (12) | 0.0314 (19) | |
O5 | 0.6096 (6) | 0.4095 (9) | 0.09149 (13) | 0.034 (2) | |
O6 | 0.3197 (5) | 0.5326 (9) | 0.07603 (13) | 0.035 (2) | |
O7 | 0.7524 (5) | 0.7570 (9) | 0.04826 (12) | 0.0302 (18) | |
O8 | 0.6109 (6) | 0.3441 (10) | 0.03819 (14) | 0.041 (2) | |
O9 | 0.3432 (6) | 0.5910 (10) | 0.02628 (15) | 0.043 (2) | |
O10 | 0.5891 (6) | 0.7327 (10) | −0.01142 (13) | 0.040 (2) | |
O11 | 0.7521 (6) | 1.6126 (10) | 0.18675 (15) | 0.042 (2) | |
O12 | 0.5340 (6) | 1.4612 (11) | 0.23173 (16) | 0.055 (3) | |
O13 | 0.8245 (6) | 1.2498 (10) | 0.23048 (14) | 0.043 (2) | |
O14 | 0.8065 (7) | 0.9177 (12) | 0.14830 (15) | 0.059 (3) | |
O15 | 0.5196 (6) | 1.0610 (9) | 0.12020 (13) | 0.035 (2) | |
O16 | 0.7650 (6) | 1.3439 (10) | 0.12222 (14) | 0.042 (2) | |
O17 | 0.4052 (5) | 1.1532 (9) | 0.18943 (12) | 0.0290 (18) | |
O18 | 0.3959 (6) | 1.3631 (10) | 0.12307 (13) | 0.037 (2) | |
O19 | 0.6581 (6) | 1.5964 (10) | 0.14171 (14) | 0.040 (2) | |
O20 | 0.4223 (6) | 1.6284 (10) | 0.18783 (17) | 0.050 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0197 (5) | 0.0140 (5) | 0.0130 (4) | 0.0018 (3) | −0.0001 (3) | 0.0002 (3) |
Ru2 | 0.0180 (4) | 0.0158 (5) | 0.0151 (4) | −0.0007 (3) | 0.0004 (3) | 0.0008 (3) |
Ru3 | 0.0219 (5) | 0.0163 (5) | 0.0161 (4) | 0.0008 (4) | 0.0006 (3) | −0.0038 (3) |
Ru4 | 0.0202 (5) | 0.0240 (6) | 0.0167 (4) | −0.0033 (4) | 0.0022 (3) | −0.0021 (4) |
Ru5 | 0.0230 (5) | 0.0227 (6) | 0.0147 (4) | 0.0039 (4) | 0.0016 (3) | 0.0000 (4) |
Ru6 | 0.0196 (5) | 0.0190 (5) | 0.0209 (5) | −0.0006 (4) | 0.0019 (4) | −0.0002 (4) |
C1 | 0.024 (6) | 0.026 (7) | 0.010 (5) | 0.003 (5) | 0.006 (5) | −0.002 (4) |
C2 | 0.025 (6) | 0.019 (7) | 0.018 (6) | −0.002 (5) | −0.004 (5) | −0.003 (5) |
C3 | 0.019 (6) | 0.026 (8) | 0.020 (6) | −0.001 (5) | 0.001 (4) | 0.006 (5) |
C4 | 0.017 (5) | 0.021 (7) | 0.020 (6) | −0.004 (4) | 0.001 (4) | 0.002 (5) |
C5 | 0.020 (6) | 0.030 (9) | 0.035 (7) | −0.008 (6) | −0.005 (5) | −0.009 (6) |
C6 | 0.030 (7) | 0.022 (7) | 0.021 (6) | 0.006 (5) | −0.002 (5) | 0.000 (5) |
C7 | 0.029 (7) | 0.012 (6) | 0.022 (6) | 0.010 (5) | −0.001 (5) | −0.001 (4) |
C8 | 0.033 (7) | 0.026 (9) | 0.020 (6) | −0.006 (6) | 0.002 (5) | −0.006 (5) |
C9 | 0.035 (8) | 0.033 (8) | 0.021 (6) | 0.005 (6) | 0.000 (5) | −0.015 (5) |
C10 | 0.042 (7) | 0.018 (7) | 0.018 (7) | 0.001 (5) | 0.001 (5) | −0.002 (5) |
C11 | 0.025 (7) | 0.050 (10) | 0.024 (6) | 0.005 (6) | −0.005 (5) | −0.002 (6) |
C12 | 0.031 (7) | 0.043 (8) | 0.021 (6) | −0.013 (6) | 0.007 (5) | −0.009 (6) |
C13 | 0.029 (7) | 0.027 (7) | 0.025 (6) | −0.005 (5) | 0.007 (6) | 0.003 (5) |
C14 | 0.039 (7) | 0.044 (9) | 0.017 (6) | 0.009 (7) | −0.005 (5) | 0.003 (5) |
C15 | 0.033 (7) | 0.028 (8) | 0.027 (7) | 0.004 (5) | 0.013 (6) | 0.000 (5) |
C16 | 0.024 (6) | 0.032 (8) | 0.020 (6) | 0.009 (5) | 0.000 (5) | 0.003 (5) |
C17 | 0.025 (6) | 0.025 (7) | 0.027 (6) | 0.008 (5) | −0.002 (5) | 0.000 (5) |
C18 | 0.033 (7) | 0.013 (7) | 0.036 (7) | 0.003 (5) | 0.011 (6) | 0.008 (5) |
C19 | 0.027 (6) | 0.029 (8) | 0.027 (6) | 0.001 (6) | −0.001 (5) | −0.004 (5) |
C20 | 0.028 (7) | 0.038 (9) | 0.034 (7) | −0.012 (6) | −0.001 (5) | 0.007 (6) |
C21 | 0.024 (6) | 0.015 (7) | 0.024 (6) | −0.006 (5) | 0.002 (5) | −0.004 (5) |
C22 | 0.019 (6) | 0.024 (7) | 0.022 (6) | −0.007 (5) | −0.003 (4) | −0.001 (5) |
C23 | 0.024 (6) | 0.033 (8) | 0.012 (5) | 0.007 (5) | −0.003 (4) | −0.001 (5) |
C24 | 0.031 (6) | 0.038 (8) | 0.017 (6) | −0.013 (5) | 0.001 (5) | 0.006 (5) |
C25 | 0.042 (8) | 0.038 (9) | 0.031 (7) | −0.009 (6) | 0.002 (6) | 0.014 (6) |
C26 | 0.049 (8) | 0.023 (8) | 0.033 (7) | −0.008 (6) | 0.002 (6) | 0.002 (5) |
C27 | 0.085 (14) | 0.13 (2) | 0.066 (13) | 0.005 (14) | −0.002 (11) | 0.033 (13) |
C28 | 0.14 (2) | 0.11 (2) | 0.089 (16) | −0.070 (16) | −0.049 (15) | 0.041 (13) |
C29 | 0.086 (13) | 0.078 (14) | 0.050 (10) | 0.005 (11) | 0.000 (9) | −0.007 (9) |
N1 | 0.021 (5) | 0.015 (5) | 0.012 (4) | 0.004 (4) | 0.004 (3) | −0.001 (4) |
N2 | 0.017 (5) | 0.019 (5) | 0.014 (4) | 0.005 (4) | −0.001 (3) | 0.004 (4) |
N3 | 0.024 (5) | 0.028 (6) | 0.025 (5) | −0.008 (4) | 0.001 (4) | 0.004 (4) |
N4 | 0.032 (5) | 0.022 (6) | 0.014 (5) | −0.002 (4) | −0.006 (4) | −0.003 (4) |
O1 | 0.026 (5) | 0.048 (6) | 0.024 (4) | 0.003 (4) | −0.001 (4) | −0.003 (4) |
O2 | 0.039 (5) | 0.027 (5) | 0.021 (4) | −0.003 (4) | −0.002 (4) | 0.003 (4) |
O3 | 0.034 (5) | 0.020 (5) | 0.043 (5) | 0.006 (4) | −0.001 (4) | −0.014 (4) |
O4 | 0.038 (5) | 0.038 (5) | 0.018 (5) | −0.002 (4) | 0.003 (3) | 0.000 (4) |
O5 | 0.036 (5) | 0.021 (5) | 0.044 (5) | 0.013 (4) | −0.008 (4) | 0.000 (4) |
O6 | 0.024 (5) | 0.039 (6) | 0.041 (5) | −0.007 (4) | 0.001 (4) | −0.010 (4) |
O7 | 0.025 (5) | 0.034 (5) | 0.032 (4) | 0.000 (4) | 0.005 (4) | −0.004 (4) |
O8 | 0.054 (6) | 0.017 (6) | 0.052 (6) | 0.007 (4) | 0.002 (4) | −0.002 (4) |
O9 | 0.028 (5) | 0.046 (6) | 0.054 (6) | −0.004 (4) | −0.006 (4) | −0.017 (4) |
O10 | 0.054 (6) | 0.043 (6) | 0.022 (5) | 0.007 (4) | 0.004 (4) | −0.001 (4) |
O11 | 0.038 (5) | 0.032 (6) | 0.055 (6) | −0.013 (4) | −0.001 (4) | 0.010 (4) |
O12 | 0.043 (5) | 0.067 (8) | 0.057 (6) | −0.003 (5) | 0.015 (5) | −0.034 (5) |
O13 | 0.035 (5) | 0.063 (7) | 0.031 (5) | 0.005 (4) | −0.005 (4) | 0.001 (4) |
O14 | 0.062 (6) | 0.069 (8) | 0.045 (6) | 0.049 (6) | −0.014 (5) | −0.010 (5) |
O15 | 0.039 (5) | 0.039 (6) | 0.028 (4) | 0.001 (4) | −0.006 (4) | −0.010 (4) |
O16 | 0.030 (5) | 0.060 (7) | 0.037 (5) | 0.001 (4) | 0.009 (4) | 0.018 (5) |
O17 | 0.028 (4) | 0.031 (5) | 0.029 (4) | −0.003 (4) | 0.003 (3) | 0.010 (4) |
O18 | 0.040 (5) | 0.047 (6) | 0.026 (4) | −0.001 (4) | −0.017 (4) | 0.002 (4) |
O19 | 0.038 (5) | 0.038 (6) | 0.044 (5) | −0.009 (4) | 0.002 (4) | 0.017 (4) |
O20 | 0.038 (5) | 0.029 (6) | 0.084 (7) | −0.001 (4) | 0.020 (5) | −0.024 (5) |
Ru1—C1 | 1.907 (11) | C1—O1 | 1.127 (12) |
Ru1—C2 | 1.909 (11) | C2—O2 | 1.126 (12) |
Ru1—C3 | 1.939 (13) | C3—O3 | 1.125 (13) |
Ru1—N1 | 2.097 (8) | C4—O4 | 1.129 (12) |
Ru1—Ru3 | 2.8544 (12) | C5—O5 | 1.130 (14) |
Ru1—Ru2 | 2.8992 (11) | C6—O6 | 1.142 (13) |
Ru1—H1 | 1.69 | C7—O7 | 1.134 (12) |
Ru2—C6 | 1.895 (12) | C8—O8 | 1.125 (14) |
Ru2—C5 | 1.918 (13) | C9—O9 | 1.115 (13) |
Ru2—C4 | 1.927 (11) | C10—O10 | 1.131 (12) |
Ru2—N2 | 2.103 (8) | C11—O11 | 1.136 (15) |
Ru2—Ru3 | 2.8509 (11) | C12—O12 | 1.140 (14) |
Ru2—H1 | 1.75 | C13—O13 | 1.121 (13) |
Ru3—C10 | 1.920 (11) | C14—O14 | 1.136 (14) |
Ru3—C8 | 1.933 (14) | C15—O15 | 1.141 (14) |
Ru3—C7 | 1.949 (12) | C16—O16 | 1.156 (13) |
Ru3—C9 | 1.964 (13) | C17—O17 | 1.125 (13) |
Ru4—C11 | 1.898 (15) | C18—O18 | 1.160 (14) |
Ru4—C12 | 1.904 (12) | C19—O19 | 1.145 (14) |
Ru4—C13 | 1.942 (12) | C20—O20 | 1.159 (15) |
Ru4—N3 | 2.094 (9) | C21—N1 | 1.336 (13) |
Ru4—Ru6 | 2.8457 (12) | C21—C22 | 1.391 (15) |
Ru4—Ru5 | 2.9124 (12) | C22—C23 | 1.363 (15) |
Ru4—H2 | 1.55 | C23—N2 | 1.356 (13) |
Ru5—C16 | 1.883 (12) | C24—N3 | 1.344 (14) |
Ru5—C15 | 1.914 (13) | C24—C25 | 1.394 (17) |
Ru5—H2 | 1.92 | C25—C26 | 1.374 (16) |
Ru5—C14 | 1.933 (13) | C26—N4 | 1.338 (15) |
Ru5—N4 | 2.115 (9) | C27—C28 | 1.29 (2) |
Ru5—Ru6 | 2.8357 (12) | C27—C29i | 1.42 (3) |
Ru5—H2 | 1.92 | C28—C29 | 1.39 (2) |
Ru6—C20 | 1.901 (14) | C29—C27i | 1.42 (3) |
Ru6—C18 | 1.925 (13) | N1—N2 | 1.351 (11) |
Ru6—C19 | 1.928 (13) | N3—N4 | 1.344 (12) |
Ru6—C17 | 1.957 (13) | ||
C1—Ru1—C2 | 92.8 (4) | C16—Ru5—C14 | 90.8 (5) |
C1—Ru1—C3 | 91.9 (4) | C15—Ru5—C14 | 98.5 (5) |
C2—Ru1—C3 | 97.5 (4) | H2—Ru5—C14 | 91.9 |
C1—Ru1—N1 | 173.1 (4) | C16—Ru5—N4 | 172.8 (4) |
C2—Ru1—N1 | 94.0 (4) | C15—Ru5—N4 | 95.7 (4) |
C3—Ru1—N1 | 88.2 (4) | H2—Ru5—N4 | 79.5 |
C1—Ru1—Ru3 | 90.6 (3) | C14—Ru5—N4 | 89.5 (4) |
C2—Ru1—Ru3 | 84.9 (3) | C16—Ru5—Ru6 | 91.6 (3) |
C3—Ru1—Ru3 | 176.5 (3) | C15—Ru5—Ru6 | 84.0 (3) |
N1—Ru1—Ru3 | 89.1 (2) | H2—Ru5—Ru6 | 85.4 |
C1—Ru1—Ru2 | 105.9 (3) | C14—Ru5—Ru6 | 176.4 (3) |
C2—Ru1—Ru2 | 139.0 (3) | N4—Ru5—Ru6 | 87.8 (2) |
C3—Ru1—Ru2 | 117.5 (3) | C16—Ru5—Ru4 | 105.8 (3) |
N1—Ru1—Ru2 | 68.1 (2) | C15—Ru5—Ru4 | 139.3 (3) |
Ru3—Ru1—Ru2 | 59.40 (3) | H2—Ru5—Ru4 | 29.2 |
C1—Ru1—H1 | 89.6 | C14—Ru5—Ru4 | 117.5 (3) |
C2—Ru1—H1 | 172.1 | N4—Ru5—Ru4 | 67.9 (2) |
C3—Ru1—H1 | 89.9 | Ru6—Ru5—Ru4 | 59.33 (3) |
N1—Ru1—H1 | 83.5 | C16—Ru5—H2 | 93.4 |
Ru3—Ru1—H1 | 87.6 | C15—Ru5—H2 | 168.5 |
Ru2—Ru1—H1 | 33.3 | C14—Ru5—H2 | 91.9 |
C6—Ru2—C5 | 91.2 (5) | N4—Ru5—H2 | 79.5 |
C6—Ru2—C4 | 93.9 (4) | Ru6—Ru5—H2 | 85.4 |
C5—Ru2—C4 | 98.0 (5) | Ru4—Ru5—H2 | 29.2 |
C6—Ru2—N2 | 173.2 (4) | C20—Ru6—C18 | 97.9 (5) |
C5—Ru2—N2 | 94.8 (4) | C20—Ru6—C19 | 92.8 (5) |
C4—Ru2—N2 | 88.2 (4) | C18—Ru6—C19 | 92.4 (4) |
C6—Ru2—Ru3 | 89.7 (3) | C20—Ru6—C17 | 92.2 (5) |
C5—Ru2—Ru3 | 86.1 (3) | C18—Ru6—C17 | 93.1 (4) |
C4—Ru2—Ru3 | 174.5 (3) | C19—Ru6—C17 | 172.0 (5) |
N2—Ru2—Ru3 | 87.7 (2) | C20—Ru6—Ru5 | 160.2 (3) |
C6—Ru2—Ru1 | 104.8 (3) | C18—Ru6—Ru5 | 101.9 (3) |
C5—Ru2—Ru1 | 141.3 (3) | C19—Ru6—Ru5 | 86.0 (3) |
C4—Ru2—Ru1 | 115.4 (3) | C17—Ru6—Ru5 | 87.2 (3) |
N2—Ru2—Ru1 | 68.6 (2) | C20—Ru6—Ru4 | 98.6 (3) |
Ru3—Ru2—Ru1 | 59.52 (3) | C18—Ru6—Ru4 | 163.4 (3) |
C6—Ru2—H1 | 89.4 | C19—Ru6—Ru4 | 89.4 (3) |
C5—Ru2—H1 | 172.8 | C17—Ru6—Ru4 | 83.6 (3) |
C4—Ru2—H1 | 89.2 | Ru5—Ru6—Ru4 | 61.68 (3) |
N2—Ru2—H1 | 84.2 | O1—C1—Ru1 | 176.1 (9) |
Ru3—Ru2—H1 | 86.7 | O2—C2—Ru1 | 179.7 (10) |
Ru1—Ru2—H1 | 32.0 | O3—C3—Ru1 | 177.1 (10) |
C10—Ru3—C8 | 100.2 (5) | O4—C4—Ru2 | 177.1 (10) |
C10—Ru3—C7 | 91.3 (4) | O5—C5—Ru2 | 176.8 (10) |
C8—Ru3—C7 | 90.9 (4) | O6—C6—Ru2 | 176.5 (10) |
C10—Ru3—C9 | 91.7 (5) | O7—C7—Ru3 | 172.4 (9) |
C8—Ru3—C9 | 93.2 (5) | O8—C8—Ru3 | 178.0 (11) |
C7—Ru3—C9 | 174.4 (4) | O9—C9—Ru3 | 175.7 (10) |
C10—Ru3—Ru2 | 161.9 (3) | O10—C10—Ru3 | 177.2 (10) |
C8—Ru3—Ru2 | 97.8 (3) | O11—C11—Ru4 | 176.9 (10) |
C7—Ru3—Ru2 | 86.7 (3) | O12—C12—Ru4 | 179.5 (11) |
C9—Ru3—Ru2 | 89.0 (3) | O13—C13—Ru4 | 176.5 (11) |
C10—Ru3—Ru1 | 100.8 (3) | O14—C14—Ru5 | 175.4 (10) |
C8—Ru3—Ru1 | 158.7 (3) | O15—C15—Ru5 | 178.2 (10) |
C7—Ru3—Ru1 | 85.1 (3) | O16—C16—Ru5 | 175.7 (10) |
C9—Ru3—Ru1 | 89.6 (3) | O17—C17—Ru6 | 173.9 (10) |
Ru2—Ru3—Ru1 | 61.08 (3) | O18—C18—Ru6 | 177.4 (10) |
C11—Ru4—C12 | 91.7 (5) | O19—C19—Ru6 | 174.6 (10) |
C11—Ru4—C13 | 93.4 (5) | O20—C20—Ru6 | 179.1 (11) |
C12—Ru4—C13 | 97.1 (5) | N1—C21—C22 | 109.0 (10) |
C11—Ru4—N3 | 172.9 (4) | C23—C22—C21 | 105.3 (9) |
C12—Ru4—N3 | 93.9 (4) | N2—C23—C22 | 109.3 (9) |
C13—Ru4—N3 | 90.3 (4) | N3—C24—C25 | 107.7 (10) |
C11—Ru4—Ru6 | 86.8 (3) | C26—C25—C24 | 106.4 (10) |
C12—Ru4—Ru6 | 88.1 (4) | N4—C26—C25 | 108.0 (11) |
C13—Ru4—Ru6 | 174.8 (3) | C28—C27—C29i | 102 (2) |
N3—Ru4—Ru6 | 89.0 (2) | C27—C28—C29 | 116 (2) |
C11—Ru4—Ru5 | 104.6 (3) | C28—C29—C27i | 122 (2) |
C12—Ru4—Ru5 | 141.6 (3) | C21—N1—N2 | 108.5 (8) |
C13—Ru4—Ru5 | 116.0 (3) | C21—N1—Ru1 | 139.1 (7) |
N3—Ru4—Ru5 | 68.3 (2) | N2—N1—Ru1 | 112.3 (6) |
Ru6—Ru4—Ru5 | 58.99 (3) | N1—N2—C23 | 107.8 (8) |
C11—Ru4—H2 | 91.7 | N1—N2—Ru2 | 110.8 (6) |
C12—Ru4—H2 | 176.6 | C23—N2—Ru2 | 141.0 (7) |
C13—Ru4—H2 | 82.6 | N4—N3—C24 | 108.4 (9) |
N3—Ru4—H2 | 82.8 | N4—N3—Ru4 | 112.2 (6) |
Ru6—Ru4—H2 | 92.2 | C24—N3—Ru4 | 139.4 (8) |
Ru5—Ru4—H2 | 37.2 | C26—N4—N3 | 109.6 (9) |
C16—Ru5—C15 | 91.3 (5) | C26—N4—Ru5 | 138.8 (7) |
C16—Ru5—H2 | 93.4 | N3—N4—Ru5 | 111.5 (7) |
C15—Ru5—H2 | 168.5 | ||
C1—Ru1—Ru2—C6 | 0.3 (4) | N1—Ru1—C2—O2 | 153 (100) |
C2—Ru1—Ru2—C6 | −113.7 (6) | Ru3—Ru1—C2—O2 | 65 (100) |
C3—Ru1—Ru2—C6 | 101.0 (5) | Ru2—Ru1—C2—O2 | 93 (100) |
N1—Ru1—Ru2—C6 | 176.7 (4) | C1—Ru1—C3—O3 | −104 (21) |
Ru3—Ru1—Ru2—C6 | −80.7 (3) | C2—Ru1—C3—O3 | −11 (21) |
C1—Ru1—Ru2—C5 | 111.6 (6) | N1—Ru1—C3—O3 | 83 (21) |
C2—Ru1—Ru2—C5 | −2.4 (7) | Ru3—Ru1—C3—O3 | 121 (19) |
C3—Ru1—Ru2—C5 | −147.7 (6) | Ru2—Ru1—C3—O3 | 147 (20) |
N1—Ru1—Ru2—C5 | −72.0 (5) | C6—Ru2—C4—O4 | 72 (17) |
Ru3—Ru1—Ru2—C5 | 30.6 (5) | C5—Ru2—C4—O4 | −19 (18) |
C1—Ru1—Ru2—C4 | −101.5 (4) | N2—Ru2—C4—O4 | −114 (17) |
C2—Ru1—Ru2—C4 | 144.6 (6) | Ru3—Ru2—C4—O4 | −157 (15) |
C3—Ru1—Ru2—C4 | −0.7 (5) | Ru1—Ru2—C4—O4 | −179 (100) |
N1—Ru1—Ru2—C4 | 75.0 (4) | C6—Ru2—C5—O5 | −72 (19) |
Ru3—Ru1—Ru2—C4 | 177.5 (3) | C4—Ru2—C5—O5 | 22 (19) |
C1—Ru1—Ru2—N2 | −178.6 (4) | N2—Ru2—C5—O5 | 111 (19) |
C2—Ru1—Ru2—N2 | 67.5 (5) | Ru3—Ru2—C5—O5 | −161 (19) |
C3—Ru1—Ru2—N2 | −77.8 (4) | Ru1—Ru2—C5—O5 | 173 (100) |
N1—Ru1—Ru2—N2 | −2.1 (3) | C5—Ru2—C6—O6 | 138 (18) |
Ru3—Ru1—Ru2—N2 | 100.4 (2) | C4—Ru2—C6—O6 | 40 (18) |
C1—Ru1—Ru2—Ru3 | 81.0 (3) | N2—Ru2—C6—O6 | −68 (19) |
C2—Ru1—Ru2—Ru3 | −33.0 (5) | Ru3—Ru2—C6—O6 | −136 (18) |
C3—Ru1—Ru2—Ru3 | −178.2 (3) | Ru1—Ru2—C6—O6 | −78 (18) |
N1—Ru1—Ru2—Ru3 | −102.6 (2) | C10—Ru3—C7—O7 | −28 (7) |
C6—Ru2—Ru3—C10 | 109.5 (11) | C8—Ru3—C7—O7 | 72 (7) |
C5—Ru2—Ru3—C10 | −159.2 (11) | C9—Ru3—C7—O7 | −150 (6) |
C4—Ru2—Ru3—C10 | −21 (3) | Ru2—Ru3—C7—O7 | 170 (7) |
N2—Ru2—Ru3—C10 | −64.2 (11) | Ru1—Ru3—C7—O7 | −129 (7) |
Ru1—Ru2—Ru3—C10 | 2.2 (11) | C10—Ru3—C8—O8 | 29 (36) |
C6—Ru2—Ru3—C8 | −75.9 (5) | C7—Ru3—C8—O8 | −62 (36) |
C5—Ru2—Ru3—C8 | 15.4 (5) | C9—Ru3—C8—O8 | 121 (36) |
C4—Ru2—Ru3—C8 | 153 (3) | Ru2—Ru3—C8—O8 | −149 (36) |
N2—Ru2—Ru3—C8 | 110.4 (4) | Ru1—Ru3—C8—O8 | −141 (36) |
Ru1—Ru2—Ru3—C8 | 176.8 (3) | C10—Ru3—C9—O9 | −2 (14) |
C6—Ru2—Ru3—C7 | −166.4 (4) | C8—Ru3—C9—O9 | −102 (14) |
C5—Ru2—Ru3—C7 | −75.1 (4) | C7—Ru3—C9—O9 | 120 (13) |
C4—Ru2—Ru3—C7 | 63 (3) | Ru2—Ru3—C9—O9 | 160 (14) |
N2—Ru2—Ru3—C7 | 19.9 (4) | Ru1—Ru3—C9—O9 | 99 (14) |
Ru1—Ru2—Ru3—C7 | 86.3 (3) | C8—Ru3—C10—O10 | −60 (21) |
C6—Ru2—Ru3—C9 | 17.2 (5) | C7—Ru3—C10—O10 | 31 (21) |
C5—Ru2—Ru3—C9 | 108.5 (5) | C9—Ru3—C10—O10 | −154 (21) |
C4—Ru2—Ru3—C9 | −114 (3) | Ru2—Ru3—C10—O10 | 114 (20) |
N2—Ru2—Ru3—C9 | −156.5 (4) | Ru1—Ru3—C10—O10 | 116 (21) |
Ru1—Ru2—Ru3—C9 | −90.1 (4) | C12—Ru4—C11—O11 | 73 (21) |
C6—Ru2—Ru3—Ru1 | 107.4 (3) | C13—Ru4—C11—O11 | −24 (21) |
C5—Ru2—Ru3—Ru1 | −161.4 (3) | N3—Ru4—C11—O11 | −145 (20) |
C4—Ru2—Ru3—Ru1 | −24 (3) | Ru6—Ru4—C11—O11 | 161 (21) |
N2—Ru2—Ru3—Ru1 | −66.4 (2) | Ru5—Ru4—C11—O11 | −142 (21) |
C1—Ru1—Ru3—C10 | 72.5 (5) | C11—Ru4—C12—O12 | 104 (100) |
C2—Ru1—Ru3—C10 | −20.3 (5) | C13—Ru4—C12—O12 | −163 (100) |
C3—Ru1—Ru3—C10 | −153 (5) | N3—Ru4—C12—O12 | −72 (100) |
N1—Ru1—Ru3—C10 | −114.4 (4) | Ru6—Ru4—C12—O12 | 17 (100) |
Ru2—Ru1—Ru3—C10 | −179.3 (3) | Ru5—Ru4—C12—O12 | −13 (100) |
C1—Ru1—Ru3—C8 | −117.0 (9) | C11—Ru4—C13—O13 | 24 (15) |
C2—Ru1—Ru3—C8 | 150.2 (9) | C12—Ru4—C13—O13 | −68 (15) |
C3—Ru1—Ru3—C8 | 18 (5) | N3—Ru4—C13—O13 | −162 (15) |
N1—Ru1—Ru3—C8 | 56.1 (9) | Ru6—Ru4—C13—O13 | 116 (15) |
Ru2—Ru1—Ru3—C8 | −8.8 (9) | Ru5—Ru4—C13—O13 | 132 (15) |
C1—Ru1—Ru3—C7 | 162.9 (4) | C16—Ru5—C14—O14 | −52 (15) |
C2—Ru1—Ru3—C7 | 70.1 (4) | C15—Ru5—C14—O14 | 39 (15) |
C3—Ru1—Ru3—C7 | −62 (5) | H2—Ru5—C14—O14 | −145.8 |
N1—Ru1—Ru3—C7 | −24.0 (4) | N4—Ru5—C14—O14 | 135 (15) |
Ru2—Ru1—Ru3—C7 | −88.9 (3) | Ru6—Ru5—C14—O14 | 174 (10) |
C1—Ru1—Ru3—C9 | −19.1 (4) | Ru4—Ru5—C14—O14 | −161 (15) |
C2—Ru1—Ru3—C9 | −111.9 (4) | C16—Ru5—C15—O15 | −10 (36) |
C3—Ru1—Ru3—C9 | 116 (5) | H2—Ru5—C15—O15 | 104.5 |
N1—Ru1—Ru3—C9 | 154.0 (4) | C14—Ru5—C15—O15 | −101 (36) |
Ru2—Ru1—Ru3—C9 | 89.1 (3) | N4—Ru5—C15—O15 | 169 (36) |
C1—Ru1—Ru3—Ru2 | −108.2 (3) | Ru6—Ru5—C15—O15 | 82 (36) |
C2—Ru1—Ru3—Ru2 | 159.0 (3) | Ru4—Ru5—C15—O15 | 107 (36) |
C3—Ru1—Ru3—Ru2 | 26 (5) | C15—Ru5—C16—O16 | −109 (14) |
N1—Ru1—Ru3—Ru2 | 64.9 (2) | H2—Ru5—C16—O16 | 81.5 |
C11—Ru4—Ru5—C16 | 5.2 (5) | C14—Ru5—C16—O16 | −10 (14) |
C12—Ru4—Ru5—C16 | 117.3 (7) | N4—Ru5—C16—O16 | 82 (15) |
C13—Ru4—Ru5—C16 | −96.0 (5) | Ru6—Ru5—C16—O16 | 167 (14) |
N3—Ru4—Ru5—C16 | −175.2 (4) | Ru4—Ru5—C16—O16 | 108 (14) |
Ru6—Ru4—Ru5—C16 | 82.3 (3) | C20—Ru6—C17—O17 | 42 (9) |
C11—Ru4—Ru5—C15 | −106.1 (6) | C18—Ru6—C17—O17 | −56 (9) |
C12—Ru4—Ru5—C15 | 6.0 (8) | C19—Ru6—C17—O17 | 170 (8) |
C13—Ru4—Ru5—C15 | 152.7 (6) | Ru5—Ru6—C17—O17 | −158 (9) |
N3—Ru4—Ru5—C15 | 73.5 (6) | Ru4—Ru6—C17—O17 | 140 (9) |
Ru6—Ru4—Ru5—C15 | −29.0 (5) | C20—Ru6—C18—O18 | −23 (22) |
C11—Ru4—Ru5—H2 | 73.0 | C19—Ru6—C18—O18 | −116 (22) |
C12—Ru4—Ru5—H2 | −174.9 | C17—Ru6—C18—O18 | 70 (22) |
C13—Ru4—Ru5—H2 | −28.2 | Ru5—Ru6—C18—O18 | 158 (22) |
N3—Ru4—Ru5—H2 | −107.4 | Ru4—Ru6—C18—O18 | 148 (21) |
Ru6—Ru4—Ru5—H2 | 150.1 | C20—Ru6—C19—O19 | −25 (10) |
C11—Ru4—Ru5—C14 | 104.6 (6) | C18—Ru6—C19—O19 | 73 (10) |
C12—Ru4—Ru5—C14 | −143.3 (8) | C17—Ru6—C19—O19 | −154 (9) |
C13—Ru4—Ru5—C14 | 3.4 (6) | Ru5—Ru6—C19—O19 | 174 (100) |
N3—Ru4—Ru5—C14 | −75.8 (5) | Ru4—Ru6—C19—O19 | −124 (10) |
Ru6—Ru4—Ru5—C14 | −178.2 (4) | C18—Ru6—C20—O20 | −12 (100) |
C11—Ru4—Ru5—N4 | −178.2 (4) | C19—Ru6—C20—O20 | 81 (100) |
C12—Ru4—Ru5—N4 | −66.1 (7) | C17—Ru6—C20—O20 | −105 (100) |
C13—Ru4—Ru5—N4 | 80.5 (4) | Ru5—Ru6—C20—O20 | 167 (100) |
N3—Ru4—Ru5—N4 | 1.4 (4) | Ru4—Ru6—C20—O20 | 171 (100) |
Ru6—Ru4—Ru5—N4 | −101.1 (3) | N1—C21—C22—C23 | 0.8 (12) |
C11—Ru4—Ru5—Ru6 | −77.1 (3) | C21—C22—C23—N2 | −0.2 (11) |
C12—Ru4—Ru5—Ru6 | 35.0 (6) | N3—C24—C25—C26 | −0.1 (14) |
C13—Ru4—Ru5—Ru6 | −178.3 (4) | C24—C25—C26—N4 | 0.0 (14) |
N3—Ru4—Ru5—Ru6 | 102.5 (3) | C29i—C27—C28—C29 | 45 (3) |
C16—Ru5—Ru6—C20 | −102.8 (11) | C27—C28—C29—C27i | −54 (3) |
C15—Ru5—Ru6—C20 | 166.0 (11) | C22—C21—N1—N2 | −1.2 (11) |
H2—Ru5—Ru6—C20 | −9.6 | C22—C21—N1—Ru1 | 178.8 (7) |
C14—Ru5—Ru6—C20 | 31 (6) | C1—Ru1—N1—C21 | −147 (3) |
N4—Ru5—Ru6—C20 | 70.0 (11) | C2—Ru1—N1—C21 | 41.4 (11) |
Ru4—Ru5—Ru6—C20 | 4.6 (10) | C3—Ru1—N1—C21 | −56.0 (10) |
C16—Ru5—Ru6—C18 | 75.7 (5) | Ru3—Ru1—N1—C21 | 126.2 (10) |
C15—Ru5—Ru6—C18 | −15.4 (5) | Ru2—Ru1—N1—C21 | −176.7 (11) |
H2—Ru5—Ru6—C18 | 169.0 | C1—Ru1—N1—N2 | 33 (3) |
C14—Ru5—Ru6—C18 | −151 (6) | C2—Ru1—N1—N2 | −138.7 (6) |
N4—Ru5—Ru6—C18 | −111.4 (4) | C3—Ru1—N1—N2 | 124.0 (6) |
Ru4—Ru5—Ru6—C18 | −176.9 (3) | Ru3—Ru1—N1—N2 | −53.8 (6) |
C16—Ru5—Ru6—C19 | −15.9 (5) | Ru2—Ru1—N1—N2 | 3.3 (5) |
C15—Ru5—Ru6—C19 | −107.0 (5) | C21—N1—N2—C23 | 1.1 (10) |
H2—Ru5—Ru6—C19 | 77.4 | Ru1—N1—N2—C23 | −178.9 (6) |
C14—Ru5—Ru6—C19 | 118 (6) | C21—N1—N2—Ru2 | 175.4 (6) |
N4—Ru5—Ru6—C19 | 157.0 (4) | Ru1—N1—N2—Ru2 | −4.6 (7) |
Ru4—Ru5—Ru6—C19 | 91.5 (3) | C22—C23—N2—N1 | −0.5 (11) |
C16—Ru5—Ru6—C17 | 168.3 (5) | C22—C23—N2—Ru2 | −172.2 (8) |
C15—Ru5—Ru6—C17 | 77.2 (5) | C6—Ru2—N2—N1 | −6 (4) |
H2—Ru5—Ru6—C17 | −98.4 | C5—Ru2—N2—N1 | 147.2 (6) |
C14—Ru5—Ru6—C17 | −58 (6) | C4—Ru2—N2—N1 | −114.9 (6) |
N4—Ru5—Ru6—C17 | −18.8 (4) | Ru3—Ru2—N2—N1 | 61.3 (6) |
Ru4—Ru5—Ru6—C17 | −84.3 (3) | Ru1—Ru2—N2—N1 | 3.3 (5) |
C16—Ru5—Ru6—Ru4 | −107.4 (3) | C6—Ru2—N2—C23 | 165 (3) |
C15—Ru5—Ru6—Ru4 | 161.5 (3) | C5—Ru2—N2—C23 | −41.4 (11) |
H2—Ru5—Ru6—Ru4 | −14.1 | C4—Ru2—N2—C23 | 56.5 (11) |
C14—Ru5—Ru6—Ru4 | 26 (6) | Ru3—Ru2—N2—C23 | −127.3 (11) |
N4—Ru5—Ru6—Ru4 | 65.5 (2) | Ru1—Ru2—N2—C23 | 174.7 (11) |
C11—Ru4—Ru6—C20 | −69.3 (5) | C25—C24—N3—N4 | 0.1 (13) |
C12—Ru4—Ru6—C20 | 22.4 (5) | C25—C24—N3—Ru4 | 179.9 (9) |
C13—Ru4—Ru6—C20 | −162 (4) | C11—Ru4—N3—N4 | 1 (4) |
N3—Ru4—Ru6—C20 | 116.4 (4) | C12—Ru4—N3—N4 | 142.8 (7) |
Ru5—Ru4—Ru6—C20 | −178.4 (4) | C13—Ru4—N3—N4 | −120.1 (7) |
C11—Ru4—Ru6—C18 | 119.9 (12) | Ru6—Ru4—N3—N4 | 54.7 (7) |
C12—Ru4—Ru6—C18 | −148.3 (12) | Ru5—Ru4—N3—N4 | −2.1 (6) |
C13—Ru4—Ru6—C18 | 27 (4) | C11—Ru4—N3—C24 | −179 (84) |
N3—Ru4—Ru6—C18 | −54.4 (11) | C12—Ru4—N3—C24 | −37.0 (12) |
Ru5—Ru4—Ru6—C18 | 10.8 (11) | C13—Ru4—N3—C24 | 60.2 (12) |
C11—Ru4—Ru6—C19 | 23.4 (5) | Ru6—Ru4—N3—C24 | −125.0 (12) |
C12—Ru4—Ru6—C19 | 115.2 (5) | Ru5—Ru4—N3—C24 | 178.1 (12) |
C13—Ru4—Ru6—C19 | −69 (4) | C25—C26—N4—N3 | 0.0 (13) |
N3—Ru4—Ru6—C19 | −150.9 (4) | C25—C26—N4—Ru5 | 176.0 (9) |
Ru5—Ru4—Ru6—C19 | −85.7 (3) | C24—N3—N4—C26 | −0.1 (12) |
C11—Ru4—Ru6—C17 | −160.6 (5) | Ru4—N3—N4—C26 | −179.9 (7) |
C12—Ru4—Ru6—C17 | −68.8 (5) | C24—N3—N4—Ru5 | −177.3 (7) |
C13—Ru4—Ru6—C17 | 107 (4) | Ru4—N3—N4—Ru5 | 2.9 (8) |
N3—Ru4—Ru6—C17 | 25.1 (4) | C16—Ru5—N4—C26 | −150 (3) |
Ru5—Ru4—Ru6—C17 | 90.3 (3) | C15—Ru5—N4—C26 | 40.6 (12) |
C11—Ru4—Ru6—Ru5 | 109.1 (4) | H2—Ru5—N4—C26 | −150.0 |
C12—Ru4—Ru6—Ru5 | −159.1 (4) | C14—Ru5—N4—C26 | −57.9 (12) |
C13—Ru4—Ru6—Ru5 | 17 (4) | Ru6—Ru5—N4—C26 | 124.3 (12) |
N3—Ru4—Ru6—Ru5 | −65.2 (2) | Ru4—Ru5—N4—C26 | −178.0 (12) |
C2—Ru1—C1—O1 | −119 (15) | C16—Ru5—N4—N3 | 26 (4) |
C3—Ru1—C1—O1 | −22 (15) | C15—Ru5—N4—N3 | −143.5 (7) |
N1—Ru1—C1—O1 | 69 (16) | H2—Ru5—N4—N3 | 26.0 |
Ru3—Ru1—C1—O1 | 156 (15) | C14—Ru5—N4—N3 | 118.0 (7) |
Ru2—Ru1—C1—O1 | 98 (15) | Ru6—Ru5—N4—N3 | −59.7 (6) |
C1—Ru1—C2—O2 | −26 (100) | Ru4—Ru5—N4—N3 | −2.1 (6) |
C3—Ru1—C2—O2 | −118 (100) |
Symmetry code: (i) −x+1/2, −y+5/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ru3H(C3H3N2)(CO)10]·C1.50H3 |
Mr | 672.43 |
Crystal system, space group | Monoclinic, I2/a |
Temperature (K) | 153 |
a, b, c (Å) | 14.2248 (11), 9.1670 (5), 59.834 (5) |
β (°) | 90.380 (9) |
V (Å3) | 7802.1 (10) |
Z | 16 |
Radiation type | Mo Kα |
µ (mm−1) | 2.35 |
Crystal size (mm) | 0.50 × 0.45 × 0.40 |
Data collection | |
Diffractometer | Stoe IPDS diffractometer |
Absorption correction | Multi-scan (Blessing, 1995) |
Tmin, Tmax | 0.224, 0.251 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18544, 4743, 4474 |
Rint | 0.041 |
θmax (°) | 22.3 |
(sin θ/λ)max (Å−1) | 0.535 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.107, 1.36 |
No. of reflections | 4743 |
No. of parameters | 532 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + 252.1712P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.00, −0.81 |
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.
Ru1—N1 | 2.097 (8) | Ru4—H2 | 1.55 |
Ru1—Ru3 | 2.8544 (12) | Ru5—N4 | 2.115 (9) |
Ru1—Ru2 | 2.8992 (11) | Ru5—Ru6 | 2.8357 (12) |
Ru1—H1 | 1.69 | Ru5—H2 | 1.92 |
Ru2—N2 | 2.103 (8) | C21—N1 | 1.336 (13) |
Ru2—Ru3 | 2.8509 (11) | C23—N2 | 1.356 (13) |
Ru2—H1 | 1.75 | C24—N3 | 1.344 (14) |
Ru4—N3 | 2.094 (9) | C26—N4 | 1.338 (15) |
Ru4—Ru6 | 2.8457 (12) | N1—N2 | 1.351 (11) |
Ru4—Ru5 | 2.9124 (12) | N3—N4 | 1.344 (12) |
N1—Ru1—Ru2 | 68.1 (2) | N4—Ru5—Ru4 | 67.9 (2) |
Ru3—Ru1—Ru2 | 59.40 (3) | Ru6—Ru5—Ru4 | 59.33 (3) |
N2—Ru2—Ru1 | 68.6 (2) | Ru5—Ru6—Ru4 | 61.68 (3) |
Ru3—Ru2—Ru1 | 59.52 (3) | N2—N1—Ru1 | 112.3 (6) |
Ru2—Ru3—Ru1 | 61.08 (3) | N1—N2—Ru2 | 110.8 (6) |
N3—Ru4—Ru5 | 68.3 (2) | N4—N3—Ru4 | 112.2 (6) |
Ru6—Ru4—Ru5 | 58.99 (3) | N3—N4—Ru5 | 111.5 (7) |
The parent cluster (I), as well as its derivatives [Ru3(µ-H){µ-N2C3H(CH3)2-3,5}(CO)10], (II), and [Ru3(µ-H)(CO)10{µ-N2C3H(CF3)2-3,5}], (III), were first synthesized by Bruce et al. (1986) from the reaction of Ru3(CO)12 and the corresponding pyrazole in refluxing cyclohexane. Only the di(trifluoromethyl)pyrazolyl derivative, (III), was obtained in good yield and studied by X-ray diffraction. More recently, Cabeza et al. (1995) synthesized (II) by protonation of the anionic cluster [Ru3{µ-N2C3H(CH3)2-3,5}(µ-CO)3(CO)7]-, which was synthesized by reaction between 3,5-dimethylpyrazole and the anionic cluster [Ru3(µ-H)(µ-CO)(CO)10]- in refluxing tetrahydrofuran. Here were report a new synthetic route and the X-ray crystal structure analysis of (I), which can be obtained in good yield by reaction of potassium dihydrobis(1-pyrazolyl)borate (Trofimenko, 1970) with Ru3(CO)12 in refluxing MeOH.
The molecular structure of [Ru3(µ-H)(µ-N2C3H3)(CO)10], (I), was confirmed by single-crystal X-ray analysis. The asymmetric unit comprises two independent molecules of (I) and half a molecule of cyclohexane. Fig. 1 shows only one independent molecule of (I), and significant bond lengths and angles are given in Table 1. The triruthenium core of (I) consists of an asymmetric Ru3 triangle, the three metal–metal bonds (average of the two molecules in the asymmetric unit) [2.850 (1), 2.907 (1) and 2.843 (1) Å] are comparable to those observed in (III) [2.849 (1), 2.902 (1) and 2.846 (1) Å]. The pyrazole ligand and the hydrido bridge two Ru atoms in an axial fashion. The Ru—N bond distances [average 2.095 (9) and 2.109 (9) Å] are sligthly shorter than those in (III) [Ru—N 2.146 (3) and 2.137 (3) Å]. The angles between the planar pyrazolyl ligands and the Ru3 planes are, respectively, 75.5° for molecule 1 and 76.8° for molecule 2.